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1.
JAMA Netw Open ; 7(5): e249131, 2024 May 01.
Article En | MEDLINE | ID: mdl-38691359

Importance: Dietary supplements for weight loss, among the most popular supplement products on the market, are promoted not only for losing weight and shedding fat, but also for added benefits of energy and performance, all packed into 1 capsule with multiple combinations of ingredients. Fraudulent marketing of weight loss supplements, some with exaggerated claims, some that are potentially dangerous, and some that contain illegal ingredients, is ever present, especially through online sources, where multiple manufacturers target service members by offering military discounts. Objectives: To examine whether select dietary supplements marketed online for weight loss from companies advertising military discounts are accurately labeled according to the Supplement Facts listed ingredients, whether they contain any ingredients prohibited for use in the military, and to qualitatively describe the products' label claims. Design, Setting, and Participants: In this case series, 30 dietary supplement products marketed for weight loss were selected and purchased in June 2023 from 12 online companies advertising military discounts. Data were analyzed from July to August 2023. Main Outcomes and Measures: Liquid chromatography-mass spectrometry was used to verify whether products were accurately labeled according to the Supplement Facts listed ingredients and whether they contained any substances on the DoD Prohibited Dietary Supplement Ingredients List. A separate analysis was conducted to describe product label claims by using the Operation Supplement Safety (OPSS) Risk Assessment Scorecard. Results: Of the 30 products tested, analysis showed that 25 had inaccurate labels. Of these, 24 had ingredients listed on the label that were not detected (misbranded); 7 had hidden components not present on the label, some of which would be considered adulterated; and 10 had substances on the DoD Prohibited Dietary Supplement Ingredients List either on or hidden from the label. All products were rated as risky when applying the OPSS Scorecard. Conclusions and Relevance: In this case series study, the majority of products had inaccurate labels. Some were misbranded, others would be considered adulterated with ingredients not allowed in dietary supplements, and some contained ingredients prohibited for use in the military.


Dietary Supplements , Weight Loss , Dietary Supplements/standards , Dietary Supplements/analysis , Humans , Military Personnel , United States , Product Labeling/standards , Advertising , Marketing , Anti-Obesity Agents/analysis
2.
Rapid Commun Mass Spectrom ; 38(5): e9705, 2024 Mar 15.
Article En | MEDLINE | ID: mdl-38343169

RATIONALE: The demand for weight loss products is increasing as slimness emerges as the new aesthetic standard and people's desire to achieve it increases. In addition, the distribution and sale of products containing illegal ingredients, pharmaceuticals, and chemicals for which safety is not guaranteed and that cannot be used as foods or dietary supplements are increasing. Thus, the development of an analytical method that could monitor these illegal products is required. METHODS: A high-performance liquid chromatography-photodiode array method capable of rapid and reliable qualitative and quantitative analyses of 43 weight loss agents was established and validated. RESULTS: The process involved dividing analytes into three groups for rapid analysis; when bisacodyl was mixed with chlorocyclopentylsibutramine, it decomposed into its metabolites: monoacetyl bisacodyl and bis-(p-hydroxypheny)-pyridyl-2-methane. This decomposition was due to NaOH that was used to prepare the chlorocyclopentylsibutramine standard solution. Bisacodyl did not degrade when mixed with neutralized chlorocyclopentylsibutramine, whereas when NaOH was added, it rapidly degraded. We identified the bisacodyl degradation products using liquid chromatography-quadrupole-Orbitrap/mass spectrometry. MS2 spectra with proposed structures of fragment peaks were also obtained. CONCLUSIONS: The developed method could be used to regulate slimming products that threaten public health, and knowledge of bisacodyl degradation will be used as the basis for developing an analytic method.


Anti-Obesity Agents , Humans , Chromatography, High Pressure Liquid/methods , Anti-Obesity Agents/analysis , Bisacodyl/analysis , Sodium Hydroxide , Dietary Supplements/analysis
3.
Nutrients ; 14(15)2022 Jul 27.
Article En | MEDLINE | ID: mdl-35893931

Food supplements of plant origin for weight control are increasingly being demanded by consumers as a way to promote good health. Among them, those based on Garcinia cambogia (GCFS) are widely commercialized considering their bioactive properties, mainly due to (-)-hydroxycitric acid ((-)-HCA). However, recently, controversy has arisen over their safety; thus, further research and continuous monitoring of their composition is required. Hence, in this work, a multi-analytical approach was followed to determine not only (-)-HCA but also other constituents of 18 GCFS, which could be used as quality markers to detect fraudulent practices in these samples. Discrepancies between the declared (-)-HCA content and that experimentally determined were detected by LC-UV in 33% of the samples. Moreover, GC-MS analyses of GCFS allowed the detection of different compounds not present in G. cambogia fruits and not declared on supplement labels, probably related to heat exposure or to the addition of excipients or other extracts. This multi-analytical methodology is shown to be advantageous to address different fraudulent practices affecting the quality of these supplements.


Anti-Obesity Agents , Garcinia cambogia , Anti-Obesity Agents/analysis , Dietary Supplements/analysis , Fruit/chemistry , Plant Extracts , Weight Loss
4.
Molecules ; 26(22)2021 Nov 16.
Article En | MEDLINE | ID: mdl-34833995

Weight loss supplements that have illegal additives of pharmaceutical drugs or analogues have additional health risks, and customers may not be aware of what they are taking. This research is an essential investigation and quantification of illegally added pharmaceuticals or prescription medications, specifically fluoxetine, phenolphthalein, and sibutramine, in herbal weight loss supplements offered for sale in the United Arab Emirates (UAE). In this case, 137 weight loss supplements were collected and analyzed in this study. Reversed-phase high-performance liquid chromatography with UV absorption detection coupled to tandem mass spectrometry (RP-HPLC-MS/MS) analyses were used to determine the presence of the pharmaceutical chemicals. Among the weight loss supplements, 15.3% (95% CI: 9.2-21.4) contained undeclared sibutramine, 13.9% (95% CI: 8.01-19.7) contained undeclared phenolphthalein, and 5.1% (95% CI: 1.4-8.8) contained undeclared fluoxetine. Amongst all weight loss supplements, 17.5% (95% CI: 11.07-24) contained significant concentrations of either sibutramine, phenolphthalein, or fluoxetine. Whilst weight loss herbal supplements offered for sale in the UAE have relatively low percentages of undeclared pharmaceuticals, many people take several different supplements daily and may encounter quite high levels of combined exposure to toxic compounds.


Anti-Obesity Agents/analysis , Dietary Supplements/analysis , Drug Contamination , Chromatography, High Pressure Liquid , Humans , Tandem Mass Spectrometry , United Arab Emirates
5.
J Chromatogr A ; 1647: 462102, 2021 Jun 21.
Article En | MEDLINE | ID: mdl-33964619

Despite the widespread use of artichoke-based food supplements for obesity control (FSOC), studies on evaluation of the quality/authenticity of these commercial products are scarce. To that aim, a new multi-analytical strategy, based on the use of gas chromatography coupled to mass spectrometry (GC-MS) and high performance liquid chromatography coupled to ultraviolet and mass spectrometry detection (HPLC-UV-MS), in combination with chemometrics, has been developed. Twenty-one artichoke FSOC and different bract and leaf extracts (used as reference samples) were analysed. Sugars, inositols, caffeoylquinic acids, dicaffeoylquinic acids, flavonoids and their glycosides were detected in reference samples and in most artichoke FSOC. Low concentrations of bioactives, and the presence of other compounds probably related to heat treatment during manufacturing (difructosyl anhydrides, 3-deoxyglucosone), or to the addition of caloric additives (maltose, maltotriose) or non-declared plants (e.g. pinitol, disaccharides, silybin derivatives) were also detected in some FSOC by either GC-MS or HPLC-UV-MS. Application of Principal Component Analysis to the combined GC-MS + HPLC-UV data matrix, proved that this multi-analytical strategy provides advantages over single analytical techniques for the detection of the wide variety of fraudulent practices affecting authenticity of artichoke FSOC and for assessment of their quality.


Anti-Obesity Agents , Cynara scolymus , Dietary Supplements , Anti-Obesity Agents/analysis , Anti-Obesity Agents/chemistry , Anti-Obesity Agents/standards , Chromatography, High Pressure Liquid/methods , Dietary Supplements/analysis , Dietary Supplements/standards , Gas Chromatography-Mass Spectrometry/methods , Plant Extracts/chemistry
6.
BMC Endocr Disord ; 21(1): 80, 2021 Apr 26.
Article En | MEDLINE | ID: mdl-33902539

BACKGROUND: Obesity associated type 2 diabetes mellitus is a metabolic disorder ; however, the etiology of obesity associated type 2 diabetes mellitus remains largely unknown. There is an urgent need to further broaden the understanding of the molecular mechanism associated in obesity associated type 2 diabetes mellitus. METHODS: To screen the differentially expressed genes (DEGs) that might play essential roles in obesity associated type 2 diabetes mellitus, the publicly available expression profiling by high throughput sequencing data (GSE143319) was downloaded and screened for DEGs. Then, Gene Ontology (GO) and REACTOME pathway enrichment analysis were performed. The protein - protein interaction network, miRNA - target genes regulatory network and TF-target gene regulatory network were constructed and analyzed for identification of hub and target genes. The hub genes were validated by receiver operating characteristic (ROC) curve analysis and RT- PCR analysis. Finally, a molecular docking study was performed on over expressed proteins to predict the target small drug molecules. RESULTS: A total of 820 DEGs were identified between healthy obese and metabolically unhealthy obese, among 409 up regulated and 411 down regulated genes. The GO enrichment analysis results showed that these DEGs were significantly enriched in ion transmembrane transport, intrinsic component of plasma membrane, transferase activity, transferring phosphorus-containing groups, cell adhesion, integral component of plasma membrane and signaling receptor binding, whereas, the REACTOME pathway enrichment analysis results showed that these DEGs were significantly enriched in integration of energy metabolism and extracellular matrix organization. The hub genes CEBPD, TP73, ESR2, TAB1, MAP 3K5, FN1, UBD, RUNX1, PIK3R2 and TNF, which might play an essential role in obesity associated type 2 diabetes mellitus was further screened. CONCLUSIONS: The present study could deepen the understanding of the molecular mechanism of obesity associated type 2 diabetes mellitus, which could be useful in developing therapeutic targets for obesity associated type 2 diabetes mellitus.


Computational Biology , Diabetes Mellitus, Type 2 , Obesity , Small Molecule Libraries/analysis , Anti-Obesity Agents/analysis , Anti-Obesity Agents/isolation & purification , Anti-Obesity Agents/pharmacokinetics , Datasets as Topic , Diabetes Mellitus, Type 2/drug therapy , Diabetes Mellitus, Type 2/genetics , Diabetes Mellitus, Type 2/metabolism , Drug Evaluation, Preclinical/methods , Gene Expression Profiling , Gene Ontology , Gene Regulatory Networks , Genetic Association Studies/methods , Humans , Hypoglycemic Agents/analysis , Hypoglycemic Agents/isolation & purification , Hypoglycemic Agents/pharmacokinetics , Molecular Docking Simulation , Obesity/drug therapy , Obesity/genetics , Obesity/metabolism , Protein Interaction Maps
7.
Clin Toxicol (Phila) ; 59(11): 975-981, 2021 Nov.
Article En | MEDLINE | ID: mdl-33755516

BACKGROUND: Weight loss and sports supplements containing deterenol have been associated with serious adverse events including cardiac arrest. OBJECTIVE: To determine the presence and quantity of experimental stimulants in dietary supplements labeled as containing deterenol sold in the United States. METHODS: Dietary supplements available for sale in the US and labeled as containing deterenol or one of its synonyms (e.g., isopropylnorsynephrine and isopropyloctopamine) were purchased online. For each brand, one container or subsample was analyzed by NSF International (Ann Arbor, MI) and one container or subsample by the Netherland's National Institute for Public Health and the Environment (RIVM, Bilthoven, The Netherlands). When differences existed between the two containers or subsamples of the same brand, both products were reanalyzed by Sciensano (Brussels, Belgium). NSF International carried out qualitative and quantitative analyses using ultra-high-performance liquid chromatography (UHPLC) quadrupole-Orbitrap mass spectrometry. RIVM performed qualitative and quantitative analysis using UHPLC quadrupole time-of-flight mass spectrometry. Sciensano carried out qualitative analysis using UHPLC quadrupole-Orbitrap mass spectrometry. RESULTS: Seventeen brands of supplements were analyzed. Many brands included more than one prohibited stimulant in the same product: 4 brands (24%, 4/17) included 2 stimulants, 2 (12%, 2/17) combined 3 stimulants, and 2 (12%, 2/17) combined 4 stimulants. The range of quantities per recommended serving size of the 9 stimulants detected were 2.7 mg to 17 mg of deterenol; 1.3 mg to 20 mg of phenpromethamine (Vonedrine); 5.7 mg to 92 mg of beta-methylphenylethylamine (BMPEA); 18 mg to 73 mg of octodrine; 18 mg to 55 mg of oxilofrine; 48 mg of higenamine; 17 mg of 1,3-dimethylamylamine (1,3-DMAA); 1.8 mg to 6.6 mg of 1,3-dimethylbutylamine (1,3-DMBA); and 5.3 mg of 1,4-dimethylamylamine (1,4-DMAA). CONCLUSION: Weight loss and sports supplements listing deterenol as an ingredient contained 9 prohibited stimulants and 8 different mixtures of stimulants, with as many as 4 experimental stimulants per product. These cocktails of stimulants have never been tested in humans and their safety is unknown.


Adrenergic Agonists/analysis , Anti-Obesity Agents/analysis , Central Nervous System Stimulants/analysis , Dietary Supplements/analysis , Adrenergic Agonists/adverse effects , Alkaloids/analysis , Amines/analysis , Amphetamines/analysis , Anti-Obesity Agents/adverse effects , Central Nervous System Stimulants/adverse effects , Consumer Product Safety , Dietary Supplements/adverse effects , Ephedrine/analogs & derivatives , Ephedrine/analysis , Heptanes/analysis , Humans , Octopamine/analogs & derivatives , Octopamine/analysis , Risk Assessment , Tetrahydroisoquinolines/analysis , United States
8.
J Forensic Leg Med ; 79: 102148, 2021 Apr.
Article En | MEDLINE | ID: mdl-33706128

A complete case example of a fatal 2,4-dinitrophenol (DNP) overdose involving a 23-year-old male is described. Included are details of not only the patient's presentation symptoms and treatment, but also the subsequent findings of the coronial investigation process including the autopsy, post-mortem computed tomography (PMCT) scanning and toxicological analysis and results. The patient presented with elevated temperature, heart rate and blood pressure. Multiple treatments were conducted to counteract these symptoms, however the patient died approximately 1.5 hours after hospital admission and some 4.5 hours after the DNP was initially consumed. Autopsy revealed the presence of cardiovascular disease that was contributory to death and post-mortem computed tomography showed evidence of decompositional intravascular gas in the neck, head, face, lower abdomen, heart and hepatic systems. Toxicological analysis was completed by protein precipitation with methanol and subsequent instrumental analysis by LC/MS/MS in negative ion mode. The antemortem blood specimen showed the presence of tadalafil, two anabolic steroids and a DNP concentration of 110 mg/kg which is consistent with other reported DNP fatalities. Despite the small amount of time between the antemortem specimen collection and death, the DNP concentration identified in the femoral blood post-mortem specimen was comparably low (5.5 mg/kg). DNP concentrations also reduced during an extended period of specimen storage prior to analysis indicating some instability in biological specimens even when refrigerated or frozen. DNP was found to be distributed primarily in the aqueous tissues (blood, vitreous, bile) rather than solid matrices (liver, kidney, muscle).


2,4-Dinitrophenol/poisoning , Anti-Obesity Agents/poisoning , Drug Overdose , Suicide, Completed , 2,4-Dinitrophenol/analysis , Anti-Obesity Agents/analysis , Bile/chemistry , Coronary Artery Disease/pathology , Gases , Humans , Male , Muscle, Skeletal/chemistry , Postmortem Changes , Tomography, X-Ray Computed , Vitreous Body/chemistry , Young Adult
9.
Article En | MEDLINE | ID: mdl-33412503

With an increase in the obese population, the indiscriminate demand for anti-obesity drugs for rapid weight loss or maintenance has grown. As a result, illegal substances that could induce unexpected negative health effects or fatal side effects are being produced and mixed into consumer products. In the present study, the metabolites of five major illegal anti-obesity drugs are analyzed for the first time. Our data can be utilized to identify related compounds and predict their toxicological effects. Didesmethylsibutramine, desmethylsibutramine, homosibutramine, chlorosibutramine, and benzylsibutramine were metabolized in in vitro and in vivo models, and the metabolites were identified using liquid chromatography quadrupole-time of flight mass spectrometry (LC-Q-TOF-MS) and tandem mass spectrometry (LC-Q-TOF-MS/MS). The in vivo metabolite analysis was carried out using urine and feces samples from rats, and the in vitro metabolite analysis was performed by incubating the analogues with human liver microsomes. We found that each sibutramine analogue was metabolized into several constituents: 2 (M1-2), 5 (M1-5), 11 (M1-11), 7 (N1-7), and 5 (O1-5). In conclusion, our metabolic study could be used for toxicological detection of illegal obesity treatments and metabolite identification in forensic cases.


Anti-Obesity Agents , Chromatography, Liquid/methods , Cyclobutanes , Illicit Drugs , Tandem Mass Spectrometry/methods , Animals , Anti-Obesity Agents/analysis , Anti-Obesity Agents/metabolism , Cyclobutanes/analysis , Cyclobutanes/metabolism , Humans , Illicit Drugs/analysis , Illicit Drugs/metabolism , Male , Microsomes, Liver/metabolism , Rats , Rats, Sprague-Dawley
10.
Nutrients ; 12(10)2020 Oct 03.
Article En | MEDLINE | ID: mdl-33022997

Fillets from marine fish species contain n-3 polyunsaturated fatty acids (PUFAs) in the form of phospholipids (PLs). To investigate the importance of PL-bound n-3 PUFAs in mediating the anti-obesogenic effect of lean seafood, we compared the anti-obesogenic properties of fillets from cod with fillets from pangasius, a fresh water fish with a very low content of PL-bound n-3 PUFAs. We prepared high-fat/high-protein diets using chicken, cod and pangasius as the protein sources, and fed male C57BL/6J mice these diets for 12 weeks. Mice fed the diet containing cod gained less adipose tissue mass and had smaller white adipocytes than mice fed the chicken-containing diet, whereas mice fed the pangasius-containing diet were in between mice fed the chicken-containing diet and mice fed the cod-containing diet. Of note, mice fed the pangasius-containing diet exhibited reduced glucose tolerance compared to mice fed the cod-containing diet. Although the sum of marine n-3 PUFAs comprised less than 2% of the total fatty acids in the cod-containing diet, this was sufficient to significantly increase the levels of eicosapentaenoic acid (EPA) and docosahexaenoic acids (DHA) in mouse tissues and enhance production of n-3 PUFA-derived lipid mediators as compared with mice fed pangasius or chicken.


Anti-Obesity Agents/analysis , Catfishes , Fatty Acids/analysis , Gadus morhua , Seafood/analysis , Adipose Tissue/metabolism , Animals , Diet, High-Fat/methods , Diet, High-Protein/methods , Docosahexaenoic Acids/metabolism , Eicosapentaenoic Acid/metabolism , Fatty Acids, Omega-3/analysis , Lipid Metabolism , Male , Mice , Mice, Inbred C57BL , Poultry Products
11.
J Med Food ; 23(3): 215-223, 2020 Mar.
Article En | MEDLINE | ID: mdl-32191576

Anti-obesity activities of Korean red ginseng saponin fraction (RGS) and/or Glycyrrhiza glabra L. extract (GG) were investigated in 3T3-L1 adipocytes and high-fat diet-induced C57BL/6J obese mice. RGS and GG extracts were mixed at a mass ratio of 3:1 (SG31), 1:1 (SG11), or 1:3 (SG13). SG31 showed the highest anti-obesity activity among the three different mass ratios of RGS and GG extracts. SG31 showed higher inhibition efficiency on triglyceride (TG) accumulation than either single extract in 3T3-L1 adipocytes and without any cytotoxicity. It also decreases the expression of adipogenic and lipogenic genes such as C/EBPα and SREBP-1c (sterol regulatory element-binding protein 1c). In the obese induced mouse model, SG31 significantly reduced white adipose tissue weight and body weight, attenuated dyslipidemia, and decreased serum TG levels. In some indices, the activity of SG31 was even higher compared with Garcinia Cambogia water extract, a positive control. The possible mechanism by which SG31 causes the above results was by activating the AMP-activated protein kinase (AMPK) pathway and stimulating the secretion of adiponectin in adipose tissue to regulate energy metabolism balance, inhibit TG formation, and promote ß-oxidation of fatty acids. Therefore, SG31 may have efficacy as an anti-obesity functional food or raw material if the results can be confirmed in human studies.


Adipocytes/drug effects , Anti-Obesity Agents/administration & dosage , Glycyrrhiza/chemistry , Obesity/drug therapy , Panax/chemistry , Plant Extracts/administration & dosage , 3T3-L1 Cells , Adipocytes/metabolism , Animals , Anti-Obesity Agents/analysis , CCAAT-Enhancer-Binding Protein-alpha/genetics , CCAAT-Enhancer-Binding Protein-alpha/metabolism , Humans , Lipogenesis/drug effects , Male , Mice , Mice, Inbred C57BL , Mice, Obese , Obesity/genetics , Obesity/metabolism , Obesity/physiopathology , PPAR gamma/genetics , PPAR gamma/metabolism , Plant Extracts/analysis , Sterol Regulatory Element Binding Protein 1/genetics , Sterol Regulatory Element Binding Protein 1/metabolism , Triglycerides/blood
12.
Food Chem ; 313: 126156, 2020 May 30.
Article En | MEDLINE | ID: mdl-31931426

Low calorie foods are products designed to replace complete meals or to control snacking in many hypocaloric diets. These products provide many nutrients to the human diet, but little is known about their mineral elements composition. Here we study the mineral profile of weight loss related products, including the analysis of 22 elements (As, Ba, Be, Bi, Cd, Co, Cr, Cu, K, Mn, Mo, Na, Ni, P, Pb, Th, Tl, Sb, U, V, Y and Zn) in 73 commercial products marketed in Spain. In general a portion of these products provide up to 20-30% of the daily dietary reference intake of essential trace minerals like Cr or Mo. On the contrary, some of these foods have large concentrations of toxic minerals like As, Cd or Pb. In fact, the intake of those products with higher concentrations of toxic elements during a weight loss program could pose a risk to human health.


Anti-Obesity Agents/chemistry , Diet, Reducing , Food Contamination/analysis , Minerals/analysis , Anti-Obesity Agents/analysis , Food Analysis , Humans , Metals/analysis , No-Observed-Adverse-Effect Level , Risk Assessment , Spain , Trace Elements/analysis
13.
J Sci Food Agric ; 100(3): 897-903, 2020 Feb.
Article En | MEDLINE | ID: mdl-31588996

Tea polyphenols (TP) are the main components in tea. Studies in vitro have shown they have significant biological activity; however, the results are inconsistent with experiments in vivo. For the low bioavailability, most TP are thought to remain in the gut and metabolized by intestinal bacteria. In the gut, the unabsorbed TP are metabolized to a variety of derivative products by intestinal flora, which may accumulate to exert beneficial effects. Numerous studies have shown that TP can inhibit obesity and its related metabolism disorders effectively. Meanwhile, it has demonstrated that TP and their derivatives may modulate intestinal micro-ecology. The understanding of the interaction between TP and intestinal microbiota will allow us to better evaluate the contribution of microbial metabolites of TP to anti-obesity activity. This review showed implications for the use of TP as functional food with potential therapeutic utility against obesity by modulating intestinal microbiota, contributing to the improvement of human health. © 2019 Society of Chemical Industry.


Anti-Obesity Agents/metabolism , Obesity/metabolism , Obesity/microbiology , Polyphenols/metabolism , Tea/metabolism , Animals , Anti-Obesity Agents/analysis , Camellia sinensis/chemistry , Camellia sinensis/metabolism , Gastrointestinal Microbiome , Humans , Polyphenols/analysis , Tea/chemistry
14.
J Pharm Biomed Anal ; 179: 113003, 2020 Feb 05.
Article En | MEDLINE | ID: mdl-31816474

The aim of this study was to simultaneously determine the presence of unauthorized drug substances in health foods and herbal products used in the treatment of conditions such as gout and anti-osteoporosis. Therefore, we developed and optimised a rapid and accurate method to simultaneously measure 20 anti-gout and anti-osteoporosis drug substances using an ultra-high-performance liquid chromatography (UPLC) system equipped with a photodiode array (PDA) detector. The method was validated to fully meet internationally accepted standards. LODs and LOQs spiked in solid and liquid negative samples were ranged from 0.12 to 1.50 µg/mL, and ranged from 0.36 to 4.50 µg/mL. Linearities (R2> 0.999), stabilities (RSD ≤ 2.92%), accuracies (84.25∼106.62%, intra-day; 84.56∼105.85%, inter-day), precisions (RSD ≤ 3.71% on the intra-day; RSD ≤ 3.47% on the inter-day), recoveries spiked in various type of blank samples such as powder, liquid, tablet, and capsule were determined within 81.20-116.20 %, respectively. From a confirmation of matrix effects (88.06∼110.50% in solid blank; 89.16∼110.52% in liquid blank), it was confirmed that this method was not significantly affected by a sample matrix. The validated method was used to analyse 116 samples containing health foods, herbal products, and seized forensic samples advertised to be effective anti-gout and anti-osteoporosis agents. Of the 20 drug substances screened, dexamethasone was detected and confirmed by comparing the tandem mass spectrometry (MS/MS) fragment ion patterns of a reference standard and the sample using LC-quadrupole-time-of-flight (Q-TOF)/MS. The concentrations of adulterants in seized forensic samples ranged from 0.013 to 0.022 %.


Chromatography, High Pressure Liquid/methods , Dietary Supplements/analysis , Food Contamination/analysis , Mass Spectrometry/methods , Anti-Obesity Agents/analysis , Gout Suppressants/analysis , Limit of Detection
15.
Biomed Chromatogr ; 34(1): e4698, 2020 Jan.
Article En | MEDLINE | ID: mdl-31762077

BACKGROUND: Dietary supplements (DS) containing undeclared substances may pose serious risk to s public health. The consumers of DS should be aware of such products in order to avoid the risk of fatal outcomes. AIM OF THE STUDY: The study is based on the determination and identification of undeclared substances - theobromine (TB), theophylline (TH), pseudoephedrine (PE), caffeine (C), hydrochlorothiazide (HTZ) and yohimbine (Y) - in market-available DS. MATERIAL AND METHODS: Ultra-high-performance liquid chromatography with diode array detection (UHPLC-DAD) was utilized to identify and quantify the presence of undeclared substances, in 52 different DS collected from the market. RESULTS: A fast and reliable UHPLC-DAD method was developed and validated for simultaneous determination of the analyte where an efficient separation was achieved within 7 min runtime (TB 1.47, TH 1.79, PE 2.08, C 2.26, HTZ 3.78, Y 6.50) with resolution >1.5. The method validation produced r2 values ranging from 0.975 to 0.999 within a linearity range of 1-300 ppm. The UHPLC method revealed the presence of undeclared substances in 11 samples (HD3, HD4, HD9, HD13, HD14, HD15, HD21, HD24, HD27, HD38 and HD40), where the most widely distributed analyte was PE and C. The analyte found to have the highes concentrations (mg) in these DS were PE (11) and C (2.01). Among the 52 DS products tested, the product HD3 revealed a greater number and amount (mg) of undeclared substances, i.e. TH (0.05), C (2.01), HTZ (0.37) and Y (0.05), followed by HD14, i.e. PE (9.31), C (0.40), HTZ (0.01) and HD9 PE (11.00), C (0.41). CONCLUSION: The abundance of undeclared substances in these DS products was PE > C > Y > HTZ. None of the DS contained TB whereas TH was present in only one sample.


Anti-Obesity Agents/analysis , Chromatography, High Pressure Liquid/methods , Dietary Supplements/analysis , Anti-Obesity Agents/standards , Dietary Supplements/standards , Drug Contamination/prevention & control , Limit of Detection , Linear Models , Principal Component Analysis , Reproducibility of Results , Saudi Arabia
16.
Food Chem Toxicol ; 136: 111036, 2020 Feb.
Article En | MEDLINE | ID: mdl-31862287

Maqui-berry (Aristotelia chilensis) is the emerging Chilean superfruit with high nutraceutical value. Until now, the research on this commodity was focused on the formulations enriched with polyphenols from the pulp. Herein, contents of tocols were compared in the seed oil of Maqui-berry obtained through three different extraction methods followed by determining their antioxidative and enzyme inhibitions in-vitro. Firstly, oilseed was extracted with n-hexane (Soxhlet method), chloroform/methanol/water (Bligh and Dyer method) and pressing (industrial). These samples were used to access their effects against DPPH, HORAC, ORAC, FRAP, Lipid-peroxidation (TBARS), α-amylase, α-glucosidase, and pancreatic lipase. All the isomers of tocopherol and tocotrienol were identified, and ß-sitosterol was the only sterol found in higher amounts than other vegetable oils. The Bligh and Dyer method could lead to the highest antioxidative capacity compared to Soxhlet and press methods likely because the latter have a higher amount of tocopherols. Further, seed oil from Maqui berry and their tocols (α, ß, γ, δ-tocopherols, tocotrienols, and ß-sitosterol) warrant clinical investigation for their antioxidative and antiobesity potential. Taken together, these findings provide relevant and suitable conditions for the industrial processing of Maqui-berry.


Anti-Obesity Agents/pharmacology , Antioxidants/pharmacology , Enzyme Inhibitors/pharmacology , Sitosterols/pharmacology , Tocopherols/pharmacology , Tocotrienols/pharmacology , Animals , Anti-Obesity Agents/analysis , Antioxidants/analysis , Enzyme Inhibitors/analysis , Lipase/antagonists & inhibitors , Magnoliopsida/chemistry , Male , Rats, Wistar , Seeds/chemistry , Sitosterols/analysis , Tocopherols/analysis , Tocotrienols/analysis
17.
J Evid Based Integr Med ; 24: 2515690X19883258, 2019.
Article En | MEDLINE | ID: mdl-31766874

The acquisition of ethnobotanical information from traditional practitioners remains an empirical aspect of understanding the ethnopharmacology research. However, integration of information on chemical composition of plant extracts and their pharmacological activities forms a key resource for synthesis of new and effective therapeutics. In traditional African medicine, Gnidia glauca has folkloric remedies against obesity and its associated oxidative stress-mediated complications. However, the upsurge in its use has not been accompanied with scientific validations to support these claims. The present study aimed to determine the antioxidant potential of G glauca as a promising antiobesity agent. The antioxidant effects of the extract were assessed against 1,1-diphenyl-2-picrylhydrazyl, hydroxyl, hydrogen peroxide, nitric oxide, and superoxide radicals as well as lipid peroxidation, iron-chelating effect, and ferric-reducing power. Phytochemical analysis was conducted using gas chromatography linked to mass spectrophotometry. The results revealed that G glauca exhibited scavenging activities against all radicals formed. Besides, the extract showed iron chelation and ferric reducing abilities. The extract indicated a lower half maximal inhibitory concentration value than the standards used. For instance, the extract inhibited 50% of the formation of 2,2-diphenyl-1-picrylhydrazine at the concentration of 1.33 ± 0.03 mg/mL relative to 1.39 ± 0.06 mg/mL of the standard, vitamin C at 1% confidence limit. Similarly, the extract scavenged 50% of hydroxyl radical at 204.34 ± 10.64 µg/mL relative to 210.05 ± 8.80 µg/mL of gallic acid. The extract also contained various phytochemicals that have been associated with antiobesity effects. The synergistic effects of these phytocompounds increase their bioavailability and action on multiple molecular targets thereby correcting obesity-induced oxidative stress.


Anti-Obesity Agents/analysis , Antioxidants/analysis , Plant Extracts/analysis , Thymelaeaceae/chemistry , Anti-Obesity Agents/isolation & purification , Antioxidants/isolation & purification , Lipid Peroxidation/drug effects , Plant Extracts/isolation & purification , Plant Leaves/chemistry
18.
Food Res Int ; 126: 108589, 2019 12.
Article En | MEDLINE | ID: mdl-31732028

The aim of the present study was to evaluate extractable (EPP), non-extractable polyphenols (NEPP) and organic acid in Roselle by-product, as well as its potential health beneficial effects in obesity control and their complication in rats fed with high caloric diet. Roselle by-product showed a higher content of dietary fiber and NEPP than Roselle calix, which was was a better source of EPP (P < .05). The UPLC-QTOF MSE analysis allowed the tentative identification of 34 EPP, and 3 hydrolysable polyphenols (NEPP), and 2 organic acids in calyx and by-product. Rats fed with a high caloric diet supplemented with 4% of dietary fiber from by-products and Roselle calyx powder generated a reduction in body weight gain (10% and 14%), adipocytes hypertrophy (17% and 13%) and insulin resistance (48% and 59%) and hepatic steatosis (15% and 25%; respectively) compared with rats fed with a high caloric diet alone. Interestingly, even though Roselle by-product has low EPP contents showed comparable beneficial health effects than Roselle calyces. These effects could be associated with high content of dietary fiber and NEPP. Together, the results of the present study indicate that Roselle by-products could be a potential ingredient to develop functional foods against obesity and its complications.


Anti-Obesity Agents/analysis , Flowers/chemistry , Hibiscus/chemistry , Phenols/analysis , Phytochemicals/analysis , Animals , Anthocyanins/analysis , Anthocyanins/pharmacology , Anti-Obesity Agents/pharmacology , Dietary Fiber/analysis , Dietary Fiber/pharmacology , Ellagic Acid/analysis , Ellagic Acid/pharmacology , Male , Phenols/pharmacology , Phytochemicals/pharmacology , Plant Extracts/analysis , Plant Extracts/pharmacology , Polyphenols/analysis , Polyphenols/pharmacology , Quercetin/analysis , Quercetin/pharmacology , Rats , Rats, Wistar
19.
Se Pu ; 37(9): 969-976, 2019 Sep 08.
Article Zh | MEDLINE | ID: mdl-31642301

A liquid chromatography-Orbitrap high resolution mass spectrometry (LC-HRMS) method and a TraceFinder database were developed for the screening and identification of 15 adulterated weight loss compounds in dietary supplements. The samples were extracted with methanol and filtered through a 0.22 µm microfiltration membrane prior to LC-HRMS analysis. The Full MS/dd-MS2 mode was utilized in both positive and negative ion modes and the collected data were imported into the TraceFinder screening software. The established compound database and screening method were used for rapid, automatic, and high-precision screening to determine if the weight loss compounds were adulterated. The method validation results indicated that all of the analytes showed excellent linear relationships with regression coefficients (r) above 0.998. The recoveries were in the range of 79.7%-95.4% while the precisions ranged from 3.3% to 8.7%. The method and database were used to screen weight loss adulterants in 29 batches of dietary supplements; six batches of samples tested positive for adulterants with the identification of four compounds including sibutramine. This method enables the automatic high-precision screening and identification of adulterants, providing a novel and powerful tool for combating the increasingly rampant occurrence of adulteration in dietary supplements.


Anti-Obesity Agents/analysis , Dietary Supplements/analysis , Drug Contamination , Chromatography, Liquid , Tandem Mass Spectrometry
20.
Food Res Int ; 123: 144-152, 2019 09.
Article En | MEDLINE | ID: mdl-31284962

Guaraná is a native fruit of the Amazon rainforest, which presents high levels of phenolic compounds. However, these bioactive compounds may be unstable in food processing and gastrointestinal conditions. Thus, this work aimed to characterize guaraná seed extract (GSE) followed by microencapsulation using a spray-chilling method and with vegetable fat as carrier, as well as to evaluate the particles. Phenolic-rich GSE was produced using 50% (w/w) hydroalcoholic solution and dehydrated by spray drying and lyophilization. Powdered GSE was characterized in relation to its inhibitory activity on digestive enzymes. Solid lipid microparticles (SLM) were evaluated for the retention of bioactive compounds and the release profile of phenolic compounds in simulated gastrointestinal conditions. Powdered GSE showed anti-obesity potential due to the high inhibitory activity of lipase. Regarding the retention of phenolic compounds, at least 75% were detected after 90 days at 25 °C in SLM. Moreover, SLM loaded with 7.5% GSE released approximately 99% of phenolic compounds in simulated gastrointestinal conditions. These results show the efficiency of spray chilling for protection and release of phenolic compounds from GSE, allowing future application in food.


Paullinia/chemistry , Plant Extracts/analysis , Seeds/chemistry , Anti-Obesity Agents/analysis , Caffeine/chemistry , Catechin/analysis , Chromatography, High Pressure Liquid , Delayed-Action Preparations , Freeze Drying , Fruit/chemistry , Lipase/metabolism , Particle Size , Phenols/analysis , Theobromine/chemistry , Theophylline/chemistry , alpha-Amylases/metabolism , alpha-Glucosidases/metabolism
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