Determination of Polar Drug Residues in Sewage and Surface Water Applying Liquid Chromatography−Tandem Mass Spectrometry

2004 ◽  
Vol 76 (22) ◽  
pp. 6548-6554 ◽  
Author(s):  
Sebastian Zuehlke ◽  
Uwe Duennbier ◽  
Thomas Heberer
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Surface Water ◽  
Tandem Mass Spectrometry ◽  
Tandem Mass ◽  
Drug Residues ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

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 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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