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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Main Authors: Eunjung Kim, Sihyun Park, Hyunjin Park, Jangduck Choi, Hae Jung Yoon, Jeong-Han Kim
Format: Article
Language:English
Published: MDPI AG 2021-04-01
Series:Molecules
Subjects:
Online Access:https://www.mdpi.com/1420-3049/26/9/2575
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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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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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