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PLoS One. 2017 Jan 13;12(1):e0169597. doi: 10.1371/journal.pone.0169597. eCollection 2017.

A Liquid Chromatography - Tandem Mass Spectrometry Approach for the Identification of Mebendazole Residue in Pork, Chicken, and Horse.

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Imported Food Analysis Division, Seoul Regional Food and Drug Administration, 212 Mokdongjungang-ro, Yangcheon-Gu, Seoul, Republic of Korea.
Department of Biotechnology, College of Life Sciences and Biotechnology, Korea University, 5-Ka, Anam-Dong, Sungbuk-Gu, Seoul, Republic of Korea.
Korea Health Supplements Association Sub. Korea Health Supplements Institute, B-dong 101, 700 Daewangpangyo-ro, Bundang-Gu, Seongnam-si, Gyeonggi-do, Republic of Korea.
Ministry of Food and Drug Safety, 187 Osongsaengmyeong2(i)-ro, Osong-eup, Heungdeok-gu, Chungju-si, Chungcheonbuk-do, Republic of Korea.
Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, 187 Osongsaengmyeong2(i)-ro, Osong-eup, Heungdeok-gu, Chungju-si, Chungcheonbuk-do, Republic of Korea.
College of Animal Bioscience and Technology, Department of Bioindustrial Technologies, Konkuk University, Hwayang-dong, Kwangjin-gu, Seoul, Korea.
Department of Packaging Science, Clemson University, Clemson, SC, United States of America.


A confirmatory and quantitative method of liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the determination of mebendazole and its hydrolyzed and reduced metabolites in pork, chicken, and horse muscles was developed and validated in this study. Anthelmintic compounds were extracted with ethyl acetate after sample mixture was made alkaline followed by liquid chromatographic separation using a reversed phase C18 column. Gradient elution was performed with a mobile phase consisting of water containing 10 mM ammonium formate and methanol. This confirmatory method was validated according to EU requirements. Evaluated validation parameters included specificity, accuracy, precision (repeatability and within-laboratory reproducibility), analytical limits (decision limit and detection limit), and applicability. Most parameters were proved to be conforming to the EU requirements. The decision limit (CCα) and detection capability (CCβ) for all analytes ranged from 15.84 to 17.96 μgkg-1. The limit of detection (LOD) and the limit of quantification (LOQ) for all analytes were 0.07 μgkg-1 and 0.2 μgkg-1, respectively. The developed method was successfully applied to monitoring samples collected from the markets in major cities and proven great potential to be used as a regulatory tool to determine mebendazole residues in animal based foods.

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