Determination of Anthelmintic and Antiprotozoal Drug Residues in Fish Using Liquid Chromatography-Tandem Mass Spectrometry
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....
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MDPI AG
2021-04-01
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author | Eunjung Kim Sihyun Park Hyunjin Park Jangduck Choi Hae Jung Yoon Jeong-Han Kim |
author_facet | Eunjung Kim Sihyun Park Hyunjin Park Jangduck Choi Hae Jung Yoon Jeong-Han Kim |
author_sort | Eunjung Kim |
collection | DOAJ |
description | 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, <i>v</i>/<i>v</i>), followed by phase separation (salting out) with MgSO<sub>4</sub> and NaCl (4:1, <i>w</i>/<i>w</i>). 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<sup>−1</sup> to 4.8 μg kg<sup>−1</sup> 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. |
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language | English |
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spelling | doaj.art-bf706964849344fb99cb86a0ae5edcef2023-11-21T17:37:40ZengMDPI AGMolecules1420-30492021-04-01269257510.3390/molecules26092575Determination of Anthelmintic and Antiprotozoal Drug Residues in Fish Using Liquid Chromatography-Tandem Mass SpectrometryEunjung Kim0Sihyun Park1Hyunjin Park2Jangduck Choi3Hae Jung Yoon4Jeong-Han Kim5Pesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Osong, Cheongju 28159, KoreaPesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Osong, Cheongju 28159, KoreaPesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Osong, Cheongju 28159, KoreaPesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Osong, Cheongju 28159, KoreaPesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Osong, Cheongju 28159, KoreaPesticide Chemistry and Toxicology Laboratory, Department of Agricultural Biotechnology and Research Institute of Agriculture and Life Sciences, Seoul National University, Seoul 08826, KoreaThe 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, <i>v</i>/<i>v</i>), followed by phase separation (salting out) with MgSO<sub>4</sub> and NaCl (4:1, <i>w</i>/<i>w</i>). 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<sup>−1</sup> to 4.8 μg kg<sup>−1</sup> 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.https://www.mdpi.com/1420-3049/26/9/2575anthelminticsantiprotozoalsLC-MS/MSresiduesfishery product |
spellingShingle | Eunjung Kim Sihyun Park Hyunjin Park Jangduck Choi Hae Jung Yoon Jeong-Han Kim Determination of Anthelmintic and Antiprotozoal Drug Residues in Fish Using Liquid Chromatography-Tandem Mass Spectrometry Molecules anthelmintics antiprotozoals LC-MS/MS residues fishery product |
title | Determination of Anthelmintic and Antiprotozoal Drug Residues in Fish Using Liquid Chromatography-Tandem Mass Spectrometry |
title_full | Determination of Anthelmintic and Antiprotozoal Drug Residues in Fish Using Liquid Chromatography-Tandem Mass Spectrometry |
title_fullStr | Determination of Anthelmintic and Antiprotozoal Drug Residues in Fish Using Liquid Chromatography-Tandem Mass Spectrometry |
title_full_unstemmed | Determination of Anthelmintic and Antiprotozoal Drug Residues in Fish Using Liquid Chromatography-Tandem Mass Spectrometry |
title_short | Determination of Anthelmintic and Antiprotozoal Drug Residues in Fish Using Liquid Chromatography-Tandem Mass Spectrometry |
title_sort | determination of anthelmintic and antiprotozoal drug residues in fish using liquid chromatography tandem mass spectrometry |
topic | anthelmintics antiprotozoals LC-MS/MS residues fishery product |
url | https://www.mdpi.com/1420-3049/26/9/2575 |
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