#archive of organic and inorganic chemical sciences | Explore Tumblr Posts and Blogs

sherristockman · 6 years

Link

Is Nonalcoholic Beer an Effective Recovery Drink? Dr. Mercola By Dr. Mercola Is it possible nonalcoholic beer was partly responsible for Germany’s success in the 2018 Winter Olympics? According to German ski team doctor Johannes Scherr,1 the answer is a resounding yes. Scherr says nearly all of his athletes drink nonalcoholic beer during training and some continued drinking it as a recovery beverage during the Winter Games. Research conducted by Scherr and others show alcohol-free beer fights inflammation and reduces upper respiratory tract infections (URTIs). Nonalcoholic beer is so intertwined with German sports, the brewery Krombacher shipped 3,500 liters (about 924 gallons) of it to the athletes' village in Pyeongchang, South Korea. German Olympic athletes such as alpine ski racer Linus Strasser and biathlete Simon Schempp are among those who routinely use beer as a recovery drink. While it may be difficult to directly link the nonalcoholic brew with Germany’s success, the country tied for first with Norway with 14 gold medals and took second place overall with a total medal count of 31. While those results are impressive, you may be wondering about the science behind beer as a sports drink. Is nonalcoholic beer an effective rehydration and recovery drink? The Science Behind ‘Recovery Beer’ for Athletes According to The New York Times,2 Scherr, who in addition to his role as an Olympic team doctor is also a sports medicine teacher at the Technical University of Munich, made the discovery about “recovery beer” in 2009. At the time, Scherr noticed athletes who drank nonalcoholic beer suffered fewer URTIs than athletes who had received a placebo. In addition, Scherr noted athletes who consumed nonalcoholic brew also experienced significantly reduced inflammation, which enabled them to recover faster between competitions. Scherr’s double-blind study, which was financed by a brewing company and published in the journal Medicine and Science in Sports and Exercise3 in 2012, involved 277 healthy male runners. The men, ages 31 to 51, were participants in the Munich Marathon. Each runner consumed 1 to 1.5 liters of nonalcoholic beer daily for three weeks prior to and two weeks immediately following the race. The placebo group received a similar foamy nonalcoholic beer with the polyphenols removed. The objective of the research was to determine if nonalcoholic beer, which contains antioxidant, antipathogenic and anti-inflammatory properties, could benefit athletes. To Scherr’s surprise, the results indicated the group of beer-drinking runners, as compared to the placebo group, experienced:4,5 A 20 percent reduction in the activity of white blood cells, a good indicator of inflammation More than a threefold reduction in the incidence of postrace URTIs Given the outcome, German athletes are not the only ones benefiting from nonalcoholic beer as a recovery beverage — a 2016 Chilean study6 published in the journal Nutrients found soccer players who downed nonalcoholic beer before their workouts stayed better hydrated than their peers who drank regular beer and water. Polyphenols and Beer: What’s the Connection? The high concentration of polyphenols contained in beer is what researchers believe delivers the powerful immune-boosting effects uncovered by Scherr and his colleagues. According to Runner’s World, “beer is known to include more than 2,000 organic and inorganic chemicals, including more than 50 polyphenols from barley and hops.”7 One of Scherr’s research partners, David Nieman, a professor in Appalachian State University's department of health and exercise science, has studied the health benefits of phenols. He suggests phenol-rich diets help lower inflammation and curb your risk of illness. In addition to their antiviral properties, Nieman states, "[Polyphenols] have a very unique molecular structure that can actually regulate the genes that control inflammation.”8 To be effective as a recovery beverage, nonalcoholic beer has to be formulated properly, says associate professor and dietitian Ben Desbrow, Ph.D., from Griffith University in Australia.9 Traditional beer provides an insufficient amount of carbohydrates and electrolytes to benefit your body after exercise, notes Desbrow, who has been experimenting with formulations that will provide the beneficial properties of a rehydration drink without the dehydrating effects of alcohol. In a 2013 study published in International Journal of Sports Nutrition and Exercise Metabolism,10 Desbrow and his colleagues found that beer with a lower alcohol content and added salt provided better hydration than traditional compositions. Given its status as a plant-based beverage, Desbrow and his team believe reduced-alcohol beer has more naturally occurring nutrients than commercial sports drinks. "A properly formulated beer beverage is likely to do you no more harm than you are likely to get from a sports drink," said Desbrow.11 A 2015 study,12 also involving Desbrow, reflects that making changes to the electrolyte concentration of low-alcohol beer appears to more significantly impact an athlete’s postexercise fluid retention than small changes made to its alcohol content. The History of German Nonalcoholic Beer Although nonalcoholic beer has been around in Germany since 1973, Scherr notes only in the past decade have beer companies been more intentional about pitching nonalcoholic products to health-conscious consumers. Once the scientific research was completed, the public began to respond to alcohol-free beer. As such, according to Euromonitor International, consumption of nonalcoholic beer in Germany grew 43 percent from 2011 to 2016, even as overall consumption of beer declined.13 According to The New York Times,14 Germans fall in second place behind Iran as the nation consuming the most nonalcoholic beer. It’s no surprise then to learn that Germany has worked hard to develop brewing techniques designed to perfect and differentiate the flavor of alcohol-free brews. The work seems to be wildly successful based on the fact more than 400 nonalcoholic beers are now available on the German market. Below are a few of the tactics German breweries have used to market their nonalcoholic beers exclusively as sports drinks:15 Bavarian brewery Erdinger touts its nonalcoholic wheat beer as “the isotonic thirst quencher for athletes” Heineken alcohol-free beer, which is dubbed “Heineken 0.0,”16 will be featured in vending machines at McFit Fitness locations nationwide Nonalcoholic beer is made available to runners at the finish line of most major German marathons, with Erdinger supplying 30,000 bottles of its "Alkoholfrei" beer to finishers of the 2017 Berlin Marathon In a press release announcing its sponsorship of a 2015 marathon in Orange County, California, Erdinger had this to say about its sober brew:17 “Brewed under the strict Bavarian Purity Law of 1516, which requires high-quality, only natural ingredients, Erdinger Non-Alcoholic replenishes the body with essential vitamins including B9 and B12, which help reduce fatigue, promote energy-yielding metabolism and support the immune system. The brew contains less than 0.5 percent of alcohol by volume, and is low in calories with just 125 per serving.” Alcohol-Free Beer Versus Traditional Sports Drinks: Which Is Better? Traditional sports drinks like Gatorade do not have much of a following in Germany. One reason for this may be the high sugar content. Nonalcoholic beer has a lower sugar content than most sports drinks and a taste that is preferred by Germans. “It tastes good, and it’s good for the body,” said Strasser after finishing his second run in the men’s giant slalom at the Winter Olympics. “Alcohol-free wheat beer, for example, is extremely healthy.”18 German speed skater Moritz Geisreiter says he drank nonalcoholic beer from the grocery store before switching to a custom sports beverage created by a nutritionist. “[Nonalcoholic beer is] a nice solution for someone who doesn’t want to pay dozens of euros a week for a nutrition drink,” he said during an interview at the Olympic speedskating oval in Gangneung, South Korea.19 Despite their increasing market share and tremendous popularity, particularly in the U.S., sports drinks are a terrible choice. They are overmarketed to children and teens and promoted as a necessity after even mild activity. In my opinion, they are among the worst beverages you can consume. If you don’t believe me, take a look at some of the ingredients featured in one popular brand: Citric acid Glycerol ester of rosin High-fructose corn syrup (Glucose-fructose syrup) Modified food starch Monopotassium phosphate Natural flavor Red 40 Salt Sodium citrate Sucrose syrup Water Many sports drinks contain as much as two-thirds the sugar of a comparable serving of soda. In addition, as reflected above, these unnaturally neon-colored beverages are filled with toxic ingredients such as artificial flavors, artificial colors and high-fructose corn syrup. On top of that, the low-calorie and sugar-free versions most likely contain artificial sweeteners, which are even worse for you than fructose. An additional concern is the fact the sugar content of a single sports drink (roughly 29 grams) represents nearly TWICE the daily recommended fructose allowance if you are insulin resistant, and it's 4 grams over the suggested limit if you are noninsulin resistant! Because your liver has to process all that sugar, you put yourself at risk of chronic metabolic disease and insulin resistance when you overconsume sugar. Unchecked, insulin resistance can progress to metabolic syndrome and Type 2 diabetes. The metabolism of fructose by your liver also creates a number of waste products and toxins, including a large amount of uric acid, which drives up your blood pressure and can cause gout. Before you decide if nonalcoholic beer is a better choice than commercial sports drinks, it’s important to consider some of the ingredients commonly found in beer. Caution: Your Favorite Beer May Contain Toxic Ingredients If the ingredients in commercial sports drinks not only have you concerned, but also thinking beer may be a better choice for hydration and recovery, think twice. You may be surprised to learn that most beer, particularly brands produced in the U.S., contain toxic ingredients known to damage your health, such as genetically engineered (GE) corn, corn syrup and high fructose corn syrup, as well as bisphenol A (BPA),carrageenan, caramel coloring, monosodium glutamate and propylene glycol, to name a few.20,21 Based on stricter regulations around food safety as well as bans on genetically modified organisms (GMOs), European beers are typically a better choice, as are organic beers. About German beers, the Food Babe says:22 “German beers are … a good bet. The Germans are very serious about the purity of their beer and enacted a purity law called ‘Reinheitsgebot’ that requires all German beers to be only produced with a core ingredient list of water, hops, yeast, malted barley or wheat. Advocates of German beers insist they taste cleaner and some even claim they don’t suffer from hangovers as a result.” If you choose to use nonalcoholic beer as a recovery beverage after strenuous workouts, be sure to do your homework and choose a brand that has a clean ingredient list. Better yet, consider coconut water. Coconut Water: Your Best Source of Natural Electrolytes While alcohol-free beer has secured its place as a popular and well-liked rehydration beverage for German athletes, including many who competed in this year’s Winter Olympics, I believe coconut water is still the best rehydration drink on the planet. Coconut water is a well-known source of natural electrolytes and boasts an outstanding nutritional profile. It’s so well-regarded, in fact, coconut water was used intravenously, short-term, during World War II to help hydrate critically ill patients in emergency situations. Coconut water is particularly beneficial if you engage in activities resulting in profuse sweating. You can drink it plain or add fresh citrus juice for flavor. Beyond its alkalizing effects, coconut water possesses unique nutritional qualities due to the fact coconut palms grow in rich volcanic soils and mineral-rich seawater. Coconut water is: A powerhouse of electrolytes and natural salts, especially magnesium and potassium Full of cytokinins, or plant hormones, which have antiaging, anticancer and antithrombotic effects in humans Light, low-calorie and low in sugar, but pleasantly sweet Packed with amino acids, antioxidants, enzymes, organic acids and phytonutrients Rich in natural vitamins (particularly B vitamins), minerals and trace elements, including iodine, manganese, selenium, sulfur and zinc Coconut Water Is the No. 1 'Sports Drink' For most amateur athletes and casual exercisers, sports drinks are not only unnecessary and costly, but also, they can damage your health. A tiny fraction of the people who consume sports drinks derive any benefit from them. Due to the number of toxic ingredients, most sports drinks do more harm than good. Fortunately, natural coconut water is free of toxins and artificial ingredients. (Watch out for bottled varieties though, as they often contain unhealthy additives.) If you exercise for 30 minutes a day at a low to moderate intensity or engage in high-intensity interval training (HIIT), clean, pure water is the main beverage you need to stay hydrated. It's only when you've been exercising for more than 60 minutes, in high heat or at extreme intensity levels, involving profuse sweating, that you may need something more than water to replenish your body.If you need electrolytes, coconut water will provide them. If you don't need electrolytes, intaking them certainly won't hurt you. To restore your salt balance, you might want to add a tiny pinch of natural Himalayan salt to your glass of coconut water.

#VitalityPath

0 notes

lupinepublishers · 2 years

Text

Lupine Publishers | Value Chain Analysis for Medicinal Plant based products in India: Case Study of Uttarakhand

Value Chain Analysis for Medicinal Plant based products in India: Case Study of Uttarakhand

Abstract

Value chain concepts and approaches can be used to understand the integration of producers of high value products in developing countries with regional and global markets. A value chain is a description of range of activities that involves processes of production, delivery and final disposal of the product after use. The value chain analysis involves the study of the structure, actors, and dynamics of value chains that connect farm and forest products. The participants, linkages, structure of cost and benefit and dynamics of the value chain are studied.

The standardization of the production procedures in case of medicinal plant industry is important to develop a uniformity and acceptability in all parts of the world. The various processes of the value chain i.e. cultivation, maintenance, harvesting, processing, storage, packaging of the medicinal and aromatic plant industry are required to be standardized to meet the criteria for the certification as well as for the assessment of the quality and safety norms of the product and extracts thus produced. Certifications and the standardization define the safety and quality of the product that are essential in the international markets for the commodities to be traded abroad. The analysis discusses about the current scenario of value chain of the medicinal plant industry and how the standardization of the value addition contributes in the trade of medicinal and aromatic plants.

Keywords:Value chain; Medicinal plants; Uttarakhand; India; Herbal industry; Spices

Introduction

Background

Value addition is the process of economically adding value to a product by altering its current place, time and from one set of characteristics to other characteristics that are more favored in the marketplace [1]. Value addition is the process of creating value in existing value chain of a product. Value addition in medicinal plant industry starts at grass root level of cultivation of medicinal plants and primary processing of medicinal and aromatic plants which includes the procedures like cleaning, drying and sorting of medicinal plants at very initial phase of collection and harvesting of medicinal plants.

The basic theory for calculating the value addition at every level of the production process is the difference between the market price of the product and the total cost of production of the inputs used for the production (Figure 1).

Figure 1: Value Addition Theoretical representation.

The demand for chemicals and products derived from medicinal and aromatic plants is increasing globally and has opened up opportunities for entrepreneurs to add value to these plants through processing, thereby generating enormous employment avenues [2]. India has abundance of medicinal plants with 8000 medicinal and 2500 aromatic species which are mined for natural chemicals and processed for commercial products that are then exported globally. An upward trend has been recorded in the exports of medicinal and aromatic plants’ products in recent years which have encouraged Government and private organizations for developing processed products with medicinal plants. Value addition through processing involves employment of unskilled rural youth and unemployed, educated urban youth. A number of value added consumer products can be developed from a single medicinal or aromatic plant for trade in national and international markets.

Value chain actors

The returns received by the actors of the medicinal plant value chain namely villagers, middlemen and wholesaler, constitute the total trade in medicinal plants. The villagers constitute the first link in the trade in medicinal plants wherein the cultivators separately or combined collect the medicinal plant produce and take them up to the processors for further refinement. There upon, the middle men intervene in the medicinal plant trade and act as facilitators due to the lack of efficient infrastructure and link the cultivators to the wholesalers for commissions. The wholesalers are the distributors of the medicinal plant products to the ultimate markets and they carry out the work through a complex network of agents and retailers.

The medicinal plant value chain also included the secondary actors which are the industries that use the medicinal plants and their extracts as their input materials and then the value added to them through the processes operated on them through which the end products are obtained. The Pharmaceutical industries and the Cosmetic industries are the prime example of the value addition made to the medicinal plants. These industries use the medicinal and aromatic plants in fixed percentages and the final products made are the blend of multiple such plants and extracts.

Research motivation

The medicinal plant industry in the North Indian state of the Uttarakhand though is established, but the industry lacks a systematic structure and direction which can grant the various actors of the medicinal plant value chain proper guidelines and direction to develop the products that match the international quality standards. The international trade in medicinal plants and allied products is based on certain qualitative and safety standards which should be in place to ensure safety of the medicinal plants traded. The application and adherence of such standards in production of the medicinal plants in the country is eminent in order to explore the entire international trade potential of the medicinal plants.

For the purpose of analyzing the impact of value addition made by different actors of the medicinal plant value chain and the value added by the standardization of the production of medicinal plant products, qualitative method of analysis has been used. The existing studies have primarily focused on determining the value addition made by various actors of the value chain of medicinal plants. A very limited number of studies have explored the benefits of standardization of the various processes that are crucial to the quality of the end products of the medicinal plant industry. This study attempts to do that.

Objectives of the research

1. To understand the value chain processes in medicinal plant industry of Uttarakhand

2. To identify the issues in the value chain processes of the industry

3. To analyze the impact of standardization of active ingredients of value chain on the trade

The study begins with the introduction of the study. The previous studies pertaining to the topic have been discussed in the literature review section. Research gaps have been identified in the same chapter and research framework has been formed. In the next chapter, research methodology has been stated in which the process that has been adopted during the entire course of the investigation has been discussed. Data analysis has been discussed in the succeeding chapter. This chapter is followed by discussions, conclusions, and recommendations for future work.

Literature Review

Value chain of MAPs

Value Chain (VC) defines a complete series of activities which are mandatory to carry the product or service from beginning through the different phases of production to the end consumer and discarding the product after its usage [3]. The value chain concept is an analytical approach that is been deployed used for evaluating the performance of the marketing initiatives of any industry or organization. This kind of analysis helps in identifying the loop holes in the performance system of marketing initiatives and implementing measures for refining the private and public interventions [4].

Medicinal plants and its related products have a wide ranging value chain activities associated with it. Recent estimates suggest that trade related activities of herbs is projected to attain a financial worth of US$ 5 Trillion by 2050. Realizing this increasing demand, it becomes important to assess the activities that can be restructured for smooth flow of medicinal herbs from producers to end consumers. This kind of analysis helps in understanding the difference that prevails in quality of the herbal medicines in different market zones and identify superior quality products over the inferior ones.

The value chain in medicinal plant industry comprises of the producers, collector, processors, wholesalers, exporters and distributors and retailer. The producers, or the cultivators or, the collectors are the upstream actors of the medicinal plant value chain and they provide the industry with the basic raw material and inputs for the other participants to function. While the processors, the wholesalers, the retailers, the traders and the exporters are the downstream actors of the medicinal plant value chain which provide the raw inputs of the medicinal plants with value and the capacity to the trade. The downstream actors enhance the utility of the medicinal plants and impart value to the products through processing and packaging of the products which increases the shelf life of the products.

Producers

The production system of MAPs products comprises of three major groups; wild crafters, plantation operators and cultivators. The three broad categories of producers differ according to the level of power they own, the practices they employ and the benefits they draw from these valuable resources. State Forest Departments are anticipated to control the harvesting of forest produce and are also expected to maintain a record of such produce. Thus, majority of information about the raw materials can directly be obtained from people working in the state forest department.

Collectors

Collectors are those middlemen who gather harvested herbal species from agriculturalists and wild crafters and make them available to processors. Because of the changeable demand of the products, collectors do not involve in the gathering process until they receive an order for the same. Formerly, several cooperative societies in Uttarakhand were assigned the role of collection process. Bhesaj Sangh, was one amongst the trusted collecting agency. But in the year 1986, Kumaon Mandal Vikas Nigam (KMVN) was started by the government officials to undertake activities pertaining to collection process and regulate the unnecessary exploitation of the growers. Thereafter, Garhwal Vikas Mandal Nigam (GVMN) was assigned the authority of regulating the allied activities of the medicinal plant agricultural sector. Despite this, Bhesaj Sangh, because of its consistent attention on collection of medicinal and aromatic plants,wasfar more popular in comparison to their counterpart.

Processors

Processing of the harvested medicinal herbs is done in two stages; semi-processing and alteration in the preparations. The first stage of the processing includes activities like cleaning the organic material stuck to the herbal species by drying; building concentrates, disinfecting, boiling and grinding. Marketing processed products adds value to their produce thereby allowing them charge higher prices for the same. The processing stage involves numerous activities including the drying, packaging, storage which enhance the shelf life and assist the marketing of the medicinal plant products.

Wholesalers and exporters

The wholesalers and the retailers constitute the organized part of the medicinal plant value chain. The links like the cultivators, collectors, processors and handlers in medicinal plant industry in Northern India are inherently unorganized and scattered in nature, while the downstream actors, the wholesalers and retailers are relatively formal in their structure. The wholesalers and the exporters provide the upstream actors of the medicinal plant value chain with valuable information of the trends and patterns of the consumer demand for the medicinal plant products in the domestic as well as in the international markets.

Distribution and retailing

The distributors and retailers play a crucial role in connecting the consumers to the producers through the wholesalers and help the consumers in attaining the products they desire. The medicinal plant cultivation usually is situated in the remote areas of the countries with abundant and rich biodiversity while a majority of the consumers are centered in the clusters of urban areas. The retailers provide the function of connecting the producers with the consumers. The retailers obtain the medicinal plants from the wholesalers and in certain cases, directly from the producers (processors) and offer the medicinal plant products in the market to the consumers for the ultimate consumption. The retail sellers of the medicinal plant industry also performs the function of acquiring the required credential sand certificates for the medicinal plants before such products can enter the consumer markets as the per the national and regional safety and quality norms [5].

The distributors, on the other hand perform, similar functions like the retailers but they interact with both the wholesalers and the retailers while the retailers interact only with the consumers.

Standardization of MAPs

Lazarowych et al. [6] in their study of the Standardization practices of the botanical drugs and the various strategies used for the standardization, have highlighted the standardization of the medicinal plants and the resultant botanical drugs has enabled the development of the required strategies for the enhancement of the quality of the products of the industry and maintenance of the homogeneity of the medicinal plant products. Well established system of standardization, according to Lazarowych et al. [6] can help to establish efficient control mechanisms for quality of the raw medicinal plants and the processed extracts of the plants. The need for standardization in medicinal plant industry has been further accentuated in a paper by Folashade et al. [7] which corresponds to the issue of standardization of the herbal plant industry. According to Folashade et al. [7] the standardization of the medicinal plant and the herbal product industry is eminent because of the act that the medicinal plants and the processes involved in their value addition are based upon a fine balance of constituents and are precariously time lined. Any deviation from the balance might lead to serious implications on the quality and nature of the end product. Without the standardization of the production and processing stages, the value chain actors may act independently and the resultant products might not be favorable for the consumers for the desired treatment of the ailments. The authors lay the responsibility of ensuring the safety of the consumers and the products that they consume on the Authorities’ shoulders and the safe procedures of production, harvesting, processing and packaging ought to be outlined by the authorities so that the ground rules for the production are set in the industry which can then be used as the basic criteria for judging the products and the assessment of the products can be assisted in similar manner.

Research gaps and framework

Certifications and the standards provide the products with the scientific seals of safety and quality that are essential in the international markets for the commodities to be traded abroad. The current study determines the importance of standardization of value chain processes by examining its impact on trade volume and trade price of Medicinal Plants (Figure 2).

Figure 2: Research Framework.

Irrespective of the increasing demand and huge market size of the medicinal products, there is a huge gap in the amount of studies that have been undertaken in the context of value chain of medicinal plants, that too specifically in the context of Uttarakhand. There exist several prior researches which focus on determining the value addition made by the various actors of the value chain of medicinal plants but not many studies explore the benefits of standardization of the various processes that are crucial to the quality of the end products of the medicinal plant industry.

Research Methodology

The aim of the study is to understand the current status of value chain processes of medicinal plants in Uttarakhand and the impact of standardization of value chain processes on trade volume and trade price of medicinal plants. This is done because it has been observed that majority of the trade in this particular sector was happening in its raw form. The data has been collected from various government sources such as State government medicinal Plant websites: NMPB, ENVIS etc. and empirical research papers related to this area. The analysis provides information about the certifications the various systems of AYUSH, value chain practices, cost and benefits and trade related information of medicinal plants. The impact of standardization on trade volume has been analyzed in the data analysis.

For the purpose of satisfying this particular objective, analysis has been performed to ascertain the impact of the standardization on the Indian export of medicinal and aromatic plants and the allied products, the year in which the standards were established in the Indian medicinal plant Industry has been used as the benchmark year and comparative analysis has been done of the Indian trade in medicinal plants five years prior and five years post the standardization of the industry in order to gather the overall impact of the standardization on the economy.

The study is descriptive in nature in the sense that it includes collection of data that explains events and then organizes to come up as a result. Secondary data related to quantity of medicinal plants collected/produced/traded have been collected from the records of the State Forest Departments in many research studies [8,9] (Figure 3).

Findings

Value chain analysis of MAPs in Uttarakhand

The value chain makes addition at every level of the production. The value chain actors are responsible for processing and adding value to the medicinal plants and developing the product to fulfill global demand. The value chain analysis of medicinal plants is done to understand the discrepancies in the process and to assess ways to improve the same.

Figure 3: Research Validation Framework through Analysis.

The division of the returns from the trade in medicinal plants among the various actors in medicinal plant trade has been depicted below. All through the medicinal plants under consideration, trend continues wherein wholesalers takes up the largest piece of the pie and get the largest share in the returns from total trade in the medicinal plants and returns to middlemen follow soon after for receiving the second highest share in the total returns from medicinal plant trade. The initial cultivator or villagers are the worst off group of players in medicinal plant trade (Figure 4).

Figure 4: Participation in the medicinal plant trade and the relative share in income.

There have been identified issues regarding the distribution of income and an attempt has been made to understand the probable reasons. One such reason can be unregistered and untrained farmers. Lack of training and understanding of the process and acknowledgement of market value of medicinal plants is the reason for unequal distribution of returns arising from sale of medicinal plants.

The analysis of the data set reveals a larger share of medicinal and aromatic plant trade going to the wholesalers which is contradicted by the findings of Shahidullah and Haque (2010) in their study of the relationship between the medicinal plant production and livelihood enhancement in the case of Bangladesh. Their study indicates that the primary and secondary- wholesale markets for the medicinal plants are dominated by the middlemen and not the primary producers and the wholesalers who benefitted from the trade in medicinal plants. According to their findings, the medicinal plant cultivation is sustainable for the relatively economically well off cultivators who usually have access to the better quality of land and the technical equipments. However, Shahidullah & Haque [10] also agreed that the small scale medicinal plant cultivators need to organize themselves in order to gain better holding in the market through an improved control over the quantity supplied in the market and hence the prices which determines their returns.

The value addition in specific species was also assessed. The comparative scrutiny of the value addition made by the cultivators for the given medicinal plants reveals that the value addition was the highest in the case of Chandramul, Kapur Kachari and Sarpgandha at Rs. 13680 while Kali Jiri had the lowest value addition made at the primary stage of cultivation. The value addition in the given data set was lowest for the plant Kali jiri while Kapur Kachari, Sarpgandha and Chandramul had the highest value added at the cultivation level of the medicinal plant value chain (Figure 5) (Table 1).

Figure 5: Value Addition of speies (Source: Envis.nic, 2011, http://jharenvis.nic.in/).

Table 1: System wise distribution (%) of good manufacturing practice and non-good manufacturing practice-compliant Ayurveda, Yoga and Naturopathy, Unani, Siddha, and Homeopathy pharmacies (Source: Samal, 2016).

Standardization of medicinal and aromatic plants and its impact on trade

The certifications of the value chain processes improve the tradability of medicinal plants since it assures the quality of the product to buyers in different countries. Certification programs have been introduced by Indian agencies as well to improve the acceptability of Indian medicinal products abroad. However, the compliance is not made mandatory for the companies and other participants. The systems wise distribution (%) of good manufacturing practice and non-good manufacturing practicecompliant Ayurveda, Yoga and Naturopathy, Unani, Siddha, and Homeopathy pharmacies has been depicted below that suggests that many of the AYUSH pharmacies do not comply to Good Manufacturing Practices and do not even have license.

AYUSH: Ayurveda, Yoga, and Naturopathy, Unani, Sidhha and Homeopathy

GMP: good manufacturing practices: The capacity of trade of medicinal plants in Uttarakhand has been assessed through number of traders present in different districts, amount of wholesale trade and trade through mandis. The district wise distribution of the medicinal plant traders in the state of Uttarakhand in the period ranging from 2008-09 to 2012-13 has been depicted below. In the year 2008-09, the total number of traders in the medicinal plant trade amounted to 571 and the highest number of traders were in the district of Pithoragarh while the lowest were in the districts of Rudraprayag. The year 2009-10, the total number of traders was 600 wherein the highest number of traders was in the Pithoragarh 259 and the lowest numbers of traders were in the Chamoli district of Uttarakhand. In the next year 2010-11, the total number of traders was 864 and the highest number of traders was in the Pithoragarh district while Uttarkashi and Rudraprayag had the lowest number of traders of the medicinal plants. The year 2011-12 witnessed the numbers of traders decline to 594 with the highest number of traders in Pithoragarh (337) and the lowest in Rudraprayag (1). The year 2012-13 witnessed an increase in the number of total traders to 732 with highest number of traders in the Pithoragarh district and the least traders in Rudraprayag. The number of traders in the given period increased from the 571 in 2008-09 to 864 in 2010-11 but declined to 594 thereafter in 2012- 13 (Figure 6).

Figure 6: Medicinal plant traders in Uttarakhand 2008-09 to 2012-13.

The impact of standardization on trade has also been assessed. The voluntary scheme of standardization scheme introduced in the year 2009 was adopted by many companies involved in the value processing of medicinal plants. The impact of the scheme on the trade values of medicinal plants has been assessed and for this, pre and post 2009, figures of trade, when standardization was introduced for the medicinal plants has been compared.

The exports figures of the medicinal plants in the years prior and post the launch of the standardization scheme by the government in the year 2009-10 have been depicted. The years 2003-04 to 2008-09 have been taken into consideration to grasp the export scenario of the medicinal plants before the launch of the medicinal plant standardization. In the year 2008-09, the total exports of the medicinal plant products was 125.4 million USD which was a major improvement since 2003-04 when the Indian exports of the medicinal plant products to the rest of the world used to be 65.71 million USD. The total exports for the given period amounted to 528.75million USD. The exports reached a high of 233.7 million USD worth of medicinal plant export in the year 2014-15. The total exports in the period ranging from 2009-10 to 2014-15 were almost the double of the total medicinal plant export of the previous period at 1068.22 million USD.

Table 2: Total export of Medicinal and Aromatic Plants (2003-2015).

Figure 7: Total exports of Medicinal and Aromatic Plants (2003-2015).

The trend of Indian exports of medicinal plants over the period ranging from 2003-04 to 2014-15 and the effect of the standardization on the total exports of the medicinal plants of the country have been analyzed. The year 2008-09 has been taken the bench mark year in which the National medicinal Plant Board of India introduced the standards in the Indian medicinal plant industry. The year post the introduction of the certification policies in the system saw a fall in the export of the medicinal plants for one year which picked up in the corresponding years. The Indian medicinal plant exports have improved over the year’s post the standardization of the industry which implies the positive impact the certification and standardization has had over the industry exports (Table 2) (Figure 7).

The analysis of the data reveals that the standardization of the medicinal plant industry does indeed has improved the foreign trade quantities of the Indian medicinal and aromatic plants in the foreign which is evident in the study of the pattern of trade which corresponds five years prior to the standardization and certification obligation (2004-05 to 2008-09) in the country and five year post the standardization (2009-10 to 2013-14) of the industry. The comparative analysis of the figures shows a boom in the Indian exports to the world in the years after the standardization was made compulsory in the year 2008-09 for the medicinal plant cultivators, processors and the marketers and traders. The basic requirement for the standardization of the medicinal plants is explained by Tierra (2002) in his research article discussing the need for standardization of the medicinal plants and extracts. Tierra emphasizes that the standardization of the medicinal plants and extracts would lead to a higher degree of technological refinement of the products of the industry as compared to unorganized system of the medicinal plants and the resultant products provide safer, stronger and more effective products that are supported by an adequate scientific evidence to substantiate the quality and the authenticity of the medicinal plants and the extracts and oils derived from them.

The standardization process is likely to minimize the gap between the prices offered in Indian market and international markets. Authenticated raw material is the basic starting point for the development and manufacturing of a botanical product. Harvesting, storing, processing and formulating methods may effect on the quality and consistency of the herbal product. Our herbal products are not getting international market because we are not capable to show the international standard of our products. A coordinated effort of all the supply chain actors and improved market facilities is likely to improve the export prices of the medicinal and aromatic plants; as discussed in Table 3. The rising export prices from the year 2008-09 till 2012-2012, shows that significant improvements were made in the traded prices of the medicinal produce. Thereafter the prices declined might be because of ineffective marketing strategies or poor market linkages.

Table 3: Export prices of Medicinal and Aromatic Plants (2008-16).

Lazarowych et al. [6] in their study of the Standardization practices of the botanical drugs and the various strategies used for the standardization, have highlighted the standardization of the medicinal plants and the resultant botanical drugs has enabled the development of the required strategies for the enhancement of the quality of the products of the industry and maintenance of the homogeneity of the medicinal plant products. Well established system of standardization according Lazarowych et al. [6] can help to establish efficient control mechanisms for quality of the raw medicinal plants and the processed extracts of the plants. The need for standardization in medicinal plant industry has been further accentuated in a paper by Folashade et al. [7] which corresponds to the issue of standardization of the herbal plant industry. According to Folashade et al. [7] the standardization of the medicinal plant and the herbal product industry is eminent because of the act that the medicinal plants and the processes involved in their value addition are based upon a fine balance of constituents and are precariously time lined. Any deviation from the balance might lead to serious implications on the quality and nature of the end product. Without the standardization of the production and processing stages, the value chain actors may act independently and the resultant products might not be favorable for the consumers for the desired treatment of the ailments [11,12].

Conclusion

The standardization of the production procedures of the medicinal plant industry is eminent for the development of a more systematic, uniform and high quality medicinal and aromatic plant industry in India. The standards of the cultivation, maintenance, harvesting, processing, storage, and packaging function of the medicinal and aromatic plant industry are necessary to set up the criteria for the certification as well as for the assessment of the quality and safety norms of the product and extracts thus produced. Certifications and the standards provide the products with the scientific seals of safety and quality that are essential in the international markets for the commodities to be traded abroad. Further, the analysis talks about the current scenario in the medicinal plant industry wherein the returns are unequally distributed among the various actors of the medicinal plant value chain which leads to the low participation in the industry as well as the poor performance at the grass root level. The wholesalers and the middlemen in the state of Uttarakhand take up a majority of the medicinal plant sector’s revenue while the small scale cultivators receive little which impedes the performance of the sector. Medicinal plant sector in the North Indian state of Uttarakhand needs a systematic organization structure which assists the value chain actors in receiving the quantum of returns due to them and the injection of standardization and uniformity of the commodities produced which further enhances the value of the products in the domestic and the international markets. There are various issues identified in the value chain process of medicinal plants such as distribution of income among the various value chain participants, lack of training and understanding of the process and acknowledgement of market value of medicinal plants and lack of quality of products. These issues can be addressed through standardization of medicinal plants value chain and a strong plan to create awareness among the participants of value chain. The government of India in collaboration with the national medicinal plant board and the state medicinal plant boards has decided permissible level of contaminants in the production of selected medicinal plants. These level needs to be adhered to in order to gain local and state level permission from the authorities to function in the markets.

for more information about Archives of Organic and Inorganic Chemical Sciences archive page click on below link

https://lupinepublishers.com/chemistry-journal/archive.php

for more information about lupine publishers page click on below link

https://lupinepublishers.com/index.php

#lupine publishers #lupine publishers group #lupine publishers LLC #archive of organic and inorganic chemical sciences

0 notes

lupinepublishers · 3 years

Text

Lupine Publishers|An Efficient Protocol for the One Pot Synthesis of Pyranopyrazoles in Aqueous Medium using Triethanolamine as a Catalyst

Abstract

Triethanolamine is an efficient and green catalyst for the synthesis of 6-amino-1, 4-dihydro-4-substituted-3-methylpyrano-[2, 3-c] pyrazole-5-carbonitrile in aqueous medium reflux conditions. The procedure is easier, eco friendly, simple with easy workup affording good yield of the corresponding products.

Keywords: Multi component reaction, Water media, Pyranopyrazole, Catalyst, Triethanolamine

Introduction

The present scenario for organic synthesis indicates the crave for green and economical synthesis of organic compounds. One of it is multi component synthesis. Strecker’s synthesis for amino acids was the first report on multi component reaction [1]. Last few decades show large development in it. The main aim of such reactions is to fasten the reaction rate by reducing number of steps involved and eventually increase the yield of reaction. In this context to achieve great efficiency catalysts are employed. Catalysts such as Nano α-Al2O3 supported ammonium dihydrogenphosphate [2], tungstate sulfuric acid [3], Fe3-xTixO4@SO3H nanoparticles [4], nano-titania sulfuric acid (15-nm TSA) [5], nanostructured MgO [6], H14[NAP5W30O110] [7] and ZnO Nanoparticles [8].

Organic catalysts such as Triethylamine [9] DABCO [10], Trishydroxymethyl aminomethane [11] are also reported in various organic transformations. Triethanolamine contains basic tertiary amine and primary alcoholic part (Figure 1).

It is used for activation of both CO2 and epoxides to convert them in to cyclic carbonates [12]. It is also reported as a legend for copper catalyzed hydroxylation of aryl halides in aqueous medium [13]. It is used as aqueous solvent for controllable preparation of ZnO nano flowers in sol gel technique [14]. Its aqueous solution is reported as electrolyte in CO2 Photo electro-conversion catalyzed by Cu- Doped Graphene-Titania Catalyst [15]. Also it is found to increase the rate of oxidation of mesitylene catalyzed by cobalt bromide [16]. It is used as sacrificial electron donor in photocatalytic system [17]. Furthermore; it improved the catalytic performance of CuBr/ PMDETA in the atom transfer radical polymerization [18]. It is also used as phase transfer catalyst for synthesis of 1-(arylsulfonyl) aryl/heterylmethanes [19]. It is used as medium for synthesis of 3-substituted coumarins using L-proline as a catalyst [20]. It is reported as catalyst in 10 mol% for synthesis of 2-amino-3-cyano- 4H-pyran derivatives under ultrasound irradiation at 600C [21].

Synthesis of substituted pyrano-[2,3-d]-pyrimidines via one-pot three-component condensation of aromatic aldehydes, malononitrile and barbituric acid or 2-thiobarbituric acid using trace amounts of ionic liquid (choline chloride.ZnCl2) and triethanolamine (0.1Mol%) at 75°C with stirring and under ultrasound irradiation [22] is also reported in literature. Herein we successfully attempted a fast and simple protocol for the synthesis of 6-amino-1,4-dihydro-4-substituted-3-methylpyrano [2,3-c]- pyrazole-5-carbonitrile by the one pot three component reaction of aromatic aldehyde, malononitrile and 3-methyl-1H-pyrazol-5(4H)- one using triethanolamine as a catalyst [23].

Results and Discussion

To explore the synthetic application of triethanolamine, in the present work we report the catalytic facet of it for the synthesis of heterocyclic compounds bearing pyrazole skeleton. To optimize the reaction conditions, we chose anisaldehyde as the prototype. Initially, 10mol% of triethanolamine was taken for solvent free reaction at room temperature. But the reaction afforded a low yield of the product after 2 hour stirring. Then we used 10ml of water for room temperature stirring [24]. After 2 hours stirring it gave 62% of yield. The yield of reaction gets drastically changed on increasing temperature. At 900C we got 85% of yield of the product. When 20mol% of triethanolamine was used then we got 92% of yield at 900C in 10 ml water. Other solvents were also studied expecting better yield but other than ethanol and water we got poor yields (Table 1). Further increase of temperature and amount of triethanolamine did not improve yield significantly (Table 1). After optimizing the reaction conditions, differently substituted aldehydes with electron donating as well as electron withdrawing groups were reacted to examine the feasibility of this catalytic reaction (Scheme 1).

Almost all aldehydes bearing various substituents such as –Cl, F, -NO2, -OMe etc afforded good yield of the corresponding products. All the synthesized compounds showed sharp peaks at 3410, 3356cm- 1(-NH2) and 2190cm-1(-CN) in IR spectra which supports for the formation of pyranopyrazole. The formed products being insoluble in water were easy to separate from the aqueous medium by simple filtration. The reason for catalytic activity of triethanolamine is it’s solubility in aqueous medium and basic nature. Products are simply purified by re crystallization with ethanol. Thus the protocol described herein is efficient for the synthesis of pyrazopyrazoles which do not need purification by column chromatography.

Model reaction* for anisaldehyde (2mmol), malononitrile (2mmol) and 3-methyl-1H-pyrazol-5(4H)-one (2mmol) using the above cited conditions @Isolated yield.

Experimental

Melting points were recorded in open capillaries and were uncorrected. Progress of reaction was monitored by TLC (30% of ethyl acetate: n-hexane). IR spectra were taken by KBr disc on Shimadzu IR Affinity 1 spectrophotometer [1]. H NMR spectra were recorded on a Varian 400MHz spectrophotometer in the specified solvents. Chemical shifts were expressed in 𝛿ppm relative to TMS. Mass spectra were recorded on a Macro mass spectrometer (Waters) by electro spray method (ES).

General method for the synthesis of 6-amino-1, 4-dihydro- 4-substituted-3-methylpyrano-[2,3-C]-pyrazole- 5-carbonitrile

To a stirred mixture of aromatic aldehyde (2mmol), malononitrile (2mmol) and triethanolamine (20mol %) in 10ml of water, 3-methyl-1H-pyrazol-5(4H)-one (2mmol) was added. The resulting mixture was stirred and heated at 900C for appropriate reaction time (Table 2). After completion of reaction, the reaction mixture was cooled, filtered off the residue as the crude product which was further purified by re crystallization form ethanol (Scheme 2).

Representative Spectral Data

6-Amino-1,4-dihydro-4-(4-methoxyphenyl)-3-methylpyrano[ 2,3-c]pyrazole-5-carbonitrile (4a)

White solid, [1]H NMR (400 MHz, DMSO-d6): 𝛿 ppm 12.08 (s, 1H), 6.87-7.23 (m, 4H), 6.81 (bs, 2H), 4.45 (s, 1H), 3.78 (s, 3H), 1.81 (s, 3H); IR (KBr) cm-1: 3425, 3128, 2928, 2200, 1597, 1153, 1203; ES-MS m/z: 283.2 (M+1)+.

6-Amino-2,4-dihydro-3-methyl-4-phenylpyrano[2,3-c] pyrazole- 5-carbonitrile (4e)

White solid, M.P. 245-246 0C; 1H NMR (400 MHz, DMSO-d6) : 𝛿 ppm 12.10 (s, 1H), 7.10-7.40 (m, 5H), 6.85 (s, bs, 2H), 4.60 (s, 1H), 1.78 (s, 3H); IR (KBr) cm−1 : 3410, 3356, 3167, 2990, 1646, 1596, 1399, 1276, 870; ES-MS m/z: 253 (M + 1) +.

6 - A m i n o - 4 - ( 4 - c h l o r o p h e n y l ) - 3 - m e t h y l - 2 , 4 - dihydropyrano[2,3-c]pyrazole-5-carbonitrile (4g)

Off-white solid, M.P. 230-2320C; 1H NMR (400 MHz, DMSO-d6): 𝛿 ppm 12.15 (s, 1H), 7.10–7.40 (m, 4H), 6.95 (s, bs, 2H), 4.63 (s, 1H), 1.80 (s, 3H); IR (KBr) cm−1 : 3478, 3035, 2985, 2193, 1647, 1596, 1398, 1284, 870; ES-MS m/z: 287 (M + 1) +.

6-Amino-4-(4-N, N-dimethylaminophenyl)-3-methyl-2, 4-dihydropyrano[2, 3-c]pyrazole-5-carbonitrile (4j)

Yellow solid, M.P. 234-235 0C; 1H NMR (400 MHz, DMSO-d6): 𝛿 ppm 12.10 (s, 1H), 6.70-7.15 (m, 4H); 6.55 (s, bs, 2H), 4.40 (s, 1H); 2.85 (s, 6H), 1.78 (s, 3H); IR (KBr) cm−1 : 3385, 3172, 2957, 2189, 1644, 1601, 1397, 1279, 868; ES-MS m/z: 296 (M + 1) +.

Conclusion

In summary, we have developed an efficient protocol for the synthesis of pyranopyrazoles by a simple method using a catalytic amount of triethanol amine. Herein; not only the yield of reaction is improved but also the reaction time is reduced. The workup of the reaction is very simple which make it easier to isolate the product.

#For more information #https://lupinepublishers.com/chemistry-journal/archive.php #Please click here #https://lupinepublishers.com/chemistry-journal/#Lupine Publishers #archive of organic and inorganic chemical sciences #Pyranopyrazole

5 notes · View notes

lupinepublishers · 3 years

Text

Lupine Publishers|The Washing Effect of Quaternary Layered NCMA Cathode Materials

Abstract

Li(Ni0.82Co0.11Mn0.05Al0.01)O2 (NCMA) cathodes are synthesized by adding Al2O3 during high temperature solid state reaction. The results show that Al element can largely increase the surface stability of cathode compared to pristine NCM cathode and thus suppress the severe capacity fading after washing process. NCMA delivers a discharge capacity of 203.8 mAh g-1 at 0.2 C, with an outstanding capacity retention of 94% after 50 cycles at 25°C. This proposed synthesis strategy demonstrates that an optimal doping method will immensely retain the electrochemical performance while reduce content of the residual lithium compounds during the washing process which promote industrial fabrication of cathode materials.

Keywords: NCMA; washing process; cathode material; Li-ion battery Abbreviations: Li(Ni0.82Co0.11Mn0.05Al0.01)O2 (NCMA); Li(Ni0.83Co0.12Mn0.05)O2 (NCM); Scanning electron microscope (SEM); X-ray diffraction spectra (XRD); Cyclic voltammetry (CV); Electrochemical impedance spectroscopy (EIS)

Introduction

Lithium-ion batteries (LIBs) have been widely studied to meet the growing demand for the portable electronic devices and electrical vehicles [1, 2]. The LiNixCoyMnzO2 cathode materials (NCM) are considered to be the most promising cathode materials due to the high specific capacity and low capital cost [3, 4].Notably, the specific capacity of NCM can be improved by increasing the Ni composition in the layered structure. However, the Ni-rich cathodes with nickel content above 80% suffer from poor surface stability which hindered the practical application of the Ni-rich cathode materials [5-8].

Compared to NCM523, NCM811 is more susceptible to atmosphere as NCM811 is a fairly hygroscopic material [9]. The residual lithium compounds such as LiOH and Li2CO3 originate from spontaneous surface reduction with moisture and air are strongly related to the safety issue and battery performance [10-14]. Li2CO3 is responsible for the gas generation which may be arise from the decomposition reaction with electrolytes when charged to high voltage (>4.1V) in the cell [15-17]. On the other hand, LiOH will increase the pH value thus causing the gelation of the slurry during the electrode fabrication process [3]. Hence, the washing process was adapted to remove the residual lithium compounds of Ni-rich cathode. Although washing process greatly reduce the residual lithium compounds and pH value, the direct contact with water will facilitates the phase transition from the layered structure to the NiO like structure which shows no electrochemical activity [18]. The degradation of surface is fatal to the electrochemical performance and practical application of Ni-rich cathodes [19-21].

Recently, Kim et al. report the quaternary layered Ni-Rich cathode which maintain the specific capacity and excellent cycling stability [22, 23]. In addition to the suppression effect of Al-doping during the H2-H3 phase transition, the substitution of Al element greatly reinforces the surface of cathode. However, quaternary layered Ni-Rich cathode still suffer from residual lithium compounds and few paper shows the battery performance of the NCMA cathode materials before and after washing process. In this paper, we report on the structure and electrochemical properties of NCMA and NCM before and after washing process by SEM, XRD, CV, EIS and galvanostatic cycle analysis.

Experimental Method

Materials Synthesis

The NCMA quaternary layered materials were synthesized by the solid-state method using LiOH (Ganfeng Lithium Co. Ltd), transition-mental hydroxide precursors Ni0.83Co0.12Mn0.05(OH)2 (GEM Co. Ltd.) as raw materials and a trance amount of Al2O3 (Sigma) was added as doping additive. The Ni0.83Co0.12Mn0.05(OH)2 precursor was mixed thoroughly with LiOH (Li:Ni+Co+Mn=1.02:1) and Al2O3 and then the mixture was calcined at 800℃ for 12h in oxygen. For comparison, the NCM cathode materials were synthesized by mixing LiOH and Ni0.83Co0.12Mn0.05(OH)2 precursor (Li:Ni+Co+Mn=1.02:1) and then calcined at 800℃ for12 h in oxygen.

The positive electrode material after sintering and crushing was mixed with purified water in a mass ratio of 1:1 and then stirred for 5 min. The materials were collected through filtering and finally dried at 120℃ in a vacuum oven, which were recorded as NCMAWD and NCM-WD, respectively.

Materials characterizations

The surface morphologies of the cathode materials were observed with the FEG250 scanning electron microscope produced by FEI Company. The test voltage was 5-15kv and the working distance was 10-11 mm. The phase and crystal structure of the materials were characterized by the XRD-7000 X ray diffractometer produced by Japan shimon using Cu-Ka radiation at 40kV. The scanning speed was 2°/min, and the 2 theta Angle was 15-75°.

The X-ray Rietveld refinement was performed by the General Structure Analysis Software (GSAS) package with the EXPGUI interface. The refining parameters included background coefficients, lattice parameters, peak shape parameters, the positional parameter of O (6c), the fractional factors of all Li, Ni, Co, Mn and Al [24-26].

Electrochemical measurement

Electrochemical properties of the cathode materials were evaluated using CR2032 coin-type half-cells. The prepared cathode materials were mixed with conductive carbon and polyvinylidene fluoride with a mass ratio of 80:10:10. Then all above materials were dissolved in N-methyl pyrrolidone solvent (NMP) and mixed uniformly using a ball mill. After mixing evenly, the uniform slurries were coated on the aluminum foil and dried at 120℃. Then the coated aluminum foil was punched into pellets with a diameter of 13 mm and dried in a vacuum oven for 8 h. Then the CR2032 coin-type half-cells were assembled in the order of battery shell (buttom), negative plate (lithium wafer), diaphragm, electrolyte, positive plate, reed, and battery shell (up) in a glovebox under argon atmosphere. The active mass loading was about 9 mg/cm2. The electrolyte was 1.0 M LiPF6 dissolved in a mixture of ethylene carbonate (EC), dimethyl carbonate (DMC), ethyl methyl carbonate (EMC) with the volume ratio of 1:1:1. The Discharge-charge tests were performed at the charge or discharge ratio of 0.5C on a LAND battery test system produced by Wuhan blue electric company. Cyclic voltammetry and AC impedance tests were carried out by the electrochemical workstation Solartron (1287+1260) with the scanning speed of 0.1 mV/s and voltage range from 3.1 V to 4.5 V for cyclic voltammograms test. The frequency range of AC impedance test was 0.01 Hz–105 Hz, and AC amplitude was 100 mV.

Results and discussion

Figure 1 shows the SEM images of pristine and washed powders of NCM and NCMA cathode materials. All of the powders display a spherical morphology and each spherical secondary particle is composed of an agglomerate of primary particles. The exquisite observation on the NCMA surface shows that edges and corners of particles became obscure and the primary particle size distributes larger compared to the pristine NCM which indicates more interact between the primary particles. In addition, the primary particles were found removed during the washing process as is marked in Figure 1c while no obvious defects were detected in NCMA powders. This implies that introducing of Al element into the NCM materials improves the spatially correlation of primary particles. Figure 2 shows the X-ray powder diffraction patterns of the samples. All of the samples exhibit a well-defined layer structure based on a hexagonal α-NaFeO2 structure with a R-3m space group without any impurity phases [27]. The clear peak splits of the (006)/(102) and (018)/(110) peaks are observed for all samples, indicating that all the samples have well-defined layered structures [28]. Rietveld refinement results shows that the Al element decrease the Li/Ni exchange from 1.9% (NCM) to 1.6% (NCMA).

Figure 3 shows the cyclic voltammetry analysis of all materials between 3.1 and 4.5 V (vs. Li/Li+) at a scan rate of 0.1 mV s-1 in the first cycle. It can be seen that the four materials have similar redox peaks at 4.16V/4.22V, which corresponds to the platform near 4.20V on the charge-discharge curve and represents the transformation between H2 and H3 of the hexagonal crystal phase. The redox peak at 3.71V/4.06V corresponds to the redox process of Ni2+/Ni4+ [29-31]. Tiny cathodic peaks P0 and P4 are observed at around 3.50V and then disappear in the subsequent oxidation process, which may be attributed to the irreversible decomposition of impurities at the electrode/electrolyte interface as no relative cathodic peaks are detected in the washed samples. As shown in the cyclic voltammetry curves, the overpotential between first redox peaks (ΔV) of NCM and NCMA are 0.350 V and 0.345 V, while the ΔV of NCM-WD and NCMA-WD are 0.353 V and 0.323V, respectively. The washing process decrease ΔV of NCMA-WD by 0.02 V, which indicates that the washing process will remove the residual lithium compounds on the material and increase the reversibility and reactivity of the cathode material. On the other hand, NCMWD shows larger overpotential than NCMA-WD which should be attributed to the stable effect of Al doping on the structure. CV curves present that the Al doping modify the surface of the powders and suppress the destruction of water.

capacities of NCM and NCMA of approximately 192 mAh g-1. However, NCM-WD and NCMA-WD show larger initial discharge capacity of 200.4 and 203.8 mAh g-1 which may be arise from the removing of impurity on the surface by washing process.

Figure 5 shows the cycle performances of all the materials, NCMA shows similar capacity retention with NCM while NCMA-WD shows greatly improved capacity retention compared with NCMWD. It should be noted that after washing process, both NCM-WD and NCMA-WD show superior capacity which may be arise from the remove of residual lithium compounds but the poor capacity retention of NCM-WD is derived from the structural instability of the material after washing process.

EIS spectra of samples has been measured after 1 cycle and 50 cycles as shown in Figure 6. The plots consist of two semicircles in the high frequency region. The semicircle at high frequency could be attributed to the resistance for Li ion migration through surface film (RSEI) and semicircle at high-to-medium frequency is assigned to the surface charge transfer process (Rct). The cathodes show similar surface film resistances, but the charge-transfer resistance, Rct, differed substantially depending on the treating process. The Rct value increased appreciably from the surface decomposition during washing process. Al element dramatically decrease the Rct which should be assigned to the surface stabilization of the Al element. In addition, the value for Rct of NCM gradually accumulated after 50 cycling and obviously vary from the NCMA although they have similar Rct after 1 cycle. As shown in Figure 5, NCMA-WD maintain the excellent ability of Li conduction after washing process while NCM-WD after 50 cycles shows tremendous Rct value compared with that of the pristine material for the structural degradation of surface during washing process.

Conclusion

We synthesized NCMA cathodes by high-temperature solid state method. The partial substitution of Ni with Al element can facilitate the growth of primary particles and improve the spatially correlation of primary particles which reduce the destruction of secondary particles during washing process. Optimal Al-doping reduce the overpotential of the cathode and retain the capacity of the material. Moreover, the EIS analysis shows that the Al-doping can retard structural degradation of surface and maintain the capacity retention during washing process. The NCMA cathode after washing process delivers a discharge capacity of 203.8 mAh g-1 at 0.2 C with an outstanding capacity retention of 94% after 50 cycles at 25°C. This proposed synthesis strategy demonstrates that an optimal doping method will immensely retain the electrochemical performance while reduce content of the residual lithium compounds during the washing process which promote industrial fabrication of cathode materials.

#For more information #https://lupinepublishers.com/chemistry-journal/archive.php #please click here #https://lupinepublishers.com/chemistry-journal/pdf/AOICS.MS.ID.000194.pdf #https://lupinepublishers.com/chemistry-journal/#Lupine Publishers #archive of organic and inorganic chemical sciences #li-on battery

2 notes · View notes

lupinepublishers · 2 years

Text

lupine publishers|A Novel 5-Bromoindolehydrazone Anchored Diiodo Salicylaldehyde Derivative as A Multifunctional Probe for Selective and Sensitive Detection of Tryptamine and F‒ Ions

A Novel 5-Bromoindolehydrazone Anchored Diiodo Salicylaldehyde Derivative as A Multifunctional Probe for Selective and Sensitive Detection of Tryptamine and F‒ Ions

Abstract A new indole based chemosensor, 2-((5-bromo-1H-indol-2-yl) methylene) hydrazono) methyl)-4, 6-diiodophenol (BHDL) has been developed for the selective and sensitive detection of biogenic tryptamine and F‒ ions. The binding affinity of probe BHDL towards F‒/tryptamine (TryptA) has been investigated by UV-visible/fluorescence spectroscopy. In the presence of TryptA, probe exhibits strong enhancement in an emission band at 433 nm and the band at 555 nm underwent a blue shift accompanied by a decrease in intensity by the inhibition of Excited State Intramolecular Proton Transfer (ESIPT) functioned on BHDL. Interestingly, complexation with F‒ ions as well triggers an enhancement in a fluorescence band at 430 nm with the concomitant disappearance of the emission band at 555 nm due to the inhibition of ESIPT and deprotonation process initiated by the hydrogen bonding complex formation. Further, Density Functional Theoretical (DFT) calculations have been performed to support the mechanism functioned on the probe BHDL in the presence of TryptA/F‒. Keywords: Chemosensor; BHDL; ESIPT; Tryptamine; Fluoride ion

Introduction Fluorescent detection of biological and environmentally important species has been a recent area of focus due to its potential application in pharmacology, physiology, and environmental production [1,2]. Initially, several fluorescent sensors have been developed [3,4] merely for the detection of metal ions because of the selective binding ability of metal ions in water. Over the past decades, detection of anions and neutral analytes using fluorescent molecular system have witnessed an explosive growth in par with cation sensing. In particular, the design of multifunctional chemosensors has gradually become a new research focus in which a single receptor can independently recognize two or more guest species with diverse spectral responses via same or different channels. Among various ions, fluoride, being a strong electronegative element can interfere with the number of enzyme systems and thus acts as an enzyme inhibitor. It is present in biological fluids tissues, especially in bone and tooth [5]. The effect of association between the elevated levels of fluoride in drinking water and skeletal fluorosis has been well documented [6-8]. On the other hand, fluoride can have a beneficial effect on human health by treating osteoporosis and protecting dental health [9-13]. Thus, the detection of F- is essential to minimize its direct effects on human health. Biogenic amines are nitrogenous organic bases or deaminated derivative of amino acids. The natural resource of biogenic amines are grapes, food, and beverages, they can be synthesized by fermentation or microbial decarboxylation of amino acids [14] and a major important component in the production of hormones, alkaloids, nucleic acids and proteins. Among various biogenic amines, [15-22] tryptamine (TryptA) is a natural derivative can influence multiple processes within the central nervous system such as sleep, cognition, memory, temperature regulation and behavior [23,24]. Hence the detection and quantification of TryptA is of particular importance as it possess a strong pharmacological effect. Among various traditional analytical methods, detection based on fluorescent sensors stands as an effective tool to explore ions and neutral species owing to their simplicity, high selectivity, sensitivity, and versatility [25-33]. Moreover, recognition of miscellaneous targets with a single receptor would lead to a faster analytical processing and potential cost reductions. It is therefore highly desirable to develop a sensor that selectively recognize both TryptA and F‒ over other competing anions/biogenic amines through different optical modes. Being the core structure of the great number of inhibitor [34,35] and drug molecules [36,37] indoles have attracted a great deal of attention amid the scientific community due to their significant role in biological activity. Most of the indole derivatives are fluorescent and this property has been successively utilized for the design of indole-based receptors for selective chemosensing of metal ions and anions [38-44]. Herein, we have synthesized a new indole based dual mode chemosensor BHDL by simple condensation method and it has been utilized for the selective and sensitive detection of TryptA and F‒ in DMSO/H2O (9:1, v/v) medium. The probe BHDL displays excellent ratiometric responses in absorbance and strong “turn-on” fluorescence responses upon addition of both TryptA/ F‒ ions, respectively. Experimental Section Materials and Methods All starting materials and reagents were purchased from Alfa Aesar, Sigma Aldrich, and used as received without further purification. The anions of Cl‒, Br‒, I‒, CN‒, H2PO4 ‒, HSO4 ‒, NO3 ‒, AcO‒ and F ‒ were purchased as their tetrabutylammonium salts from Sigma-Aldrich Pvt. Ltd. Different category of amines like azane, methylamine, dimethylamine, trimethylamine, phenylethylamine, spermidine, spermine, tyramine, cadaverine, serotonin, histamine, tryptamine, L-tryptophan, dopamine, putrescine, D-glucosamine, glycine were purchased from Sigma-Aldrich Pvt. Ltd. Silica gel-G plates (Merck)

were used for Thin-layer Chromatography (TLC) analysis with a mixture of petroleum ether and ethyl acetate as an eluent. 1H and 13C NMR spectra were obtained on a Bruker 300 MHz NMR instrument with TMS as internal reference using DMSO-d6 as solvents. Standard Bruker software was used throughout. 19F-NMR spectra were recorded at 293 K on BRUKER 400 MHz FT-NMR spectrometers using DMSO-d6 as solvents. Electro Spray Ionisation Mass Spectrometry (ESI-MS) analysis was performed in the positive/negative ion mode on a liquid chromatography-ion trap mass spectrometer (LCQ Fleet, Thermo Fisher Instruments Limited, US). Fluorescence microscopic imaging measurements were logged using Operetta High Content Imaging System (PerkinElmer, US). Synthesis of (Z)-5-bromo-3-(hydrazonomethyl)-1H- indole (BMI) The starting material BMI was prepared by the condensation between 5-bromoindole-3- carboxaldehyde (500 mg, 2.23 mmol) and excess of hydrazine hydrate in methanol (50 ml) for 5 h. The pale orange colored solid product was obtained by washed with ethyl acetate (yield 90 %).1H NMR (300 MHz, DMSO-d6) δ (ppm): 11.67 (s, 1H), 8.83 (s, 1H), 8.44 (s, 1H), 7.99 (s, 2H), 7.76 (s, 1H), 7.42 - 7.14 (m, 2H). 13C NMR (75 MHz, DMSO-d6) δ (ppm): 156.03, 136.63, 134.04, 127.10, 125.90, 124.83, 114.87, 113.98, 112.35. Synthesis of 2-((Z)-(((Z)-(5-bromo-1H-indol-3-yl) methylene) hydrazono) methyl)-4, 6-diiodophenol (BHDL). The probe BHDL was synthesized by condensation between precursor BMI (50 mg, 2.10 mmol) and 3, 5- diiodosalicylaldehyde (80 mg, 2.10 mmol) in methanol (50 ml) solution for 10 h. The orange-colored solid product was found and thoroughly rinsed with ethyl acetate. The pure solid product was obtained (yield 80 %). 1H NMR (300 MHz, DMSO-d6) δ (ppm):13.05 (s, 1H), 12.15 (s, 1H), 9.14 - 8.70 (m, 2H), 8.41 (s, 1H), 8.08 (t, 3H), 7.43 (d, 2H). 13C NMR (75 MHz, DMSO-d6) δ(ppm): 161.64, 160.07, 159.48, 158.24, 136.70, 135.90, 135.11, 133.41, 126.93, 126.26, 124.91, 121.60, 114.92, 114.48, 111.74, 111.16. MS (ESI): 591.60 (M-H). UV-visible and fluorescence titrations Sensing aptitude of BHDL towards different amines/anions in DMSO/H2O (9:1, v/v) system was investigated by absorbance and emission spectroscopy. Tetrabutylammonium salts of anions in dimethylsulfoxide were used throughout the studies. Optical mode analysis of BHDL was inspected with different amines like azane, methylamine, dimethylamine, trimethylamine, phenylethylamine, spermidine, spermine, tyramine, cadaverine, serotonin, histamine, tryptamine, L-tryptophan, dopamine, putrescine, D-glucosamine, and glycine. Absorption measurements were performed on JASCO V-630 spectrophotometer in 1 cm path length quartz cuvette with a volume of 2 mL at room temperature. Fluorescence measurements were made on a JASCO and F-4500 Hitachi Spectrofluorimeter with excitation slit set at 5.0 nm band pass and emission at 5.0 nm band pass in 1 cm × 1 cm quartz cell. Computational details Density functional theory (DFT) calculations were executed using Gaussian 09 program [45]. Further, to support the fluorescent enhancement of BHDL with tryptamine and fluoride ions, the optimized structures of BHDL, BHDL-TryptA and BHDL- F‒ were obtained by DFT-B3LYP method using 6-311G /LANL2DZ basis sets, respectively. Results and Discussion Synthesis of BHDL In the synthetic route, simple condensation between 5-bomoindole-3-carboxaldehyde and hydrazine hydrate in excess yieldsthe precursorBMIin the initialstep. Successively, condensation process sustained between BMI and 3,5-diiodosalicylaldehyde in methanol. Finally, the chemoreceptor moiety BHDL was obtained with good yield as depicted in Scheme 1. Further to confirm the probe BHDL via diverse analytical methods such as 1H and 13C NMR and ESI-MS spectroscopy (Figures 1-4). UV-vis and fluorescence studies of BHDL towards anions To investigate the interactions of receptor BHDL with anions, absorbance and fluorescence intensity changes have been

for more information about archive of organic and inorganic chemical sciences archive page click on below link

https://lupinepublishers.com/chemistry-journal/archive.php

for more information about lupine publishers page click on below link

https://lupinepublishers.com/index.php

#lupine publishers group #archive of organic and inorganic chemical sciences #fluorescence intensity changes

0 notes

lupinepublishers · 3 years

Text

Lipine publishers|Development and Qualification of an Assay Method for Deferoxamine Mesylate and p-SCN-DFO

Development and Qualification of an Assay Method for Deferoxamine Mesylate and p-SCN-DFO

Abstract A simple, colorimetric assay method has been developed for deferoxamine mesylate and a related bifunctional chelating agent, p-SCN-DFO. A classic back-titration is performed where an excess amount of a standardized zirconium solution is added to the chelating agent solution. The excess zirconium is then titrated with standard EDTA. A qualification study was undertaken to evaluate the integrity of the method. Accuracy, specificity, and precision were evaluated and found to be excellent. The method is traced back to an analytical primary standard thus avoiding the need to create and use compound-specific reference standards. Keywords: Zirconium; assay; p-SCN-DFO; titration; deferoxamine

Introduction An assay method is a typical quality control test for both raw materials and products in the pharmaceutical industry. It measures the amount of the target substance present in a material. Tracing an assay test to a primary standard lends a high degree of accuracy to the analysis. The reason is primary standards are extremely pure, stable, and have no waters of hydration. Over the years the American Chemical Society has defined several reagents as primary standards. Potassium dichromate and sodium oxalate are primary standards for redox titrations. Tris(hydroxymethyl)amino methane (TRIS) and Potassium hydrogen phthalate are acid-base primary standards. Calcium carbonate is a primary standard for chelometric titrations. Assay tests can also be traced to established reference standards. The United States Pharmacopeia (USP) [1] provides reference standards (RS) for official articles in the USP or National Formulary (NF). An RS is typically specified in a monograph for use in the Assay test or an Identification test. An RS is considered 100.0% pure for quantitative applications unless a calculation value for an adjustment is stated on the label. For example, if a specific HPLC purity test shows the purity of the RS is 98.1%, a multiplier of 0.981 must be incorporated into an assay test. USP RSs are available for purchase for legal metrology purposes. The USP states that per the International Vocabulary of Metrology, they are defined as reference standards [2]. There exists a United States Pharmacopeia (USP) monograph for Deferoxamine Mesylate (DFO) [3]. The drug substance is used to treat sudden iron poisoning. It is also used to treat high levels of iron because of numerous blood transfusions. The USP monograph for DFO describes an assay test that is based on the use of a reference standard (Deferoxamine Mesylate RS). There is great value when scientists on different sides of the world can test a product to the same standard. However, since RSs typically lack the chemical properties of a primary standard, assay tests that can be traceable to a primary standard are inherently superior. There is no USP monograph for the related bifunctional chelating agent, p-SCN-DFO. It does not fall under the “official article” definition by the USP [4] That is, it is not considered a drug product, drug substance, dietary ingredient, dietary supplement, excipient, compounded preparation, other ingredient, device, or part of a device. As a result, there is no USP reference standard. DFO and its derivatives (e.g., p-SCN-DFO) are used as raw materials for bioconjugations. They can be conjugated to a peptide or antibody. Both compounds are commonly considered raw materials, critical raw materials, or registered starting materials when used in conjugations. For quality assurance purposes, however, the regulations of a drug substance are commonly placed upon them. Regardless of how they are considered, having an assay test with an appropriate specification on the material is a good idea.

A second goal of this work was to incorporate the use of a standardized zirconium solution into the assay test. Both DFO and p-SCN-DFO can be attached to antibodies and peptides for PET imaging with Zr-89. [5-8] Use of standardized zirconium solution can then demonstrate the molecules’ ability to bind zirconium [9]. The last goal was to qualify the assay method. In the early stages of drug substance development, analytical methods must be based on sound science. When a higher degree of confidence in an analytical method is desired, the methods are qualified. Down the road, when the highest degree of confidence in methods is required, validation is undertaken. The ICH Guidance Document Q2(R1) contains strict requirements for what must go into validating an analytical method [10], the requirements for qualifying a method are not defined. In short, a qualified method is a subset of a validated method. It gives the user more confidence in the reliability of the analytical results [11]. Much debate can go into what subset is appropriate to carry out. Our decision and justification are discussed. Materials and Methods The following reagents were ACS grade: ZrOCl2-8H2O, DMSO, EDTA disodium salt, xylenol orange, nitric acid, calcium carbonate, and hydroxy naphthol blue. Calcium carbonate is a chelometric standard with an assay of 99.95-100.05% on a dried basis. Deferoxamine mesylate was purchased from Millipore Sigma. The compound p-SCN-DFO is available as catalog number B-705 from Macrocyclics Inc. Deferoxamine mesylate RS was purchased from the USP and is catalog number 1166003. Class A volumetric flasks and pipets were used for critical volumes. The quantities used were chosen to optimize the number of significant figures while minimizing the quantity of materials needed for the test.A single EDTA solution was prepared and used by all analysts. Any error associated with this solution preparation or standardization is imparted to all assay test results equally. The solution was standardized using the calcium carbonate chelometric standard after drying. Hydroxy naphthol blue was used as in indicator. A sharp color change from purple to blue denotes the endpoint. Strict instructions for carrying out a test can be found in the supporting information. The zirconium assay method that was developed is a classic back titration. Excess standardized zirconium solution is present in a solution of DFO or p-SCN-DFO. The excess zirconium is titrated with a standardized EDTA solution. Xylenol orange is used as the indicator. A sharp color change from pinkish orange to yellow denotes the endpoint. Based on the volume of EDTA, the concentration of zirconium, and the concentration of EDTA, an apparent formula weight of the original solid DFO or p-SCN-DFO can be calculated. The ratio of the theoretical value to the calculated formula weight can then give an assay value. Strict instructions for carrying out a test can be found in supporting information. Three zirconium solutions were prepared. Analyst one used zirconium solution number one to perform all his/her assay tests on DFO and p-SCN-DFO. Analyst two used zirconium solution two and so on. The titrator that was used was an SI Analytics TITRONIC Basic. The burette holds 20mL and can dose in 0.01mL increments. Since its purchase, the instrument has routinely been tested to meet a 0.5% RSD for dosing small and large volumes. Since the endpoint can be determined with the naked eye, the assay test is performed by manual dosing. However, the titration could be automated with the incorporation of a photo rode if desired. For a residue on ignition test, a crucible with cover was placed at 900°C for two hours to clean. Solid

ZrOCl2-8H2O was dried to obtain an easily weighable solid that had a formula of approximately ZrOCl2- 4H2O based on the results obtained. This solid was weighed in the crucible after cooling. The solid was placed in the furnace for a total of 4 hours. Assuming the residue that remains is pure ZrO2, the percentage Zr in the original solid can be calculated.

Results and Discussion Assay Method Many colorimetric methods have been developed over the years for the determination of zirconium including those in the presence of interfering ions. [12-20] No method was found in the literature that worked for our application. Hundreds of titrations with varying conditions were carried out before settling on the optimal conditions. The method has many of the hallmarks of an ideal colorimetric titration. The titration can be performed quickly (i.e., minutes) so there is no long wait for equilibrium to be achieved. The method is colorimetric so there is no need for a UV/VIS instrument to determine an endpoint. The method is a classic complexometric method that uses EDTA as titrant, so no precipitation/filtration steps are required. The method uses commercial ACS reagents, so no expensive fine chemicals are needed. Lastly, solution preparations are simplified to dissolving solids in aqueous/DMSO solutions. No tricky heating or transfer steps that can add error are needed. The final conditions developed for the DFO and p-SCN-DFO assay test are found in (Tables 1,2). Due to the limited solubility of p-SCN-DFO in water, its sample preparation differs slightly. Conditions in (Table 1,2) are considered the 100% level. The order of addition is critical to prevent the zirconium from turning into an unreactive form in solution. Thus, the solutions or solids must be added in order from top to bottom.Preparation of Zirconium Solution The preparation of solutions of many metal ions can easily be prepared from their chloride or nitrate salts. The preparation of zirconium solutions is not straightforward. Unlike some transition metals, zirconium does not form a simple aqua ion in solution. The aqueous speciation depends on several factors such as pH, concentration, and counterions. [21-25] This work does not attempt to identify what species exist in solution under the conditions employed. It was sufficient to demonstrate the conditions we used were repeatable when preparing solutions. It was critical to prepare a zirconium solution that can easily be prepared and standardized. Originally, a NIST-traceable zirconium standard was tested. These standards are commonly used for ICP quantification of zirconium. Despite their preparation in acidic solutions, we could not come close to the zirconium value listed on the certificate of analysis. The solution preparation of this standard is not reliable for our purposes. Instead, we decided to prepare our own solution from ACS grade chemicals. The best solution preparation was made by dissolving ZrOCl2-8H2O in 1.0N nitric acid. ZrOCl2-8H2O was chosen over ZrO (NO3)2-xH2O because the latter is difficult to dissolve in acid solutions. It can be dissolved in a reasonable time only after heating. ZrOCl2-8H2O, on the other hand, dissolves readily in acidic solutions. Nitric acid was chosen over hydrochloric acid. When zirconium solutions are prepared in hydrochloric acid, the titration endpoint takes minutes. While it is a sharp endpoint, each drop of titrant near the end takes minutes to discern if the endpoint was reached. Since not every analyst has the same amount of patience, the nitric acid solution preparation was chosen instead. As a result, endpoints are both sharp and immediate. Regarding acid content, 1.0N acid was optimal although 2N HNO3 was also acceptable. When zirconium solutions were prepared in 0.1N HNO3 or less, or in >2N HNO3, the endpoint was unclear. It was critical to verify all the zirconium in prepared solutions is in a form that can react with EDTA, DFO, and p-SCN-DFO. A residue on ignition (ROI) test was used as a separate method to verify the results of the titration.

Three sources of ZrOCl2-8H2O were used to prepare and standardize three solutions of zirconium. The same sources of ZrOCl2-8H2O were tested for ROI. The % Zr was calculated using both methods. The results agreed to ≤ 0.8% absolute. This is a very good agreement for the comparison of two different methods. Consequently, we believe all the zirconium in solution is available to take part in the reaction.

For more information about An archive of organic and inorganic chemical sciences archive page click on below link

For more information about lupine publishers page click on below link

https://lupinepublishers.com/index.php

#lupine publishers group #An archive of organic and inorganic chemical sciences #Despite their preparation

4 notes · View notes

lupinepublishers · 3 years

Text

Lupine Publishers|Phytochemical Screening and Proximate Analysis of Garlic (Allium Sativum)

Abstract

Natural products have been an integral part of ancient traditional medicine systems. The objective of the study was to investigate the phytochemical constituents and proximate composition of Garlic (A. sativum) extracts. The phytochemical screening of the Garlic for various phytochemical constituents was conducted using laboratory method. The proximate and mineral composition was determined using standard method. The qualitative phytochemical screening of Allium sativum aqueous and ethanol extracts indicated the presence of Alkaloid, terpenoids, flavonoids, steroid, phenol, Anthraquinones, saponin, tannin and glycoside. Quantitatively, Alkaloid was found to be the abundant constituent making about 7.2%, followed by Tannin and saponin constituting 4.8% and 4.3% respectively. The qualitative proximate composition of the bulb extract of Allium sativum bulb in g/100g showed the extract contain carbohydrate, protein, fats, fibre, moisture and ash while the quantitative analysis result was presented as carbohydrate with 66.00%, protein 16.23%, fats 2.44%, crude fibre 03.96%, moisture content 5.52% and ash content 05.85%. The mineral composition analysis of the bulb indicates the presence of calcium (23.40%), potassium (10.95%), magnesium (3.90%), zinc (0.44%), phosphorous (9.85%), iron (5.20%) and copper (0.05%). The presence of nutrients proves why A. sativum bulb can be used as food supplement.

Keywords: Antimony; Consciousness Energy Healing Treatment; The Trivedi Effect®; PXRD; Particle size

Introduction

Natural products have been an integral part of ancient traditional medicine systems, e.g. Chinese, Ayurvedic and Egyptian [1]. Over the years, they have assumed a very central stage in modern civilization as natural source of chemotherapy as well as amongst scientist in search for alternative sources of drugs. According to the World Health Organization [2], a medicinal plant is any plant which in one or more of its organs, contains substances that can be used for therapeutic purposes, or which are precursors for chemo-pharmaceutical semi synthesis. Such a plant will have its parts including leaves, roots, rhizomes, stems, barks, flowers, fruits, grains or seeds, employed in the control or treatment of a disease condition and therefore contains chemical components that are medically active [3]. Phytochemicals are bio-active chemicals of plant origin. They are regarded as secondary metabolites because the plant that manufactures them may have little need for them. They are naturally synthesized in all parts of the plant body; bark, leaves stem, root, flower, fruits, seeds, etc. i.e. any part of the plant body may contain active components [4].

Garlic (Allium sativum L.) is one of those plants that were seriously investigated over several years and used for centuries to fight infectious diseases [5]. It is belong to family Amaryllidaceae [6]. It is a cultivated food highly regarded throughout the world. Garlic is originally from Central Asia, and as one of the earliest of cultivated plants [7]. Therapeutic use of garlic has been recognized as a potential medicinal value for thousands of years to different microorganisms. For example; antifungal, antiviral, antibacterial antihelmantic, antiseptic and anti-inflammatory properties of garlic are well documented. Moreover, garlic extracts exhibited activity against both gram negative (E. coli, Salmonella sp. and Citrobacter Enterobacter, Pseudomonas Klebsiella) and gram positive (S. aureus, S. pneumonia, streptococcus and Bacillus anthrax) all of which are cause of morbidity worldwide [8].

In Africa, particularly in Nigeria, it is used to treat abdominal discomfort, diarrhea, otitis media and respiratory tract infections [9]. In Europe and India, it was used to treat common colds, hay fever and asthma [10]. In addition to its reputation as a healthy food, garlic has shown anti-viral, anti-bacterial, antifungal and antioxidant capacities. Additionally, anti-atherosclerotic and anti-cancer properties have also been demonstrated. Many researches had demonstrated its effectiveness and broad spectrum antimicrobial activity against many species of bacteria, viruses, parasites, protozoan and fungi [9]. Garlic extract inhibits the growth of Gram positive and Gram negative bacteria, such as Staphylococcus, Streptococcus, Micrococcus, Enterobacter, Escherichia, Klebsiella, Lactobacillus, Pseudomonas, Shigella, Salmonella, Proteus, and Helicobacter pylori [11]. The objective of the present study was to investigate the phytochemical constituents and proximate composition of Garlic (A. sativum) extracts.

Materials and Methods

Sample collection and identification of Garlic bulb

Fresh bulbs of Garlic Allium sativa (Family Amaryllidaceae) were purchased from Kano main Market in Kano city, Nigeria. Identification and authentication of the Garlic was done at Herbarium in the Department of Plant Science, Bayero University Kano with the following voucher number BUKHAN 297. Voucher specimens were deposited in the Herbarium for reference.

Preparation of extracts

The collected bulbs were washed with distilled water, air dried for two weeks and grounded into fine powder using sterile pestle and mortar under laboratory condition. Fifty (50) grams of the powder was mixed with 500ml of Distilled water and ethanol in a sterile conical flask separately and stand for 3 days with intermittent shaking. The mixtures were filtered using filter paper and concentrated in water bath at 70 °C for 3 hours. Each extract was kept in a sterile container and refrigerated at 4 °C for further experiment.

Phytochemical screening

The phytochemical screening of the Garlic for various phytochemical constituents such as terpenoids, flavonoids, alkaloids, reducing sugars, steroid, glycoside, phenol, Anthraquinones, saponin and tannin was conducted using standard methods as described by Sofowora [12] and Trease and Evans [13].

Quantitative phytochemical analysis

Different methods were used in evaluating the quantity of phytochemical constituents of the plant materials used. Spectrophotometric method was used to determine Terpenoids, tannins, steroids, anthraquinone, and glycosides. Folin-Ciocalteu procedure was used to determine phenol content. Flavonoids, alkaloids and saponins were determined by the methods described by Adeniyi et al. [14].

Proximate analysis

Proximate analysis of the Moringa leaves was conducted to determine the ash content; crude protein, crude fibre, crude lipid, carbohydrate and dry matter using methods described by Udo and Oguwele [15]; James [16] and Association of Official Analytical Chemist (AOAC) [17]. The proximate parameters were expressed in percentage (%).

Mineral analysis

The mineral composition of the leaves including potassium (K), calcium (Ca), magnesium (Mg), and zinc (Zn), phosphorous (P) and iron (Fe) were determined using the atomic absorption spectrophotometer, as described the methods of AOAC [17]. Phosphorus was determined colorimetry method.

Results

Go toPhytochemical screening

The qualitative phytochemical screening of Allium sativum aqueous and ethanol extracts is presented in Table 1. The result indicated the presence of Alkaloid, terpenoids, flavonoids, steroid, phenol, Anthraquinones, saponin, tannin and glycoside.

The qualitative phytochemical screening of Allium sativum extracts is presented in table below (Table 2). Quantitatively, Alkaloid was found to be the abundant constituent making about 7.2 %, followed by Tannin and saponin constituting 4.8 % and 4.3 % respectively.

Proximate analysis

The qualitative and quantitative proximate analysis of Allium sativum bulb is presented in the table below (Table 3). The qualitative proximate composition of the bulb extract of Allium sativum bulb in g/100g showed the extract contain carbohydrate, protein, fats, fibre, moisture and ash while the quantitative analysis result was presented as carbohydrate with 66.00%, protein 16.23%, fats 2.44%, crude fibre 03.96%, moisture content 5.52% and ash content 05.85%

Mineral analysis

The mineral analysis of Allium sativum bulb is presented in Table 4. The mineral composition analysis of the bulb indicates the presence of calcium (23.40%), potassium (10.95%), magnesium (3.90%), zinc (0.44%), phosphorous (9.85%), iron (5.20%) and copper (0.05%).

Discussion

The results of the present study suggested that several phytochemicals are present in Allium sativum bulb extracts. Phytochemicals give plants their colour, flavour, smell and are part of a plant`s natural defense system and protect them against herbivorous insects and vertebrates, fungi, pathogens, and parasites [18]. The phytochemicals saponin, flavonoid, tannin, reducing sugar, steroid, and terpenoid were present in Allium sativa extracts according to this study. The phytochemical content of the extract of A. sativum revealed that the Alkaloids was found to be the most abundant phytochemical (7.2 %) followed by tannin (4.8 %), saponin (4.3 %) and flavonoids (2.18 %).

Based on the finding of this study, terpenoid is present in the both the extracts. Terpenoids have been found to be useful in the prevention and therapy of several diseases, including cancer. Terpenoids are also known to possess antimicrobial, antifungal, antiparasitic, antiviral, anti-allergenic, antispasmodic, antihyperglycemic, anti-inflammatory and immunomodulatory properties [19]. Flavonoids are also present in the extracts as a potent water-soluble antioxidant and free radical scavenger, which prevent oxidative cell damage and also have strong anticancer activity [20]. It also helps in managing diabetes induced oxidative stress. Steroids are importance in pharmacy as they possess compounds like sex hormones and can be used for drug production [21]. Tannin and saponin were present in the extract. Saponins protect against hypercholesterolemia and antibiotics properties. In addition, it has been found that saponins have antitumor, antioxidant and anti-mutagenic activities and can lower the risk of human cancers by inhibiting the growth of cancer cells [22]. The growth of many fungi, yeast, bacteria and viruses was inhibited by tannins [23]. The finding of this study correlate with the finding of Abaoab et al. [24] which found that clove extract possessed a broad spectrum of antimicrobial activity exhibited for both bacteria and fungi due to presence saponin, tannin, flavonoid and terpenoid. The result of this study on Phytochemistry of Garlic supported the study conducted by Deresse [8] who found that garlic extracts exhibited activity against both gram negative (E. coli, Salmonella sp, and Citrobacter Enterobacter, Pseudomonas Klebsiella) and gram positive (S. aureus, S. pneumonia, streptococcus and Bacillus anthrax) due to presence of some phytochemicals such saponin and tannin.

The results of the present study indicate that the qualitative proximate composition of A. sativum bulb contain carbohydrate, protein, fats, fibre, moisture and ash while the quantitative analysis result was presented as carbohydrate with 66.00%, protein 16.23%, fats 2.44%, crude fibre 03.96%, moisture content 5.52% and ash content 05.85%. This indicated the higher content of carbohydrate when compared to the rest. The higher carbohydrate content may be useful in making A. sativum bulb a good source of energy for the body. The presence of moisture, ash, lipid and protein in A. sativum bulb suggests that it may be useful for body building, prevention of ageing while the high dietary crude fibre content will help in bowel movement. This important nutrients composition in A. sativum bulb provides a justification that the bulb could be used as food supplement. Finding of this study indicated low fat content in A. sativum bulb, and low fat foods are known to reduce cholesterol level [25]. This result was inconformity with that of Harsh et al. [26].

According to the result of this study, the mineral analysis of Moringa leaf extract contained some important essential minerals such as; calcium (23.40%), potassium (10.95%), magnesium (3.90%), zinc (0.44%), phosphorous (9.85%), iron (5.20%) and copper (0.05%). The presence of such minerals in A. sativum bulb could be utilized as a nutritionally valuable and healthy ingredient for food. The mineral elements contained in these spices are very important in human nutrition. Sodium, potassium, calcium and magnesium play a central role in the normal regulation of blood pressure [27]. They could also be valuable in improving immune system and preventing malnutrition related diseases. Mineral elements are required for normal growth, activities of muscles and skeletal development (such as calcium), cellular activity and transport of oxygen (copper and iron), chemical react ion in the body and intestinal absorption (magnesium), fluid balance and nerve transmission (sodium and potassium), as well as the regulation of acid-base balance (phosphorus). Iron is useful in prevent ion of anemia and other related diseases [28]. Manganese plays a role in energy production and in supporting the immune system while zinc is useful for protein synthesis, normal body development and recovery from illness [29].

Conclusion

Based on the findings of the present study, phytochemical constituents, proximate and minerals components of A. sativum bulb were determined. The phytochemical components of A. sativum bulb contain alkaloid, saponins, flavonoids, glycoside, anthraquinones, tannin and terpenoids. The results of the proximate and mineral analyses of the whole leaf indicated the presence of considerable amount of nutrients. The presence of the phytochemicals has authenticated its usefulness by traditional herbalists in ethno medicine and potentials in drug formulation and development. In addition to that, the presence of nutrients proves why A. sativum bulb can be used as food supplement.

#For more #Information #https://lupinepublishers.com/chemistry-journal/archive.php #Please click here #https://lupinepublishers.com/chemistry-journal/#Lupine publishers #ARCHIVES OF ORGANIC AND INORGANIC CHEMICAL SCIENCES #Antimony

2 notes · View notes

lupinepublishers · 3 years

Text

Lupine Publishers | Chloride-Induced Highly Active Catalyst for Methyl Esterification of Alcohols

Lupine Publishers | ARCHIVES OF ORGANIC AND INORGANIC CHEMICAL SCIENCES

Abstract

In this work, a series of active Au/NiOx catalysts were successful to prepare by tracing the concentrations of chloride in the re-dispersed aqueous solutions. By characterizations, we found that the appropriate amount of residual chloride in Au catalyst would induce Au nanoparticles (Au NPs) to locate on the edges of NiOx particles, which resulted in the active Au/NiOx-9 sample. Fine control of chloride in the aqueous solution provides a new perspective to push for addressing the controllable preparation of active heterogeneous catalysts.

Keywords: Au catalyst, Preparation, Chloride, Esterification

Introduction

In recent decades, Au catalysts have received growing attentions and been widely applied in many important research fields [1], since good performance of Au catalysts was discovered [2]. However, the controllable preparation of highly active heterogeneous catalysts is still a longstanding challenge till now, especially Au catalysts. Many efforts have been devoted to this problem. The active site, structure and the quantum size effect of Au catalyst [3], active oxygen species of the support [4], suitable reducible oxide supports [5],and so on, have been extensively studied. Additionally, catalyst precursors, bases, pH value, aging time, and calcinations temperature are also crucial conditions [2,6]. Nevertheless, the controllable preparation of highly active Au catalyst is still difficult to realize even strictly following all above conditions. Chloride (usually as Cl-) is generally regarded as a poison for Au catalyst, Because of strong interaction of chloride and Au. We realized the reproducible preparation of Au/Fe2O3 catalyst for CO oxidation [7]. It is meaningful to explore whether this method can be applied to other catalysts and reactions or not. In this work, Methyl esterification of alcohols was chosen as model reaction. The controllable preparation of highly active Au/ NiOx catalyst was realized by tracing the concentrations of chloride in the re-dispersed aqueous solutions.

Experimental Details

Au/NiOx catalyst preparation

20ml Ni(NO3)36H2O (0.011 M) and 1.05 ml HAuCl4 (0.24M) were mixed together and were drop wise added into 60 ml Na2CO3 solution (0.31M) under vigorous stirring in 3h. The turbid liquid was divided into four sections and separation by centrifugation. Each section of the recovered precipitate was re-dispersed in different amount of deionised water and ultrasonically washed for 1h. The chloride concentration in the re-dispersed aqueous solution of each section was determined by CHI660D electrochemical workstation. Then, the solid was separated by centrifugation, dried at 80o C for 3h and calcined at 350 oC for 0.5 h to produce the catalyst sample, which was denoted as Au/NiOx-X, in which X suggested the chloride concentration in ppm.

Catalyst activity test

1mmol benzyl alcohol, 30 mg catalyst and 2 ml methanol were added into a glass tube. And then it was exchanged with oxygen and reacted at 60o C (1 atom, O2 balloon). After reaction, it was cooled to room temperature. Biphenyl was used as internal standard and a certain amount of ethanol were added into the reaction mixture up to 10mL for quantitative analysis by GC-FID (Agilent 7890A).

Results and Discussion

The catalytic activities of 15 Au/NiOx samples, which were prepared from the re-dispersed aqueous solutions with chloride concentrations in the range of 2 to 108 ppm, for esterification of benzyl alcohol were studied. According to the results shown in Figure 1, catalytic activity of Au/NiOx varied with the changing of chloride concentration. The yields of methyl benzoate were lower than 21% if the catalysts were prepared from aqueous solutions containing >22ppm chloride. More active catalysts were produced when the chloride concentrations were going down. The Au/ NiOx catalysts with the highest catalytic activity were prepared from aqueous solutions containing 8-13ppm chloride, the yield of methyl benzoate of catalyst Au/NiOx-9 was >99%. Surprisingly, the catalysts turned less active again when the chloride concentrations were < 8ppm. Typically, the yield of methyl benzoate was 20% with catalyst Au/NiOx-3.

TEM measurement results of Au/NiOx are shown in Figure 2. Their TEM images were similar and seemed amorphous. For the sample of Au/NiOx-22, the lattice of gold could be observed and wrapped in NiOx particle. For active Au/NiOx-9, the most of Au NPs connected with the edges of NiOx particles or the junctions of several NiOx particles [8]. In consideration of the best catalytic performance of this sample, this observation strongly supported the former results about active site in Au catalyst, i.e. the interface between Au and iron oxide [3]. It suggested that the appropriate amount of chloride might act as the linkage between Au NPs and the edges of NiOx particles to gain the active Au catalyst, For Au/ NiOx-22 and Au/NiOx-3, too much or less chloride was presented, the interaction of Au NPs and NiOx like Au/NiOx-9 decreased significantly. Accordingly, the catalytic activity lost sharply. By metering more than 150Au NPs, the mean diameters of Au NPs in samples Au/NiOx-3, Au/NiOx-9 and Au/NiOx-22were 4.1, 3.8 and 6.6 nm with 1.91, 1.84 and 3.06 standard deviations. The size distributions of Au NPs in Au/NiOx-3 and Au/NiOx-9 samples were extremely similar. The marked difference of catalytic activities of these two catalysts did not come from the size effect of Au particles, but the contact way of Au NPs and NiOx supports.

At present, there is still not sufficient evidence to explain the real role of chloride in the formation of Au catalysts. However, according to the known evidence, we can make some reasonable conjectures. Firstly, as pH value of the mother aqueous solution rises, chlorine in chloroauric acid is substituted by the hydroxyl. Au-Cl bond breaks and then small Au NPs form. Finally, chloride is adsorbed on the support NiOx as well as Au NPs. Due to the stronger interaction of chlorideon the edges than on planes of NiOx crystallites, after the ultrasonication and washing operations, chloride located on the edges of NiOx crystallites remains. As shown in Figure 3, it is this kind of residual chloride that induces Au NPs to anchor on the edges of NiOx crystallites.

Conclusion

In summary, by tracing the chloride concentrations in the re-dispersed aqueous solution, we successfully prepared active Au/NiOx catalyst for catalytic methyl esterification of alcohols. If the chloride concentration was not in the range of 8-13ppm, the catalytic activity dropped dramatically. These results indicated that the presence of appropriate amounts of residual chloride was beneficial to obtain highly active heterogeneous catalysts. This work can offer a new perspective to realize the controllable preparation of active heterogeneous catalysts

For More ARCHIVES OF ORGANIC AND INORGANIC CHEMICAL SCIENCES

https://lupinepublishers.com/chemistry-journal/

https://lupinepublishers.com/chemistry-journal/fulltext/chloride-induced-highly-active-catalyst-for-methyl-esterification-of-alcohols.ID.000154.php

#lupine publishers #Chemical Sciences #Chloride

7 notes · View notes

lupine-publishers-aoics · 3 years

Text

Lupine Publishers | Phytochemical and Antimicrobial Screening of the Leaves of Crotalaria Lachnosema Against Staphylococcus Aureus, Salmonella Typhi, Escherichia Coli and Klebsiella Pneumoniae

Lupine Publishers | An archive of organic and inorganic chemical sciences

Abstract

The leaves of Crotalaria lachnosema were freshly collected, dried under-shade and ground into powder. The ethanolic extract of the sample was obtained by cold extraction and was fractionated with solvent of varied polarity. The fractions were analyzed for their phytochemicals and screened antimicrobial against Staphylococcus aureus, Salmonella typhi and Escherichia coli. The phytochemicals were distributed among the test fractions. Tannins were found to be present in all the fractions and methanol fraction contains all the other tested phytochemicals except alkaloids and cardiac glucosides. The activities of the fractions were found to be more pronounced against E. coli than against the other test organisms.

Keywords: Phytochemical Screening; Antimicrobial; Crotalaria lachnosema; Staphylococcus aureus; Salmonella aureus; Salmonella typhi; Escherichia coli; Klebsiella pneumoniae

Introduction

For many centuries, man explores and utilizes the natural endowment offered by both the species of flora and fauna to provide the basic necessity of life such as clothing, shelter, food and indeed health care. Medicinal plants are the richest and commonest natural resource used in traditional medicine. Of the 250, 000 higher plant species on earth, more than 80,000 are medicinal [1]. Although plants had been priced for their medicine, flavoring effect and aromatic qualities for centuries, but the synthetic products of the modern age had for some time surpassed their importance. However, the blind dependence on synthetics is over and people are returning to the naturals with hope of safety and security [1]. The development of drug resistance in human pathogens against commonly used antibiotics has necessitated a search for new antimicrobial substances from other sources including plants [2]. Many reports have attested the efficacy of herbs against microorganisms, as a result, plant is one of the bedrocks of modern medicine to attain new principles [3]. The therapeutic properties of plants may not be unconnected to the variety of chemical substances biosynthesized by the plants as “secondary metabolites’’ that bring about definite physiological action in the human body. The most important of these bioactive constituents of plants are alkaloids, tannins, flavonoids, saponins and etc. [4]. Presently many governments and major health institutions including the World Health Organization [5] have recognized, pharmacologically validated and improved many traditional herbal medicines and eventually integrated them in formal health care system [1]. Thus, in light of the evidence of rapid global spread of resistant clinical isolates, the need to find new antimicrobial agent is of paramount importance. However, the past record of rapid, widespread emergence of resistance to newly introduced antimicrobial agents, indicates that even new families of antimicrobial agents will have a short life expectancy [6]. For this reason, researchers are increasingly turning their attention to herbal products, looking for new leads to develop better drugs against MDR microbe strains [7].

Crotalaria lachnosema belongs to the family Fabaceace (Leguminoseae), sub-family Papilionoideae. It is a woody plant with a height of about 2 cm high. The plant is known as ‘Fara birana’ in Hausa, ‘komp’ in Yoruba, ‘Ake dinwo’ in Ibo and Birjibei in Fulani [8]. The genus Crotalaria is widespread in the tropics and subtropical region and has about 550 species [9]. C. lachnosema was found to be important in the treatment of scabies. The whole plant grounded and mixed with water are fed to animals to treat liver disease [8]. The presence of resins and balsams might support the use of the plant as emollient as well as for treatment of sore throat, rheumatism, wounds and burns. Since some basalms and resins has antiseptic properties [3]. Few species of Crotalaria have been assessed against some pests. For example, under greenhouse condition, C. retusa and C. juncea have been found to be resistant to attack by the nematode, Pratyylenchus zeae and also that C. retusa has shown a higher degree of resistance to attack by the nematode, Rotylenchus rnifirmis Linford and Olivera. It was also reported that, the non-polar extract of C. retusa contain some active ingredients for controlling flea beetle a pest on okro plant. So, could be useful in pest management [10].

Materials and Methods

Sampling and Sampling Sites

The leaves of Crotalaria lachnosema were freshly collected on 4th July 2011 at an uncultivated land in Damanko village about 9km west of Zaria main town, Zaria Local Government, Kaduna State. The plants were identified and authenticated by Mallam Umar Shehu Galla of the Herbarium unit, biological science, Ahmadu Bello Univesity, Zaria. The leaves of the plant were dried under-shade for seven days and ground into powder using clean pestle and mortar.

Extraction and Fractionation of Plant Materials

Cold extraction (Percolation) was adopted in this research, this is part of the appropriate measure to preserve constituents that may potentially be active and retain their original identities in the course of preparing the extract [11]. 200g of the powdered plant sample was weighed and sucked in1000cm3 of ethanol for 14 days. The crude extract was prepared by decantation, filtration and concentration of the filtrate using Rota vapor machine (RVO) at 400C and finally by drying the concentrated crude ethanol extract. Fractions of various degrees of polarities were obtained from ethanol extract by macerating the ethanol extract with different solvents in sequence starting with solvent of least polarity to the one of highest polarity [12]. For the fractionation, 30cm3 of n-hexane was poured into the beaker that contained the dried and gummy ethanol extract and stirred for 5minutes and the liquid portion was then drained into another cleaned and empty beaker. This process was repeated until a clear solution was obtained at the end. The entire procedure was repeated with other solvents in the series; chloroform, ethyl acetate and methanol. Four fractions were thus obtained from the exercise and were labeled as followed: n-hexane fraction, chloroform fraction, ethyl acetate fraction and methanol fraction.

Phytochemical Screening of Plant Sample

The phytochemical analyses of the fractions were conducted by subjecting the fractions to different standard confirmatory tests. This is to determine the presence of certain phytochemical classes.

Test for Alkaloids: Each fraction (0.5g) was stirred with 5ml of 1 percent aqeous hydrochloric acid on a steam bath; 1ml of the filtrate was treated with a few drops of Mayer’s reagent and a second 1ml portion was treated similarly with Dragendoff’s reagent. Turbidity or precipitation with either of these reagents was taken as evidence for the presence of alkaloids in the extract being evaluated [13].

Test for Saponins: Each fraction (0.5g) was shaken with water in a test tube. Frothing which persists on warning confirmed the presence of saponins [14].

Test for Tannins: Each fraction (0.5g) was stirred with 10ml of water. This was filtered, and ferric chloride reagent was added to the filtrate, a blue-black precipitate indicated the presence of tannins [15].

Test for Flavonoids: A portion of each fraction was heated with 10ml of ethylacetate over a steam bath for 3mins. The mixture was filtered and 4ml of the filtrate was shaken with 1ml of dilute ammonia solution. A yellow colouration indicated the presence of flavonoid.

Test for Reducing Sugar: 1ml of each fraction was taken in five separate test tubes. These were diluted with 2ml of distilled water followed by addition of Fehling’s solution (A+B) and the mixtures were warmed. Brick red precipitate at the bottom of the test tube indicated the presence of reducing sugar [16].

Test for Cardiac Glycosides: 2ml of each fraction was placed in a sterile test tube. This was followed by adding 3ml of 3.5% iron III chloride (FeCI3), then 3ml ethanoic acid. This gave a green precipitate and a dark colored solution respectively. Finally, concentrated H2SO4 was carefully poured down the side of the test tub e which resulted in the formation of brownish red layer, at the interface. This confirms the presence of cardiac glycosides.

Antimicrobial Activity Test

Agar disc diffusion technique was adopted for the sensitivity test as described by [17].

Preparation of Test Fractions’ Concentration: Discs of about 6mm diameter were punched from Whatman’s No 1 filter paper using a paper puncher. Batches of 10 of the paper discs were transferred into vial bottles and sterilized in an oven at 1400C for 60 minutes. Stock solutions of 100mg/ml of the fractions were prepared by dissolving 200mg of each fraction in 2ml of DMSO (Dimethyl sulphoxide). By means of 1ml sterile syringe, 0.1ml, 0.2ml, 0.5ml and 1.0ml were transferred into labeled vial bottles preoccupied with 10 paper discs from a stock solution of each fraction and the solution were subsequently diluted with 0.9ml, 0.8ml, 0.5mland 0.0ml (i.e. without dilution) of DMSO that correspondingly resulted to 1mg/disc, 2mg/disc, 5mg/disc and 10mg/disc concentration. The prepared concentrations of the test fractions in the labeled bottles were kept in refrigerator until required for use.

Preparation of Inoculum from the Test Micro-Organisms: Staphylococcus aureus, Salmonella typhi, Escherichia coli and Klebsiella pneumoniae that were sourced from Microbiology unit of Aminu Kano Teaching Hospital (AKTH) Kano, were the microorganisms used for the research. The identities of the microorganisms were confirmed by standard biochemical test [18]. The test organism was cultured and maintained in a nutrient agar slant at 40C. The organism was then inoculated into nutrient broth and incubated overnight at 370C for 24 hrs. They were then diluted with normal saline until they give concentration of bacterial cells equivalent to 0.5 McFarland standard of Barium sulphate solution (1% v/v) [19].

Antibacterial Susceptibility Test (Bio Assay)

A suspension of nutrient agar (28g in 1000ml of distilled water) was prepared and autoclaved at 1210C for 15mins according to the manufacturers’ instruction. It was then carefully poured into sterile petri-dishes and allowed to solidify. The standardized inoculums of the bacteria were swabbed on the surface of the solid nutrient agar plates by means of sterile wire loop for the confluent growth of the bacteria. Four paper discs of 10mg/disc, 5mg/disc, 2mg/ disc, 1mg/disc concentrations were taken from the prepared test fraction solutions and were carefully and aseptically placed on the inoculated surface of the nutrient agar and a positive control disc (Tetracycline 1mg/disc) was placed at the centre of the plate. The plates were incubated inverted at 370C for 18 hours. The diameters of clear areas surrounding the discs where growths of the organisms were impeded (Zone of inhibition) were measured in millimeter and recorded. The assay was repeated two more times. The mean and the standard deviation (±SD) for the triplicate values were then calculated.

Results and Discussion

Tables 1-3 Mean of the triplicates ± S.D (standard deviation). A total ethanolic extract of 16.05g was produced from the 200g powdered plant sample. The highest percentage mass (63.05%) of the total mass macerated was methanol fraction and the least percentage mass (0.56g) was the pet. ether fraction. The result of phytochemical analysis revealed the availability of some secondary metabolites in the fractions of the plant sample. The presence of these secondary metabolite’s accounts for the activities of the plants. This complied with several reports by researchers that plants contain bioactive substances. Tannins were detected in all the fractions of the plant sample and tannins were reported to have various physiological effects like anti-irritant, anti secretolytic, antiphlogistic, antimicrobial and antiparasitic effect. Phytotherapeutically, tannins containing plants are used to treat non-specific diarrhea, inflammations of mouth and throat and slightly injured skins [20-22]. While cardiac glucosides which are used as lexative and carthatic drugs were confirmed in chloroform and ethyl acetate fractions. Alkaloids that were present in n-hexane and chloroform fractions act as antimalarial and anti-amoebic agents [22]. The antimicrobial sensitivity test result revealed a varied degree of activities exhibited by the fractions of the plant against the test organisms. Although, the plant sample exhibited low activities when compare to the control, the results show that activity of the different fractions may increase further if the concentrations of the fractions were to be increased. The result also showed that the activities of the plant fractions were comparatively more pronounced against E. coli than against S. aureus, S. typhi. and K. pneumoniae. With the exception of chloroform fraction that demonstrated some activities against S. aureus with zone of inhibition of 12mm at1000ug/disc all other fractions were inactive against S. aureus. However, n-hexane and ethyl acetate fractions exhibited low activities against S. typhi.

Conclusion

The activities of the fractions of the plant sample are more pronounced against E. coli than against the other test organisms. E. coli can cause diarrhea, urinary tract infections, respiratory illness, bloodstream infections and other illness. So, the plant leaves can be used in the treatment of the aforementioned illnesses. However, the relative low activities of the plant sample fractions against S. typhi and K. pneumoniae revealed its un-befitting nature as an antityphoid and anti-pnuemoniie drug.

Recommendation

The other parts of the plant should also be exploited. To harness its full medicinal potential, the plant sample fractions should be tested against other bacteria isolates and further research should be carried out to isolate and characterize the active compounds in the plant.

https://lupinepublishers.com/chemistry-journal/pdf/AOICS.MS.ID.000173.pdf

https://lupinepublishers.com/chemistry-journal/fulltext/phytochemical-and-antimicrobial-screening-of-the-leaves-of-crotalaria-lachnosema-against-staphylococcus-aureus.ID.000173.php

For more Lupine Publishers Open Access Journals Please visit our website: https://lupinepublishersgroup.com/

For more Open Access Journal on Chemistry articles Please Click Here: https://lupinepublishers.com/chemistry-journal/

To Know More About Open Access Publishers Please Click on Lupine Publishers

Follow on Linkedin : https://www.linkedin.com/company/lupinepublishers Follow on Twitter : https://twitter.com/lupine_online

#Lupinepublishers #Lupine publishers #Lupine Publisher Group #inorganic chemistry #organic chemistry

1 note · View note