scholarly journals Development and Validation of a UHPLC-ESI-MS/MS Method for Quantification of Oleandrin and Other Cardiac Glycosides and Evaluation of Their Levels in Herbs and Spices from the Belgian Market

Toxins ◽  
2020 ◽  
Vol 12 (4) ◽  
pp. 243 ◽  
Author(s):  
Svetlana V. Malysheva ◽  
Patrick P. J. Mulder ◽  
Julien Masquelier
Keyword(s):  
Cardiac Glycosides ◽  
Solid Phase ◽  
Plant Secondary Metabolites ◽  
Naturally Occurring ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass ◽  
Repeatability And Reproducibility ◽  
Culinary Herbs ◽  
The Mean ◽  
Development And Validation

Cardiac glycosides (CGs) are naturally occurring plant secondary metabolites that can be toxic to humans and animals. The aim of this work was to develop a targeted analytical method utilizing liquid chromatography—tandem mass spectrometry (LC-MS/MS) for quantification of these plant toxins in a herbal-based food and human urine. The method included oleandrin, digoxin, digitoxin, convallatoxin, and ouabain. Samples of culinary herbs were extracted with acetonitrile and cleaned using Oasis® MAX solid-phase extraction (SPE), while samples of urine were diluted with acidified water and purified on Oasis® HLB SPE cartridges. Limits of quantification were in the range of 1.5–15 ng/g for herbs and 0.025–1 ng/mL for urine. The mean recovery of the method complied with the acceptable range of 70–120% for most CGs, and relative standard deviations were at maximum 14% and 19% for repeatability and reproducibility, respectively. Method linearity was good with calculated R² values above 0.997. The expanded measurement uncertainty was estimated to be in the range of 7–37%. The LC-MS/MS method was used to examine 65 samples of culinary herbs and herb and spice mixtures collected in Belgium, from supermarkets and local stores. The samples were found to be free from the analyzed CGs.

scholarly journals A Rapid Method Based on Hot Water Extraction and Liquid ChromatographyTandem Mass Spectrometry for Analyzing Tetracycline Antibiotic Residues in Cheese

2007 ◽  
Vol 90 (3) ◽  
pp. 864-871 ◽  
Author(s):  
Sara Bogialli ◽  
Cristina Coradazzi ◽  
Antonio Di Corcia ◽  
Aldo Lagana ◽  
Manuel Sergi
Keyword(s):  
Mass Spectrometry ◽  
Extraction Efficiency ◽  
Solid Phase ◽  
Signal To Noise Ratio ◽  
Hot Water ◽  
Phase Dispersion ◽  
Relative Standard ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
The Mean

Abstract A rapid, specific, and sensitive procedure for determining residues of 4 widely used tetracycline antibiotics and 3 of their 4-epimers in cheese is presented. The method is based on the matrix solid-phase dispersion (MSPD) technique followed by liquid chromatography/tandem mass spectrometry (LC/MS/MS). After dispersing samples of mozzarella, asiago, parmigiano, gruyere, emmenthal, and camembert on sand, target compounds were eluted from the MSPD column by passing through it 6 mL water heated at 70C. After acidification and filtration, 200 L of the aqueous extract was directly injected into the LC column. For analyte identification and quantification, MS data acquisition was performed in the multireaction monitoring mode, selecting 2 precursor ion-to-product ion transitions for each target compound. Hot water appeared to be an efficient extractant, because absolute recoveries were no lower than 78%. Using demeclocycline as a surrogate analyte, recoveries of analyte added to the 6 types of cheeses at the 30 ng/g level were 96117%, with relative standard deviation (RSD) not higher than 9%. Statistical analysis of the mean recovery data showed that the extraction efficiency was not dependent on the type of cheese analyzed. This result indicates that this method could be applied to other cheese types not considered here. At the lowest concentration considered, i.e., 10 ng/g, the accuracy of the method ranged between 90 and 107%, with RSDs not larger than 12%. Based on a signal-to-noise ratio of 10, limits of quantitation were estimated to be 12 ng/g.

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 Determination of 1,4-Dioxane in Household Detergents and Cleaners

2008 ◽  
Vol 91 (2) ◽  
pp. 439-444 ◽  
Author(s):  
Akiko Tanabe ◽  
Kuniaki Kawata
Keyword(s):  
Solid Phase ◽  
Stable Isotope Dilution ◽  
Household Products ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Recovery Study ◽  
The Mean ◽  
Household Detergents ◽  
Domestic Effluent

Abstract A possible human carcinogen, 1,4-dioxane, was investigated as to its concentration levels in household detergents and cleaners currently sold in Japan. A solid-phase extraction combined with stable isotope dilution and gas chromatographic/ mass spectrometric determination was evaluated for the determination of 1,4-dioxane in household products. The evaluation of the method was performed using a recovery study of 1,4-dioxane-d8 from detergent and cleaner samples. The mean overall recovery and relative standard deviation were 78 and 15, respectively. The limit of quantitation was 0.05 mg/kg. This method was satisfactorily applied to the determination of 1,4-dioxane in household products. 1,4-Dioxane was detected in 40 out of the 51 investigated samples. The concentrations ranged from 0.05 to 33 mg/kg, and the mean was 2.7 mg/kg. The mean of the products that included anionic surfactants, i.e., alkylpoly(oxyethylene)sulfates, was 7.2 mg/kg, which was higher than the 0.39 mg/kg mean for the other surfactants. Moreover, the 1,4-dioxane load/person was estimated to be 0.061 mg/day/person in Japan, which was 27 of the load from the domestic effluent.

Determination of Eight Parabens in Water-Based Food Simulants Migrated from Antibacterial Plastic Packaging by LC/MS/MS

2013 ◽  
Vol 333-335 ◽  
pp. 1993-1997
Author(s):  
Xiao Jing Li ◽  
Xi Tang ◽  
Xue Hui Zhou ◽  
Min Shi Chen ◽  
Jin Lan Dai ◽  
...  
Keyword(s):  
Acetic Acid ◽  
Solid Phase ◽  
Reversed Phase ◽  
Quantitative Detection ◽  
Distilled Water ◽  
Food Simulants ◽  
Relative Standard ◽  
Water Based ◽  
Liquid Chromatography Tandem Mass ◽  
Phase Liquid

A method based on reversed-phase liquid chromatography-tandem mass spectrometry (LC/MS/MS) combined with solid phase extraction (SPE) was developed and validated for qualitative and quantitative detection of eight parabens in three types of water-based food simulants including distilled water, 3% acetic acid, 10% alcohol. Detection limits of eight parabens after SPE procedure were 0.005-0.010 μg/L in distilled water, 0.006-0.015 μg/L in 3% acetic acid and 0.005-0.017 μg/L in 10% alcohol. The relative standard deviations (RSDs) were in the range of 1.90-8.48% for distilled wsater, 1.01-3.73% for 3% acetic acid and 5.78-12.97% for 10% alcohol. The method could make a complement for detecting parabens migrated to food and feeds.

scholarly journals Multiresidue Determination of Quinolone and Fluoroquinolone Antibiotics in Fish and Shrimp by Liquid Chromatography/Tandem Mass Spectrometry

2007 ◽  
Vol 90 (2) ◽  
pp. 604-612 ◽  
Author(s):  
Guy Dufresne ◽  
Andre Fouquet ◽  
Don Forsyth ◽  
Sheryl A Tittlemier
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Solid Phase ◽  
Tandem Mass ◽  
Fluoroquinolone Antibiotics ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass ◽  
Multiresidue Determination

Abstract A multiresidue method was developed to measure low levels of 8 fluoroquinolones (norfloxacin, ofloxacin, danofloxacin, ciprofloxacin, desethylene ciprofloxacin, enrofloxacin, sarafloxacin, and difloxacin) and 4 quinolones (oxolinic acid, flumequine, nalidixic acid, and piromidic acid). Method detection limits range from 0.1 ng/g for quinolones to 0.4 ng/g for fluoroquinolones. Average recoveries range from 57 to 96%, depending on analyte and commodity; relative standard deviations are all less than 18%. The drugs are extracted from tissues using a mixture of ethanol and 1% acetic acid, diluted in aqueous HCl, and defatted by extraction with hexane. The compounds are further isolated using cation-exchange solid-phase extraction and measured using liquid chromatography with electrospray tandem mass spectrometry detection. The method has been evaluated and applied to the analysis of salmon, trout, and shrimp. Detectable residues were observed in 10 out of 73 samples, at concentrations ranging from 0.28 to 16 ng/g.

RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR ESTIMATION OF DESVENLAFAXINE SUCCINATE BULK DRUG IN ARTIFICIAL URINE

INDIAN DRUGS ◽  
2017 ◽  
Vol 54 (05) ◽  
pp. 37-40
Author(s):  
A. S. Bansode ◽  
◽  
V. D. Shelke ◽  
S. S. Gaikwad
Keyword(s):  
Method Development ◽  
Depressive Disorders ◽  
Solid Phase ◽  
Linear Regression Analysis ◽  
Analysis Data ◽  
Hplc Method ◽  
Relative Standard ◽  
Bulk Drug ◽  
Hplc Method Development ◽  
Development And Validation

Desvenlafaxine (DSV) succinate is a novel serotonin (5HT) and nor-epinephrine reuptake inhibitor (SNRI), which is currently used for the treatment of major depressive disorders and is being studied for use in the management of vasomotor symptoms in postmenopausal women. DSV is a major active metabolite of venlafaxine. DSV has only 30 % of protein binding and approximately 45% of the total oral dose of DSV is excreted unchanged in the urine. The chromatographic separation was performed with acetonitrile and phosphate buffer in the ratio of 25:75 (v/v) at a flow rate of 1 ml/min with UV detection at 224 nm. The extraction was done using C8 solid phase cartridges. The method is validated for precision, linearity, recovery and stability as per the USFDA guideline and the results met the acceptance criteria. The linear regression analysis data for the calibration plots showed a good linear relationship (R2 = 0.995) over a concentration range of 5-30 ppm. The percentage relative standard deviation (% RSD) values of precision were

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