Quality Of Dietary Supplements Research Articles

Development and validation of methodology of quantitative determination of sibutramine in dietary supplements by high performance liquid chromatography

Sibutramine is a highly effective drug for the treatment of obesity. In this regard, unscrupulous manufacturers can add sibutramine as a biologically active synthetic substance prohibited for use in the composition of dietary supplements. Thus, the problem associated with the illegal circulation of such dietary supplements is especially actual, given the scale of the sale of these products. The development and validation of methods for the determination of sibutramine in dietary supplements for slimming (anorexigenic action) for the purpose of quality control in order to ensure the quality of dietary supplements when introduced into civil circulation at customs and on the market. The aim of the study - to develop a method for the quantitative determination of sibutramin in dietary supplements for weight loss by high performance liquid chromatography (HPLC) and to validate it. Material and methods. For the quantitative determination of sibutramine in dietary supplements, we used an Agilent 1100 high performance liquid chromatograph with a UV-detector. The stationary phase was a chromatographic column C18 NUCLEOSIL 4.6×150 mm, particle size 5 μm. The mobile phase contained 0.05 M formate buffer pH 4.0 and acetonitrile in a ratio of 40:60 (by volume). Results and discussion. A methodology has been developed for the determination of sibutramine in dietary supplements for weight loss, which makes it possible to control the quality of dietary supplements. Based on the obtained chromatograms, the specificity was determined; the plant components did not influence the determination of sibutramine in model mixtures. The suitability of the chromatographic system was determined: the retention factor of the compound - 2.222 (more than 2.0), N - 5776 theoretical plates (more than 5000), T peak of sibutramine - 0.939 (not more than 1.5). Within the analytical area of the linearity method: R2=0.9993 (over 0.9950). ε=0.46% (does not exceed 1.5%), the confidence interval includes the value of 100%, the calculated value of the Student's criterion tcalc (2.47) was less than the tabular ttable (2.80), which proved the correctness of the methodology. The precision of the results was determined by the obtained RSD value, which was 0.91% (less than 1%). Limit of detection (LOD) and limit of quantification (LOQ) took values of 0.1 and 1.0%, respectively. The range of measured concentrations was 0.01-20.0 mg/g. Conclusion. As a result of the studies, the method for sibutramine determination in dietary supplements with anorexigenic action was tested and can be used in quality control of dietary supplements.

Quality of Dietary Supplements Containing Plant-Derived Ingredients Reconsidered by Microbiological Approach.

Dietary supplements cover a wide range of products, the most popular are those containing plant-based ingredients. Supplements are consumed by consumers of all ages as well as by both healthy and sick people. The lack of unified regulation in this sector increases the probability that supplements are poor chemical and microbiological quality and can be dangerous for patients. The aim of this paper is to highlight selected issues associated with the microbiological quality of dietary supplements containing plant materials. We focus on the most recent reports referring to bacterial and fungal contaminations as well as the presence of mycotoxins. Dietary supplements containing plant ingredients commonly show a variety of microbial contaminants, which might be crucial for consumer safety. They often contain microorganisms potentially pathogenic to humans. Metabolites produced by microorganisms may pose a threat to the health of consumers. Because of that, in this review, we emphasize the risk that may be associated with the lack of appropriate studies of the quality of the supplements.

Performance Comparison of Rapid Petrifilm™ Test Methods vs. Conventional Test Methods for Microbiological Testing of Dietary Supplements

Abstract Objectives The aim of this study is to show suitability of 3M™ Petrifilm™ across various types of common multi ingredient finished dietary supplement products. Methods In present investigation, parallel analysis and suitability was conducted using gold standard methods prescribed under U.S. Pharmacopeia general chapter dietary supplement ⟨2021⟩/⟨2022⟩, US FDA's Bacteriological Analytical Manual (BAM), and AOAC using 3M™ Petrifilm™. Five commonly used tests in food and dietary supplement quality testing were deployed in this study, namely: Total Aerobic Microbial Count (TAMC), Total Yeast and Mold Count (TYMC), Escherichia coli, Staphylococcus aureus, and Coliforms. Dietary supplements selected for this investigation are from most common types of dietary supplements categories sold in US market i.e., multivitamin and mineral, protein, multi mineral, Prenatal, Vitamin D, and Omega 3 Fish oil. Three individual lots of each of the five products were tested to increase robustness of data. Acceptance criteria was set same as USP ⟨2021⟩/⟨2022⟩ requirements, that is to demonstrate a greater than 70% recovery in comparison to a control. Results AOAC using 3M™ Petrifilm™ results show recovery of >70% compared to control for all five test Total Aerobic Microbial Count (TAMC), Total Yeast and Mold Count (TYMC), Escherichia coli, Staphylococcus aureus, and Coliforms: Multivitamin and mineral product recovery ranges were between 79%–111%, Protein product recovery ranges were between 94%–104%, Multi mineral product recovery ranges were between 94%–107%, Prenatal product recovery ranges were between 74%–117%, Vitamin D product recovery ranges were between 93%–123%, and Omega 3 fish oil product recovery ranges were between 83%–101%. Conclusions We found that AOAC based 3M™ Petrifilm™ methods are suitable for selected major categories of dietary supplement finished products. All results from AOAC using 3M™ Petrifilm™ microbiological testing achieved >70% bioburden recovery in comparison to a control. We also found that AOAC using 3M™ Petrifilm™ provides consistent and comparable results to USP ⟨2021⟩/⟨2022⟩/FDA's BAM results for the same samples as well. Funding Sources Reliance Vitamin.

An educational intervention improved knowledge of dietary supplements in college students

BackgroundWe have previously reported on the prevalence of dietary supplements among college students; it was deduced that their intake of supplements increased according to their grade (i.e., 13.1% in the first grade to 20.5% in the sixth grade). We also reported that some students had experienced adverse events in Japan due to their intake of these supplements. However, awareness of dietary supplements among college students remains limited, even among pharmaceutical students. Being appropriately educated about them is important for pharmaceutical students, both for themselves as well as for their future careers as pharmacists.MethodsWe conducted a lecture-based educational intervention about dietary supplements on 328 college students in Japan—184 from pharmaceutical science and 144 from environmental science or food and life science disciplines. The purpose of this study was to evaluate the effects of an educational intervention on college students’ understanding of dietary supplements. The intervention involved a lecture that covered the quality of dietary supplements, how they differed from drugs, and a summary of their adverse events. The lecture was evaluated using a 14-question questionnaire. We then compared the pre- and post-intervention responses to the same questionnaire using a Wilcoxon signed-rank test. The questions were assessed using a Likert scale that ranged from “strongly agree” to “strongly disagree”; the latter being the preferred answer.ResultsBefore the intervention had taken place, the students’ understanding of dietary supplements was shown to be deficient. Conversely, post-intervention, their knowledge levels had significantly improved, especially concerning agreement on whether “Dietary supplements are safe because they are just food items”. Pre-intervention, 2.7% strongly agreed and 37.5% agreed; post-intervention, 1.2% strongly agreed and 15.6% agreed. On whether “Dietary supplements made from natural ingredients or herbs are safe”, at the pre-intervention stage 2.8% strongly agreed and 44.0% agreed and post-intervention, 2.2% strongly agreed and 16.9% agreed. On whether “Dietary supplements made from food items are safe”, 4.0% strongly agreed and 43.6% agreed pre-intervention and 0.9% strongly agreed and 16.6% agreed post-intervention. Despite there being a greater number of pharmaceutical students who had a correct understanding of dietary supplements before the intervention, these students still showed improvement after the lecture.ConclusionAn intervention in the form of a single educational lecture has the capacity to improve college students’ understanding of dietary supplements. It is important for pharmacists to be appropriately educated about dietary supplements when they consult with patients. We will evaluate the long-term effects of the intervention on the alumni (pharmacists) in a subsequent study.

Features of standardization and registration of dietary supplements compared to drugs

The constant increase in the number of dietary supplements and the demand for them, as well as the progression of self-medication with the use of over-the-counter medicines, raises questions about their effectiveness, safety and bioequivalence. There are also questions about the criteria for ingredients, production, standardization and registration of finished medicines and dietary supplements.The aim. The aim of the work is to summarize information on the features of standardization, certification and registration of dietary supplements in comparison with drugs in the territory of Ukraine.Materials and methods. Data were collected and analyzed from the current scientific literature and regulatory documents to perform the research.Results. Production, standardization and circulation of finished medicines and dietary supplements is carried out in accordance with the current legislation of Ukraine, international standards (ISO, ICH, GxP) and the requirements of the State Pharmacopoeia of Ukraine. According to these documents, the requirements for the quality of medicines and dietary supplements differ, but unlike ten years ago, today there can be increased regulation and control on the part of the state and law enforcement agencies to eliminate cases of falsification and circulation of unregistered means.The current legislation of Ukraine regulating the production, quality and circulation of finished medicines harmonized with the EU puts forward requirements for providing the population with quality imported / domestic medicines. Regarding dietary supplements, the procedure of harmonization of the legislation of Ukraine with the EU has started, which in the future should lead to improvement of the quality of these remedies and increase of control from the state.Discussion. We generalized requirements for the features of standardization and registration of dietary supplements in the territory of Ukraine, which must be observed in the manufacture, quality control, registration and sale of dietary supplements.Conclusions. Simpler registration, implementation and wider market conditions (multi-level marketing system, Internet) lead to a rapid increase in the production of dietary supplements in Ukraine and their imports. We generalized information about the requirements for the quality of dietary supplements in comparison with finished medicines, and the features of their registration in the territory of Ukraine according to the current legislation

Biochemometrics and Required Tools in Botanical Natural Products Research: A Review.

This review serves to highlight the role of chemometrics and biochemometrics in recent literature as well as including a perspective on the current state of the field, as well as the future needs and possible directions. Specifically examining the analytical methods and statistical tools that are available to chemists, current applications of QTOF-MS, Orbitrap-MS, LC with PDA/UV detectors, NMR, and IMS coupled MS are detailed. Of specific interest, these techniques can be applied to botanical dietary supplement quality, efficacy, and safety. Application in natural products drug discovery, industrial quality control, experimental design, and more are also discussed.

Risks associated with sub- and overdosing of water-soluble vitamins in professional or amateur athletes and the quality of dietary supplements

Risks associated with sub- and overdosing of water-soluble vitamins in professional or amateur athletes and the quality of dietary supplements

High throughput dietary supplement quality control and pharmacovigilance

High throughput dietary supplement quality control and pharmacovigilance

Should states and local governments regulate dietary supplements?

Federal regulation of dietary supplements in the United States is governed by the Dietary Supplement Health and Education Act of 1994. The law has been criticized as weak and ineffective. Alarming research has emerged demonstrating that supplements may be mislabelled, contaminated, adulterated with dangerous or unknown compounds, or sold at toxic doses. As a result, the health community has raised concerns about the safety and quality of dietary supplements. Increased federal oversight is an important avenue for improving supplement safety; however, states and local governments may also pursue strategies to strengthen the overall regulatory control of dietary supplements. States and local governments have substantial experience in regulating other products that pose a risk to public health, such as tobacco. Additionally, much has been learned about the tactics the tobacco industry has employed to protect its interests. Lessons learned may be applied to new regulatory efforts aimed at improving the safety of dietary supplements at the state and local levels. Copyright © 2015 John Wiley & Sons, Ltd.

Too Little, Too Late: Ineffective Regulation of Dietary Supplements in the United States

Millions of people in the United States consume dietary supplements hoping to maintain or improve their health; however, extensive research has failed to demonstrate the efficacy of numerous supplements in disease prevention. In addition, concerns about the safety of routine and high-dose supplementation have been raised. The Food and Drug Administration regulates dietary supplement quality, safety, and labeling, and the Federal Trade Commission monitors advertisements and marketing; still, vast enforcement challenges remain, and optimal governmental oversight has not been achieved. If the composition and quality of ingredients cannot be reliably ensured, the validity of research on dietary supplements is questionable. Moreover, the health of the US public is put at risk.

Monokomponentni dijetetski suplementi folne kiseline na tržištu Republike Srbije - farmaceutsko-tehnološka ispitivanja i karakteristike

Introduction. Disintegration of the solid dosage form of dietary supplements and folic acid dissolution rate are of particular importance for its bioavailability. However, current legislation in the Republic of Serbia does not set criteria for the pharmaceutical technical quality of dietary supplements. The United States Pharmacopoeia, on the other hand, gives testing standards for disintegration, dissolution and weight variation of dietary supplements. Aim. The objective of this study was to investigate and compare pharmaceutical technical quality of solid dosage forms of dietary supplements marketed in Serbia, with regard to the United States Pharmacopoeia standards for dietary supplements and European Pharmacopoeia standards for solid dosage forms of pharmaceutical preparations. Methods. Seven monocomponent folic acid dietary supplements commercially available in Serbia, from which three uncoated tablets, three coated tablets and one hard capsules, were subjected, depending on the dosage form, to the weight variation, friability, hardness, disintegration and dissolution testing. Conclusion. The obtained results have shown that six out of seven investigated products complies with United States Pharmacopoeia standards for pharmaceutical technical quality of dietary supplements, while only one (hard capsules) failed to meet the requirements for disintegration.

Pyrazolopyrimidines in ‘all-natural’ products for erectile dysfunction treatment: the unreliable quality of dietary supplements

A herbal food supplement advertised as a potency pill was screened for the presence of PDE5 inhibitors. The resulting signals were characterised by UV, LC-MS in ESI-negative mode, and NMR spectroscopy using 1D and 2D experiments. Several substances were identified, bearing the basic chemical structure of sildenafil, but were not supposed to exhibit PDE5 inhibition. These compounds may be process-related impurities or by-products of different reaction steps in the synthesis of PDE5 analogues. As they were found to be present in different capsules at different concentrations, this is an example of the unreliable quality of dietary supplements.

Summit on Human Performance and Dietary Supplements Summary Report

The use of dietary supplements to enhance human performance among active individuals, athletes, the military, and other tactical populations is an increasingly popular topic that often is not well understood. There are important differences in nutrient needs between the general public and active adults. The United States has an established regulatory framework for dietary supplements, and the safety and quality of dietary supplements can be strengthened through education, third-party certification programs, and increased attention to serious adverse event reporting. This summary highlights these key issues, as well as research needs, areas for future consideration, and other topics that were discussed during the Human Performance and Dietary Supplements Summit, heldAugust 9 to 10, 2012, in Bethesda, Maryland. Nutr Today. 2014;49(1):7Y15 The use of dietary supplements to enhance human performance among athletes, the military, and other tactical populations is an increasingly popular topic that often is not well understood. To review the evidence base and discuss key issues, the National Strength and Conditioning Association, National Institutes of Health Office of Dietary Supplements, the American Society for Nutrition, and the EAS Academy hosted a Human Performance and Dietary Supplements Summit August 9 to 10, 2012, in Bethesda, Maryland (Table 1). More than 200 professionals from the medical, nutrition, and athletic performance fields, as well as the military, participated in the summit. This summary highlights the key topics covered, research needs, future study considerations, and discussion points as presented at the summit, without further elaboration. N T

Simultaneous Identification of Hydroxythiohomosildenafil, Aminotadalafil, Thiosildenafil, Dimethylsildenafil, and Thiodimethylsildenafil in Dietary Supplements Using High-Performance Liquid Chromatography-Mass Spectrometry

We developed a method for the separation and identification of illegal adulterants (hydroxythiohomosildenafil, aminotadalafil, thiosildenafil, dimethylsildenafil, and thiodimethylsildenafil) from dietary supplements using high-performance liquid chromatography-mass spectrometry. The separation was achieved on a C18 column: the mobile phase consisted of 5 mM ammonium formate (pH 6.3)-acetonitrile (75 : 25, v/v) and acetonitrile, with gradient elution at a flow rate of 0.2 mL/min. The proposed method could also be used to separate vardenafil, homosildenafil, and dimethylsildenafil, all of which have the same molecular weight. Furthermore, the proposed method could simultaneously separate hydroxythiohomosildenafil, aminotadalafil, thiosildenafil, dimethylsildenafil, thiodimethylsildenafil, vardenafil, and homosildenafil. Thus, this method may be useful to identify medicinal ingredients for erectile dysfunction and their analogs and to control the quality of dietary supplements.

Assuring dietary supplement quality for cancer patients: An integrated formulary systems approach.

e20663 Background: Studies reveal up to 80% of cancer patients use some form of dietary supplements (DS). Despite the need for additional research, evidence exists that some DS may be of clinical value. In order to provide safe DS recommendations to patients, we created a Dietary Supplement Formulary Committee (DSFC). Methods: Twelve manufacturers (marketing 19 DS brands) with a reasonable reputation among providers for quality were selected. A survey tool was created to measure critical quality, GMP and FDA compliance practices; information was obtained via non-disclosure agreements; manufacturing documents were audited and compared to survey responses; FDA audit reports were obtained under Freedom of Information requests; site audits were conducted; and third party analytical testing was performed. Results: All 12 companies claimed to be operating in full compliance with FDA regulations. However, 3 had received Warning Letters from FDA for GMP violations; 2 performed a product recall within the last 5 years; 4 reported products that failed Consumerlab.com for potency or purity; 1 did not have product specifications; 1 was found by FDA to have inadequate testing; 1 was found to have a lack of sufficient controls throughout the supply chain to guard against microbiological contamination; and 2 had confirmed melamine contamination or lack of melamine testing on protein powders. Additional concerns included the use of subcontractors for certain operations, lack of stability data to support expiration dates, material discrepancies between claims and actual practice, and failure to change UPC (Universal Product Code) numbers when active ingredient formulas change. Conclusions: We observed considerable variation in the quality of DS, and in the level of compliance, which raises concerns for patient safety. One company met all quality standards. The combined use of the measures described above allowed for informed product selection. The variable quality practices identified here emphasize the need for careful formulary oversight. The USP (United States Pharmacopeial Convention), ConsumerLab.com, and the NSF International’s certification programs are current resources available to help identify quality DS.

Botanical origin of dietary supplements labeled as “Kwao Keur”, a folk medicine from Thailand

In the course of our study on the quality of dietary supplements in Japan, both the internal transcribed spacer (ITS) sequence of nrDNA and the rps16 intron sequence of cpDNA of products labeled as "Kwao Keur" were investigated. As a result, the DNA sequence of Pueraria candollei var. mirifica, which is the source plant of Kwao Keur, was observed in only about half of the products. Inferred from the determined sequences, source plants in the other products included Medicago sativa, Glycyrrhiza uralensis, Pachyrhizus erosus, and Ipomoea batatas, etc. These inferior products are estimated to lack the efficacy implied by their labeling. In order to guarantee the quality of dietary supplements, it is important to identify the source materials exactly; in addition, an infrastructure that can exclude these inferior products from the market is needed for the protection of consumers from potential damage to their health and finances. The DNA analysis performed in this study is useful for this purpose.

Microbiological quality and safety of dietary supplements sold in Saudi<br>Arabia

The global market for dietary supplements has advanced in recent years capitalizing on the growing awareness of healthy living worldwide. Supplements provide enhanced nutritional levels for daily competitive performance. However, there is a need to explore the quality of dietary supplements as there are few studies related to this area. Therefore, the objective of this study was to determine the microbiological quality of dietary supplements in the local markets of Saudi Arabia. The total bacterial count, coliform, Escherichia coli, Salmonella, and Staphylococcus aureus were included in this analysis. The 80 most popular supplements were tested in this study. Our results showed that microbial contamination was present in only nine products. The microbial level ranged from 1.69–8.43 Log CFU/mL. The higher level of total count (8.43 Log CFU/mL) and S. aureus (8.39 Log CFU/mL) were found in supplement glutamine. Amino acids, dynamisan, glucosamine sulfate, glucosaiene, creatine monohydrate, whey protein, and folate acid also showed the presence of bacterial contamination. Our findings suggested that improvements are needed in these supplements which were tested for microbiological contamination. These findings highlight the fact that a review of product safety and quality is becoming increasingly important for consumer health. This will help to ensure safe products available for today’s savvy, health-conscious consumer.

Heavy Metal Contents in Registered Dietary Supplements in Malaysia: A Pilot Study from the Drug Safety Perspective

Objectives: In Malaysia dietary supplements are ram- pantly consumed for general health and well-being and therefore, available in community pharmacies, health food stores, night markets, grocery stores and even obtained via internet. However, gap in the level of Malaysian consumer’s awareness regarding the toxicity of dietary supplements is a major issue, which needs to be addressed by the analysis of their constituents. This study was aimed to evaluate and analyze the heavy metal contents such as lead (Pb), cadmium (Cd), arsenic (As) and mercury (Hg) in registered dietary supplements available in community pharmacies in Malaysia Methods: This study was focused on Eurycoma longifolia (Tongkat Ali), glucosamine, Allium sativum (garlic) and Zingiber officinale (ginger) products. A total of twenty registered single ingredient dosage form dietary supple- ments from different brands were purchased from com- munity pharmacies located in Penang. The samples were then evaluated and subjected to analysis by atomic absorption spectrometry. Results: The study showed that variable amounts of lead have been quantified as 0.29 -0.47 ppm (Tongkat Ali), 0.19 – 0.27 ppm (glucosamine), 0.01 – 0.38 ppm (garlic) and 0.26 – 0.74 ppm (ginger) products. While for cad- mium detection, the amounts indicated 0.02 – 0.24 ppm (Tongkat Ali), 0.03 – 0.22 ppm (glucosamine), 0.06 ppm (ginger) and was absent in garlic No traces of arsenic and mercury were found in all four product samples. The regression linear coefficients (r2) for Pb, Cd, As and Hg standards were 0.9990, 0.9958, 0.9960 and 0.9989, respectively. Conclusions: The amount of Pb, Cd, As and Hg in all the products were found within the limits as per the re- quirement stated by National Pharmaceutical Control Bureau (NPCB). Thus, in order to ensure the safety and quality of dietary supplements, the analysis of heavy metals must be carried out on routine basis using simple and robust atomic absorption spectrometry (AAS) technique

Fast CE analysis of adrenergic amines in different parts of Citrus aurantium fruit and dietary supplements

A CE method has been developed for the simultaneous analysis of the adrenergic amines synephrine, octopamine and tyramine in Citrus aurantium (bitter orange) fruit extracts and in dietary supplements. The analytes were separated on a fused silica capillary (50 microm id, 40.0 cm effective length, 48.5 cm total length) using a BGE composed of phosphate buffer (pH 2.5, 50 mM) and applying a 30 kV potential. The samples were injected hydrodynamically at 50 mbar for 25 s. The use of photodiode array detection (lambda=195 nm) allowed the quantification of the analytes and the control of peak purity. The method has been fully validated, obtaining satisfactory values of precision and extraction yield. The analytes are extracted with water from the dried whole fruits or fruit parts (endocarp, mesocarp and exocarp) or from the commercial formulations and directly injected into the CE apparatus. The results obtained were satisfactory in terms of precision (RSD < 5.7%) and accuracy (recovery > 89%). Thus, the method has demonstrated to be suitable for the qualitative and quantitative determination of synephrine, octopamine and tyramine in C. aurantium extracts, for dietary supplement quality control and for food adulteration identification.

Making Sense of Dietary Supplements: The Dietary Supplements Labels Database

ABSTRACT This article describes the Dietary Supplements Labels Database, a new resource from the National Library of Medicine that integrates information from dietary supplement manufacturers, government agencies, and clinical research into an easy-to-use interface. This database contains information on more than 2,000 brands of dietary supplement and more than 800 active ingredients. This resource will greatly assist consumers and health care providers in evaluating the safety, efficacy, and quality of dietary supplements. Features of the resource will be described as well as the browse and search methods used to access the information.