scholarly journals Evaluation of 99 Pesticide Residues in Major Agricultural Products from the Western Highlands Zone of Cameroon Using QuEChERS Method Extraction and LC-MS/MS and GC-ECD Analyses

Foods ◽  
2018 ◽  
Vol 7 (11) ◽  
pp. 184 ◽  
Author(s):  
Joseph Galani ◽  
Michael Houbraken ◽  
Abukari Wumbei ◽  
Joseph Djeugap ◽  
Daniel Fotio ◽  
...  
Keyword(s):  
Scientific Evidence ◽  
Chili Pepper ◽  
Agricultural Products ◽  
Electron Capture Detection ◽  
Limit Of Quantification ◽  
Kidney Beans ◽  
Sampling Locations ◽  
Liquid Chromatography Tandem Mass ◽  
Food Commodities ◽  
Almost All

There is no information available on pesticide residue levels in major food commodities harvested in Cameroon, especially from the western highlands region, the food basket of the country. Hence, this study evaluated the residues of 99 pesticides in 72 samples of 12 agricultural products collected in the region, using QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) method extraction, and analyzed by liquid chromatography tandem mass spectrometry (LC-MS/MS) and gas chromatography with electron capture detection (GC-ECD). This method was suitable for detecting the targeted compounds: For 81 pesticides by LC-MS/MS, the limit of quantification (LOQ) was between 0.0004 and 0.0537 mg/kg; and for 18 halogenated pesticides by GC-ECD, it ranged from 0.0012 to 0.2180 mg/kg. The residues of 62 pesticides, including 12 banned compounds, were found in the samples. Insecticides (39.7%) were the most prevalent group, with all the samples containing at least one pesticide. Twenty-one pesticides (34.4%) exceeded their European Union maximum residue limits (MRLs) and 22 pesticides (34.4%) were found in all 6 sampling locations. Malathion and p,p′-DDT were the most distributed pesticides, found in almost all the samples and sampling sites. Food items with the highest rates of positive results were chili pepper (23.2%), white pepper (20.2%), kidney beans (17.3%), and soybeans (17.2%). Samples with residues above their MRLs represented 38% of all the positive analyses; chili pepper (6.4%) and kidney beans (5.5%) were found to have the most residues above their MRLs. The most critical food commodities were kidney beans, soybeans, chili pepper, and maize. This data presents scientific evidence that investigation into continuous monitoring and good regulation of pesticide usage in Cameroon is needed, and paves the way for health risks analysis.

scholarly journals Preliminary monitoring of the presence of perfluoroalkyl substances in Italian eggs from different breeding systems

2019 ◽  
Vol 8 (2) ◽  
Author(s):  
Elisa Ghelli ◽  
Maria Teresa Tondo ◽  
Elisa Zironi ◽  
Giampiero Pagliuca ◽  
Federico Sirri ◽  
...  
Keyword(s):  
Daily Intake ◽  
Environmental Pollutant ◽  
Breeding Systems ◽  
Contamination Level ◽  
Limit Of Quantification ◽  
Equal Distribution ◽  
Significant Difference ◽  
Liquid Chromatography Tandem Mass ◽  
Almost All ◽  
Chicken Eggs

Perfluoroalkylated substances (PFASs) are a wide cluster of fluorinated molecules largely engaged industrially and commercially for many purposes. Because of the strength of the fluorine-carbon bond, PFASs show a firm tenacity against thermal degradation, hydrolysis, photolysis and biodegradation. On the other hand, such chemical stability gives them persistent environmental pollutant feature. In 2012, EFSA published a scientific report on PFASs in food, mentioning their adverse effects on health. Based on observational studies evidences, EFSA has recommended a tolerable daily intake (TDI) for the two most known PFASs, i.e. PFOS 150 ng/kg b.w./day and PFOA 1500 ng/kg b.w./day. The aim of this study was to monitor, for the first time, the level of contamination of PFASs in chicken eggs laid in Northern Italy. The eggs were collected from different rearing systems, in order to search a correlation between this variable and the contamination of PFASs. In this study four PFASs [perfluoro-nnonanoic acid (PFNA), perfluoro-noctanoic- acid (PFOA), sodium perfluoro-1- hexanesulfonate (PFHxS) and sodium perfluoro- 1-octanesulfonate (PFOS)] were analyzed by liquid chromatography-tandem mass spectrometer (LC-MS/MS). 132 eggs were analyzed, split up in 11 groups according to the geographical origin and rearing system. Results accord with literature data available for chicken eggs: almost all the samples show a PFASs contamination level under the limit of quantification (LOQ) of 0.25 ng/mL. No significant difference results from the rearing system, attesting an equal distribution and a concentration of PFASs detectable under the limit of quantification.

scholarly journals Validation and Application of a Methodology for Quantifying Levels of Parabens in Sports Supplements from Brazil Using Liquid Chromatography-Mass Spectrometry

2022 ◽  
Author(s):  
Bruno Rocha ◽  
Cibele Cesila ◽  
Airton Martins ◽  
Marília Souza ◽  
Fernando Barbosa Jr.
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Food Samples ◽  
Limit Of Quantification ◽  
Detection Rates ◽  
Sports Supplements ◽  
Liquid Chromatography Tandem Mass ◽  
Almost All ◽  
Harmful Effects

Although parabens have been reported to be used as antimicrobial preservatives in personal care products, pharmaceuticals, and foodstuffs, little is known about the occurrence of these compounds in sports supplements. In this study, a simple, fast and sensitive liquid chromatography tandem mass spectrometry method for simultaneous determination of five commonly used parabens, methyl-, ethyl-, propyl-, butyl-, and benzylparaben in sports supplements was established. The analytical method was validated with the values of parameters being acceptable. The method proved reliable, accurate, and sensitive and was successfully applied for the quantitation of parabens in 85 sports supplements samples. Almost all sports supplements contained at least one of the parabens analyzed, and the total concentrations of five parabens ranged from below the limit of quantification to 145 μg g-1, with a median value of 0.171 μg g-1. Ethylparaben and methylparaben were the most frequent paraben analogs found in samples (detection rate > 60%). Propylparaben, butylparaben and benzylparaben are forbidden in food samples, their detection rates were 49.4, 21.2 and 4.7%, respectively. Therefore, our study suggests that Brazilian population may be exposed to estrogenic not allowed parabens and their harmful effects through the intake of sports food supplements.

scholarly journals High-Performance Liquid Chromatography-Tandem Mass Spectrometry for Buprenorphine Evaluation in Plasma—Application to Pharmacokinetic Studies in Rabbits

Molecules ◽  
2021 ◽  
Vol 26 (2) ◽  
pp. 437
Author(s):  
Marta Tikhomirov ◽  
Błażej Poźniak ◽  
Tomasz Śniegocki
Keyword(s):  
High Performance ◽  
Pharmacokinetic Profile ◽  
Pharmacokinetic Studies ◽  
Limit Of Quantification ◽  
Reliable Determination ◽  
Main Challenge ◽  
Analytical Protocol ◽  
Liquid Chromatography Tandem Mass ◽  
Cost Efficient

The precise and reliable determination of buprenorphine concentration is fundamental in certain medical or research applications, particularly in pharmacokinetic studies of this opioid. The main challenge is, however, the development of an analytical method that is sensitive enough, as the detected in vivo concentrations often fall in very low ranges. Thus, in this study we aimed at developing a sensitive, repeatable, cost-efficient, and easy HPLC analytical protocol for buprenorphine in rabbit plasma. In order to obtain this, the HPLC-MS2 system was used to elaborate and validate the method for samples purified with liquid-liquid extraction. Fragment ions 468.6→396.2 and 468.6→414.2 were monitored, and the method resulted in a high repeatability and reproducibility and a limit of quantification of 0.25 µg/L with a recovery of 98.7–109.0%. The method was linear in a range of 0.25–2000 µg/L. The suitability of the analytical procedure was tested in rabbits in a pilot pharmacokinetic study, and it was revealed that the method was suitable for comprehensively describing the pharmacokinetic profile after buprenorphine intravenous administration at a dose of 300 µg/kg. Thus, the method suitability for pharmacokinetic application was confirmed by both the good validation results of the method and successful in vivo tests in rabbits.

scholarly journals Dilution of QuEChERS Extracts Without Cleanup Improves Results in the UHPLC-MS/MS Multiresidue Analysis of Pesticides in Tomato

2021 ◽  
Author(s):  
Fabiane M. Stringhini ◽  
Lucila C. Ribeiro ◽  
Graziela I. Rocha ◽  
Juliana D. de B. Kuntz ◽  
Renato Zanella ◽  
...  
Keyword(s):  
Matrix Effect ◽  
Practical Method ◽  
Analysis Method ◽  
Multiresidue Analysis ◽  
Limit Of Quantification ◽  
Chromatography Tandem Mass Spectrometry ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Ultrahigh Performance Liquid Chromatography ◽  
Positive Results

AbstractTomato is well-known to be one of the most cultivated and consumed vegetables worldwide and frequently contain pesticide residues. Therefore, a simple multiresidue method was established and validated to determine 129 pesticides and metabolites in tomato samples using a modified acetate QuEChERS without cleanup for sample preparation and determination by ultrahigh-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS). Dilution of the raw extract in different proportions of mobile phase was evaluated and a dilution of 10 times presented adequate results improving analysis performance while minimizing the matrix effect. Validation performed according to SANTE guideline presented satisfactory results. Practical method limit of quantification was 0.01 mg kg−1 for most compounds. Recoveries between 70 and 120% with precision ≤ 20% were found for most compounds and spike levels evaluated. Matrix effect results were not significant for most part of compounds. Method proved to be simple, robust, and effective to be applied in routine analysis. Method applicability was performed by analysis of samples commercialized in Brazil and positive results were found demonstrating the importance of the proposed method.

scholarly journals Determination of 77 Multiclass Pesticides and Their Metabolitesin Capsicum and Tomato Using GC-MS/MS and LC-MS/MS

Molecules ◽  
2021 ◽  
Vol 26 (7) ◽  
pp. 1837
Author(s):  
Harischandra Naik Rathod ◽  
Bheemanna Mallappa ◽  
Pallavi Malenahalli Sidramappa ◽  
Chandra Sekhara Reddy Vennapusa ◽  
Pavankumar Kamin ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Solid Phase ◽  
Graphitized Carbon Black ◽  
Limit Of Quantification ◽  
Gas And Liquid Chromatography ◽  
Relative Standard ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Primary Secondary Amine

A quick, sensitive, and reproducible analytical method for the determination of 77 multiclass pesticides and their metabolites in Capsicum and tomato by gas and liquid chromatography tandem mass spectrometry was standardized and validated. The limit of detection of 0.19 to 10.91 and limit of quantification of 0.63 to 36.34 µg·kg−1 for Capsicum and 0.10 to 9.55 µg·kg−1 (LOD) and 0.35 to 33.43 µg·kg−1 (LOQ) for tomato. The method involves extraction of sample with acetonitrile, purification by dispersive solid phase extraction using primary secondary amine and graphitized carbon black. The recoveries of all pesticides were in the range of 75 to 110% with a relative standard deviation of less than 20%. Similarly, the method precision was evaluated interms of repeatability (RSDr) and reproducibility (RSDwR) by spiking of mixed pesticides standards at 100 µg·kg−1 recorded anRSD of less than 20%. The matrix effect was acceptable and no significant variation was observed in both the matrices except for few pesticides. The estimated measurement uncertainty found acceptable for all the pesticides. This method found suitable for analysis of vegetable samples drawn from market and farm gates.

scholarly journals Quantitation of Benzodiazepines and Metabolites in Urine by Liquid Chromatography–Tandem Mass Spectrometry

2018 ◽  
Vol 3 (3) ◽  
pp. 397-407
Author(s):  
Yu Zi Zheng ◽  
Dustin R Bunch ◽  
Katherine Lembright ◽  
Sihe Wang
Keyword(s):  
Precise Measurement ◽  
High Sensitivity ◽  
Urine Samples ◽  
Limit Of Quantification ◽  
Internal Standards ◽  
Independent Laboratory ◽  
Chromatography Tandem Mass Spectrometry ◽  
Analytical Recovery ◽  
Liquid Chromatography Tandem Mass ◽  
Analytical Time

Abstract Background Benzodiazepines (BZDs) are central nervous system depressants that are prescribed to prevent seizures, manage anxiety, or help sleep. When misused, BZDs can lead to addiction and sometimes cause death. Measurement of BZDs in urine is used to identify their use, especially in pain management settings. LC-MS/MS is preferred for these measurements because of its high sensitivity and specificity. Here, we report an LC-MS/MS assay for measuring 7 BZDs and metabolites in urine. Methods Urine sample was incubated at 60 °C for 30 min after addition of internal standards and a β-glucuronidase solution. After centrifugation, the supernatant was diluted with methanol and water before being injected onto a C18 analytical column in an LC-MS/MS system for quantification. The analytical time between injections was 4.35 min. The analytes included 7-aminoclonazepam, α-hydroxyalprazolam, α-hydroxytriazolam, oxazepam, lorazepam, nordiazepam, and temazepam. Results The lower limit of quantification ranged from 30 ng/mL to 50 ng/mL with an analytical recovery >80% for all 7 analytes. Total CV was <10% for all analytes (3 concentration levels of 100, 2500, and 5000 ng/mL; n = 30 each). This method had 100% agreement with a GC-MS method offered by an independent laboratory for negative urine samples. For the positive urine samples, this method showed a strong correlation (R > 0.96) with the GC-MS method. Conclusions The LC-MS/MS assay allows accurate and precise measurement of 7 BZDs and metabolites in a single analytical run with a short analytical run time and broad measuring ranges.

scholarly journals Medicinal Plants Used for the Traditional Management of Diabetes in the Eastern Cape, South Africa: Pharmacology and Toxicology

Molecules ◽  
2018 ◽  
Vol 23 (11) ◽  
pp. 2759 ◽  
Author(s):  
Samuel Odeyemi ◽  
Graeme Bradley
Keyword(s):  
South Africa ◽  
Medicinal Plants ◽  
Scientific Evidence ◽  
Traditional Healers ◽  
Bioactive Molecules ◽  
Eastern Cape ◽  
Insulin Mimetic ◽  
Almost All

The use of medicinal plants for the management of diabetes mellitus is on the rise in the developing countries, including South Africa. There is increasing scientific evidence that supports the claims by the traditional healers. In this review, we compare the families of previously reported anti-diabetic plants in the Eastern Cape by rating the anti-diabetic activity, mode of action and also highlight their therapeutic potentials based on the available evidence on their pharmacology and toxicity. Forty-five plants mentioned in ethnobotanical surveys were subjected to a comprehensive literature search in the available electronic databases such as PubMed, ScienceDirect, Google Scholar and Elsevier, by using “plant name” and “family” as the keywords for the primary searches to determine the plants that have been scientifically investigated for anti-diabetic activity. The search returned 25 families with Asteraceae highly reported, followed by Asphodelaceae and Alliaceae. Most of the plants have been studied for their anti-diabetic potentials in vivo and/or in vitro, with most of the plants having a higher percentage of insulin release and inhibition against carbohydrate digesting enzymes as compared with insulin mimetic and peripheral glucose uptake. Almost all the investigated plants also inhibit oxidative stress as part of their hypoglycemic activity with less toxicity. However, the isolation of their bioactive molecules is still lacking. This review provides a resource to enable thorough assessments of the therapeutic profiles of available medicinal plants used for the management of diabetes in the Eastern Cape, South Africa. Further studies such as the identification of the active ingredients of potent plants still need to be carried out; this may lead to new molecules in drug discovery and development.

Increased levels of bisphenol A (BPA) in Thai girls with precocious puberty

2016 ◽  
Vol 0 (0) ◽  
Author(s):  
Vichit Supornsilchai ◽  
Chutima Jantarat ◽  
Wichit Nosoognoen ◽  
Sopon Pornkunwilai ◽  
Suttipong Wacharasindhu ◽  
...  
Keyword(s):  
Bisphenol A ◽  
Estrogenic Activity ◽  
Age At Onset ◽  
Ultra Performance Liquid Chromatography ◽  
Cross Sectional Study ◽  
Normal Weight ◽  
Control Groups ◽  
Limit Of Quantification ◽  
Cross Sectional ◽  
Liquid Chromatography Tandem Mass

AbstractReports on the secular trend of pubertal onset indicate a recent earlier start especially in girls. Bisphenol A (BPA), which posses estrogenic activity, might be a cause of advanced puberty. The objective of the study was to determine the association between BPA and advanced puberty.A cross-sectional study was conducted in patients with advanced puberty (n=41) compared to age-matched controls (n=47). Anthropometric measurements, estradiol, basal and gonadotropin releasing hormone (GnRH)-stimulated follicle stimulating hormone (FSH) and luteinizing hormone (LH) levels, uterine sizes, ovarian diameters and bone ages were obtained. Urinary BPA concentrations were analyzed by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC/MSMS) with the lower limit of quantification (LLOQ) of 0.05 ng/mL.The median adjust-BPA concentration in advanced puberty group was higher than in control groups [1.44 vs. 0.59 μg/g creatinine (Cr): p<0.05]. We also found that the median adjust-BPA concentration in girls with advanced puberty who were overweight/obese, was greater than in the normal pubertal overweight/obese girls (1.74 vs. 0.59 μg/g Cr: p<0.05), and was in the same trend among normal weight girls with advanced and normal puberty (0.83 vs. 0.49 μg/g Cr: p=0.09), but not statistically significant.The present findings suggest that BPA exposure appears to be related to an earlier age at onset of puberty especially in obese girls.

scholarly journals Rapid and Sensitive Method for Quantitative Determination of Lopinavir and Ritonavir in Human Plasma by Liquid Chromatography- Tandem Mass Specrtometry

2009 ◽  
Vol 6 (1) ◽  
pp. 223-230 ◽  
Author(s):  
G. A. Temghare ◽  
S. S. Shetye ◽  
S. S. Joshi
Keyword(s):  
Liquid Chromatography ◽  
Human Plasma ◽  
Solid Phase ◽  
Internal Standard ◽  
Therapeutic Monitoring ◽  
Tandem Mass ◽  
Limit Of Quantification ◽  
Liquid Chromatography Tandem Mass ◽  
Sensitive Method

A rapid and sensitive liquid chromatography-mass spectrometric (LC-MS-MS) method for the simultaneous determination of lopinavir and ritonavir in human plasma using abacavir as internal standard has been developed and validated. Sample preparation of plasma involved solid phase extraction. Detection was performed using an Applied Biosystems Sciex API 2000 Mass spectrometer. The assay of lopinavir and ritonavir was linear over the range of 50 ng mL-1to 20000 ng mL-1and 20 ng mL-1to 3000 ng mL-1 respectively with a precision of <15% and accuracy in the range of 85-115%. The limit of quantification in plasma for lopinavir and ritonavir was 50 ng mL-1and 20 ng mL-1respectively. The described method has the advantage of being rapid and easy and it could be applied in therapeutic monitoring of these drugs in human plasma

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