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 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 Determination of Insecticides in Honey by Matrix Solid-Phase Dispersion and Gas Chromatography with Nitrogen–Phosphorus Detection and Mass Spectrometric Confirmation

2002 ◽  
Vol 85 (1) ◽  
pp. 128-133 ◽  
Author(s):  
Consuelo Sánchez-Brunete ◽  
Beatriz Albero ◽  
Ester Miguel ◽  
José Luis Tadeo
Keyword(s):  
Solid Phase ◽  
Single Step ◽  
Organophosphorus Insecticides ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Relative Standard ◽  
The Matrix ◽  
Low Volume ◽  
Nitrogen Phosphorus

Abstract A multiresidue method was developed for the determination of 12 organophosphorus insecticides (diazinon, parathion methyl, fenitrothion, pirimiphosmethyl, malathion, fenthion, chlorpyrifos, quinalphos, methidathion, ethion, azinphosmethyl, coumaphos), one carbamate (pirimicarb), and one amidine (amitraz) in unifloral and multifloral honeys. The analytical procedure was based on the matrix solid-phase dispersion of honey on a mixture of Florisil and anhydrous sodium sulfate in small glass columns and subsequent extraction with a low volume of hexane–ethyl acetate (90 + 10, v/v), assisted by sonication. The insecticide residues were determined by capillary chromatography with nitrogen–phosphorus detection and confirmed by mass spectrometry. Average recoveries at the 0.05–0.5 μg/g levels were >80% for organophosphorus insecticides and about 60% for the other insecticides, pirimicarb and amitraz, with relative standard deviations <10%. The detection limit for the different insecticides ranged between 6 and 15 μg/kg. The main advantages of the proposed method are that extraction and cleanup are performed in a single step with a low volume of organic solvent. The method is simple, rapid, and less laborious than conventional methods. Several Spanish honeys were analyzed with the proposed method and no residues of the studied insecticides were found.

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.

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