scholarly journals Determination of Anthelmintic and Antiprotozoal Drug Residues in Fish Using Liquid Chromatography-Tandem Mass Spectrometry

Molecules ◽  
2021 ◽  
Vol 26 (9) ◽  
pp. 2575
Author(s):  
Eunjung Kim ◽  
Sihyun Park ◽  
Hyunjin Park ◽  
Jangduck Choi ◽  
Hae-Jung Yoon ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Tandem Mass ◽  
Drug Residues ◽  
Simple Modification ◽  
Chromatography Tandem Mass Spectrometry ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass

The objective of this study is to develop a comprehensive and simple method for the simultaneous determination of anthelmintic and antiprotozoal drug residues in fish. For sample preparation, we used the “quick, easy, cheap, effective, rugged, and safe” (QuEChERS) method with a simple modification. The sample was extracted with water and 1% formic acid in acetonitrile/methanol (MeCN/MeOH) (95:5, v/v), followed by phase separation (salting out) with MgSO4 and NaCl (4:1, w/w). After centrifugation, an aliquot of the extract was purified by dispersive solid-phase extraction (d-SPE) prior to liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis. The method was validated at three concentration levels for all matrices, in accordance with the Codex guidelines (CAC/GL-71). Quantitative analysis was performed using the method of matrix-matched calibration. The recoveries were between 60.6% and 119.9%, with coefficients of variation (CV) <30% for all matrices. The limit of quantitation (LOQ) of the method ranged from 0.02 μg kg−1 to 4.8 μg kg−1 for all matrices. This comprehensive method can be used for the investigation of both anthelmintic and antiprotozoal drugs belonging to different chemical families in fishery products.

scholarly journals Determination of Cyclamate in Foods by Ultraperformance Liquid Chromatography/Tandem Mass Spectrometry

2008 ◽  
Vol 91 (5) ◽  
pp. 1095-1102 ◽  
Author(s):  
Robert Sheridan ◽  
Thomas King
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Sample Preparation ◽  
Tandem Mass Spectrometry ◽  
Limit Of Detection ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass

Abstract A highly sensitive and selective method that requires minimal sample preparation was developed for the confirmation and quantitation of cyclamate in a variety of foods by high-performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS). Sample preparation consisted of homogenization followed by extraction and dilution of cyclamate with water. HPLC separation was achieved using a bridged ethyl hybrid C18 high-pressure column with a mobile phase consisting of 0.15 acetic acid and methanol. Under electrospray ionization negative conditions, quantitation was achieved by monitoring the fragment m/z 79.7 while also collecting parent ion m/z 177.9. Two food matrixes, diet soda and jelly, were subjected to a validation procedure in order to evaluate the applicability of the method. The cyclamate limit of detection for both matrixes was determined to be 0.050 g/g with a limit of quantitation of 0.150 g/g. The correlation coefficient of the calibration curves was &gt;0.9998 from 0.0005 to 0.100 g/mL. The method has been used for the determination of cyclamate in several foods and the results are presented.

Method Validation for Quantitative Analysis of Metribuzin in Wheat by Liquid Chromatography–Tandem Mass Spectrometry

2020 ◽  
Vol 59 (1) ◽  
pp. 47-54
Author(s):  
Dipak Kumar Hazra ◽  
Aloke Purkait ◽  
Durgesh Raghuwanshi ◽  
K Sri Rama Murthy
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Sample Preparation ◽  
Tandem Mass Spectrometry ◽  
Accurate Determination ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass

Abstract A high-performance liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was developed and validated for the accurate determination of metribuzin levels in wheat. The widespread use of this herbicide in the production of wheat is of concern and could follow as well as the need for methodology, which required simple sample preparation being needed. Validation of method was done as per single laboratory validation approach. Samples were extracted through a modified quick, cheap, effective, rugged and safe technique. Sample preparation includes extraction by acetonitrile solvent and cleans up by C18, primary secondary amine and anhydrous MgSO4 for dispersive solid-phase extraction. LC–MS/MS was calibrated at 5 calibration levels with high correlation coefficients (r2) &gt;0.995. Limit of detection and limit of quantitation of metribuzin were 0.01 and 0.03 μg/g, respectively. The mean recovery percentages lie in the range of 87–97 with standard deviation for repeatability (RSDa) &lt;10% at three spiking levels (0.03, 0.15 and 0.30 μg/g). Combined uncertainty (U = 0.0017) and expanded uncertainty (2U = 0.0033) were fairly consequential. The method may successfully be applied to other cereals samples for determination of metribuzin.

scholarly journals Determination of Deltamethrin Residues in Plant Materials by Liquid Chromatography/Tandem Mass Spectrometry with Electrospray Ionization

2006 ◽  
Vol 89 (3) ◽  
pp. 786-796 ◽  
Author(s):  
Dieter Zimmer ◽  
Christiane Philipowski ◽  
Birgit Posner ◽  
Agnes Gnielka ◽  
Edgar Dirr ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Electrospray Ionization ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass

Abstract This paper describes a selective and sensitive method that uses liquid chromatography/tandem mass spectrometry with positive electrospray ionization (ESI+) for the determination of deltamethrin in a variety of crops. Samples were extracted by conventional high-speed blending. Some samples required no further cleanup; others were cleaned up by gel permeation chromatography, strong cation-exchange cartridges, or partitioning with n-hexane. In the determinative step, the buffered neutral mobile phase, consisting of 10 mM ammonium acetate (pH 6.8) and methanol, and ESI+ provided strong ammonium adduct formation to [M+NH4]+ at m/z 523, and the multiple-reaction monitoring (MRM) transition at m/z 523/281 was used for the quantitation of deltamethrin. A second MRM transition at m/z 525/283 was used for confirmation. The limit of quantitation (LOQ) values were 0.01 mg/kg for edible materials and 0.05 mg/kg for nonedible materials. Mean overall recoveries at the LOQ and the 10-fold LOQ ranged from 73 to 96%, and the relative standard deviations were &lt;10% for all samples materials analyzed.

scholarly journals Determination of Macrocyclic Lactone Drug Residues in Animal Muscle by Liquid Chromatography/Tandem Mass Spectrometry

2009 ◽  
Vol 92 (1) ◽  
pp. 348-358 ◽  
Author(s):  
Limin He ◽  
Donghao Zhao ◽  
Yijuan Su ◽  
Yahong Liu ◽  
Jianrong Nie ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Macrocyclic Lactone ◽  
Tandem Mass ◽  
Drug Residues ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass

Abstract A robust, credible, and practical multiresidue method based on liquid chromatography/tandem/mass spectrometry (LC/MS/MS) was developed for the simultaneous determination of 9 macrocyclic lactone drugs (abamectin B1a, doramectin, erythromycin, ivermectin B1a, josamycin, kitasamycin, roxithromycin, tilmicosin, and tylosin A) in bovine, porcine, chicken, and sheep muscles. The drugs were extracted with acetonitrile, and the extracts were defatted with n-hexane and further cleaned up on a C18 solid-phase extraction cartridge. LC/MS/MS data acquisition was achieved by using the multiple-reaction monitoring (MRM) mode, i.e., 2 transitions, to provide a high degree of sensitivity and repeatability. Matrix-matched standard calibration curves were used to achieve the best accuracy of the method by compensating for the matrix effect. The calibration graphs were linear (r &gt;0.998) from 10 to 1000 ng/mL for erythromycin, josamycin, kitasamycin, roxithromycin, tilmicosin, and tylosin, and from 5 to 250 ng/mL for abamectin, doramectin, and ivermectin. The average recoveries of the 9 drugs were between 64.5 and 105, calculated by using matrix-matched calibration, with relative standard deviation values ranging from 1.6 to 14. The limits of detection were 0.1 g/kg for erythromycin, josamycin, roxithromycin, and tylosin; 0.2 g/kg for tilmicosin and kitasamycin; and 0.5 g/kg for abamectin, doramectin, and ivermectin. For confirmation, the MRM ratios for the 9 drug residues in the samples and the solvent were evaluated and found to be within the ratio criteria set by the guidelines of the European Union.

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