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•A GC–MS method for determination of bisphenols in dietary sport supplements.•The first described study focused on the BPs occurrence in sport supplements.•Five bisphenol analogues ...were detected except bisphenol Z in the samples.•Detected BPs levels indicate the possibility of migration from the packaging.
Bisphenol A (BPA) and its analogues showing structural and functional similarity to BPA are commonly applied in various industrial applications and thus are becoming ubiquitous in the environment. At the same time there is increasing scientific evidence that exposure to these chemicals may lead to adverse health effects in human and wildlife. In recent years dietary and nutritional supplements dedicated for athletes have become more popular and are widely used even by people who are not professionals. This study presents the development, optimization and validation of an analytical procedure for determination of six bisphenol analogues in dietary supplements using gas chromatography – mass spectrometry technique. All validation parameters met the established acceptance criteria in accordance with international guidelines. The method was linear within the tested range of 50–1000 ng/mL, the limit of quantitation was set as the lowest calibration point 50 ng/mL, detection limit for each bisphenol was calculated as standard estimation error on the basis of the linearity testing and was in the range of 8.73–15.44 ng/mL. Method trueness, accuracy (within and between runs) and precision were also verified and were in the range of 78.8 – 100.4%, 94.3 – 103.1%,
0.5 – 9.6% respectively.
The developed procedure was successfully applied for real samples analysis, namely for fifteen sport supplements of different composition and designated for various purposes, i.e. for increasing effectiveness, promoting muscle recovery and endurance, reducing tiredness and fatigue or increasing immune ability. For the majority of samples, bisphenols were either not detected or detected at the LOD level except bisphenol A which was quantitated in few samples at LOQ level or higher (in the range 0.852–2.892 ng/mg)
The field of bisphenol analogues analytics has increased in recent years due to law regulations becoming more strict, thus the development of new analytical tools for quality control of dietary products is needed and fully justified.
The fatty acid (FA) profiles of 240 samples of ricotta whey cheese made from sheep, goat, cow, or water buffalo milk were analyzed by gas-chromatography (GC). Then, sequential preprocessing through ...orthogonalization (SPORT) was used in order to classify samples according to the nature of the milk they were made from. This strategy achieved excellent results, correctly classifying 77 (out of 80) validation samples. Eventually, since 36 (over 114) sheep ricotta whey cheeses were PDO products, a second classification problem, finalizing the discrimination of PDO and Non-PDO dairies, was faced. In this case, two classifiers were used, SPORT and soft independent modelling by class analogy (SIMCA). Both approaches provided more than satisfying results; in fact, SPORT properly assigned 63 (of 65) test samples, whereas the SIMCA model accepted 14 PDO individuals over 15 (93.3% sensitivity) and correctly rejected all the other samples (100.0% specificity). In conclusion, all the tested approaches resulted as suitable for the two fixed purposes. Eventually, variable importance in projection (VIP) analysis was used to understand which FAs characterize the different categories of ricotta. Among the 22 analyzed compounds, about 10 are considered the most relevant for the solution of the investigated problems.
We investigated a possible association between polymorphisms in vitamin D binding protein (GC) and vitamin D receptor (VDR) genes and obesity in Bahraini adults. For this purpose, 406 subjects with ...varying body mass indexes (BMIs) were selected. Plasma levels of 25-hydroxyvitamin D3 (25OHD3) were measured by chemiluminescence immunoassay. Six single nucleotide polymorphisms, 2 in the VDR gene (rs731236 TC and rs12721377 AG) and 4 in the GC gene (rs2282679 AC, rs4588 CA, rs7041 GT, and rs2298849 TC), were genotyped by real-time polymerase chain reaction. We found that the rs7041 minor allele (G) and rare genotype (GG) were associated with higher BMI (p = 0.007 and p = 0.012, respectively), but they did not influence 25OHD3 levels. However, the minor alleles of rs2282679 (A) and rs4588 (C) were associated with low 25OHD3 plasma levels (p = 0.039 and p = 0.021, respectively), but not with BMI. Having categorized the subjects based on their sex, we found that (i) rs7041 GG associated with high BMI in females (p = 0.003), (ii) rs4588 CC associated with high BMI in females (p = 0.034) and low 25OHD3 levels in males (p = 0.009), and (iii) rs12721377 AA associated with low 25OHD3 levels in females (p = 0.039). Notably, none of the common haplotypes (6 in the GC gene and 3 in the VDR gene) were associated with BMI. Therefore, polymorphisms in the GC (rs2282679, rs4588, rs7041) and VDR (rs12721377) genes were independently associated with obesity and 25OHD3 levels with a clear sex dimorphism.
•Detection of 362 targeted prohibited compounds in equine urine for doping control.•A unified and generic sample preparation is followed by LC–MS and GC–MS analysis.•The method enables accurate mass ...determinations and acquisition in full scan mode.•The method allows retrospective analysis and easy incorporation of new substances.•Supplementary automated detection through library searching by using AMDIS-DRS.
In the present study a general screening protocol was developed to detect prohibited substances and metabolites for doping control purposes in equine sports. It was based on the establishment of a unified sample preparation and on the combined implementation of liquid and gas chromatographic MS analysis. The sample pretreatment began with two parallel procedures: enzymatic hydrolysis of sulfate and glucuronide conjugates, and methanolysis of the 17β-sulfate steroid conjugates. The extracts were treated for LC–TOF-MS, GC–HRMS and GC–MS assays. The majority of the prohibited substances were identified through a high mass accuracy technique, such as LC–TOF-MS, without prior derivatization. The sample preparation procedure included the formation of methylated and trimethylsilylated derivatives common in toxicological GC–MS libraries. The screening method was enhanced by post-run library searching using automated mass spectral deconvolution and identification system (AMDIS) combined with deconvolution reporting software (DRS). The current methodology is able to detect the presence of more than 350 target analytes in horse urine and may easily incorporate a lot of new substances without changes in chromatography. The full scan acquisition allows retrospective identification of prohibited substances in stored urine samples after reprocessing of the acquired data. Validation was performed for sixty representative compounds and included limit of detection, matrix interference – specificity, extraction recovery, precision, mass accuracy, matrix effect and carry over contamination. The suitability of the method was demonstrated with previously declared positive horse urine samples.
The Deepwater Horizon (DWH) explosion in 2010 is the largest oil spill (Macondo) in U.S.
We focused on gaining an understanding of the physical health and mental health effects attributable to the ...Macondo oil spill. This is a report of a cross-sectional cohort study (wave 1) to establish 'baseline' findings and meant to provide descriptive information to be used for a multi-wave, longitudinal study. Gulf Coast Health Alliance: health Risks related to the Macondo Spill (GC-HARMS) uses a Community-Based Participatory Research approach, thus including multi-disciplinary, multi-institutional academic partners and representatives of three communities impacted by the spill. Three research sites were selected for human sampling along the Gulf of Mexico coast including two from Mississippi and one from Louisiana, with Galveston, Texas, serving as a comparison site, given that it was not directly impacted by the spill. One hundred participants were selected from each community, representing adults, seniors and children, with approximately equal numbers of males and females in each group. Participants completed initial assessments including completion of a 'baseline' survey and, rigorous physical assessments. Results from wave 1 data collection reported herein reveal changes in self-reported physical health and mental health status following the oil spill, disparities in access to healthcare, and associations between mental health and emotional conditions related to displacement/unemployment. Few environmental health studies have been conducted in communities impacted by significant oil spills. Results imply potential prolonged effects on mental health and community vulnerability.
Diuretics are drugs that increase the rate of urine flow and sodium excretion to adjust the volume and composition of body fluids. There are several major categories of this drug class and the ...compounds vary greatly in structure, physicochemical properties, effects on urinary composition and renal haemodynamics, and site and mechanism of action. Diuretics are often abused by athletes to excrete water for rapid weight loss and to mask the presence of other banned substances. Because of their abuse by athletes, diuretics have been included on The World Anti‐Doping Agency's (WADA) list of prohibited substances; the use of diuretics is banned both in competition and out of competition and diuretics are routinely screened for by anti‐doping laboratories. This review provides an overview of the pharmacology and toxicology of diuretics and discusses their application in sports. The most common analytical strategies currently followed by the anti‐doping laboratories accredited by the WADA are discussed along with the challenges laboratories face for the analysis of this diverse class of drugs.
In official doping controls, about 300 drugs and metabolites have to be screened for each sample. Moreover, the number of determinations to be routinely processed increases continuously as the number ...of both samples and potential illicit drugs keeps growing. As a consequence, increasingly specific, sensitive, and, above all, fast methods for doping controls are needed. The present study presents an efficient fast‐GC/MS approach to the routine screening of two different classes of doping agents, namely β‐adrenoceptor ligands and diuretics (belonging to the S3, P2, and S5 groups of the WADA list of prohibited substances). Narrow bore columns (100 mm id) of different lengths and coated with apolar stationary phases were successfully used to separate the derivatized analytes; preliminary experiments (results not shown) showed better performances with OV‐1701 for the separation of β‐adrenoceptor ligands. On the same stationary phase some diuretics required too high a temperature or a long isothermal time for elution, in which case a DB1‐MS column was preferred. Two methods of sample preparation, derivatization, and analysis were used on aqueous standard mixtures of, respectively, (i) eight β‐adrenoceptor ligands, including five β1‐antagonists (acebutolol, alprenolol, atenolol, metoprolol, pindolol) and three β2‐agonists (salbutamol, clenbuterol, terbutaline) and (ii) seventeen diuretic drugs (acetazolamide, althiazide, bendroflumethiazide, bumethanide, canrenone, chlorothiazide, chlortalidone, clopamide, ethacrinic acid, furosemide, hydrochlorothiazide, hydroflumethiazide, indapamide, indomethacine, spironolactone, triamterene, trichloromethiazide) and one masking agent (probenecid). The mixture of β‐adrenoceptor ligand derivatives was efficiently separated in about 5.6 min, while the one of 18 diuretics and masking agents required less than 5 min for analysis. Limits of detection were from 1 μg/L for pindolol, ethacrinic acid, furosemide, indomethacine, and trichloromethiazide, to 20 μg/L for terbutaline, salbutamol, and metoprolol, and 50 μg/L for clopamide; the instrumental repeatability proved to be excellent (area RSD% <2 for almost all analytes). For this work a quadrupole MS with inert ion source has been used, demonstrating that the quadrupole technology is perfectly adequate to provide precise integration of 400 ms‐wide GC peaks.
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