Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, Seoul 143-701, Republic of Korea.
Natural Products Chemistry Laboratory, College of Agriculture and Life Sciences, Chonnam National University, Gwangju, Republic of Korea.
Food Chem. 2021 Jun 30;348:129105. doi: 10.1016/j.foodchem.2021.129105. Epub 2021 Jan 19.
Herein, an analytical method was developed for simultaneous determination of 12 anthelmintics (closantel, niclosamide, nitroxynil, rafoxanide, cymiazole, fluazuron, levamisole, morantel, praziquantel, pyrantel, thiophanate, and trichlorfon) in fishery products (eel, flatfish, and shrimp) using liquid-liquid extraction coupled with liquid chromatography-tandem mass spectrometry. A reversed-phase analytical column was then used to separate the analytes from various matrices. Linear matrix-matched calibration curves were generated with coefficients of determination ≥ 0.9935. Recovery rates at three spiking levels (5, 10, and 20 µg/kg) ranged between 61.58% and 119.37% with relative standard deviations ≤ 19.05%. Limits of detection were in the range of 0.3-1.6 μg/kg, whereas limits of quantification ranged between 1.0 and 5.0 μg/kg. The matrix effect was moderate with values ranging from -99.47% to 51.98%. Matrices procured from large markets tested negative for the 12 anthelmintics. The developed method proved amenable to real sample testing and can be used for simultaneous determination of target analytes in aquatic products.
本文建立了一种同时测定水产品（鳗鱼、比目鱼和虾）中 12 种驱虫药（氯硝柳胺、硝氯酚、硝碘酚腈、三氯苯达唑、苯硫胍、氟虫脲、左旋咪唑、莫能菌素、吡喹酮、噻苯达唑、涕灭威和三氯杀螨醇）的液液萃取-液相色谱-串联质谱分析方法。采用反相分析柱，可使分析物与各种基质分离。采用线性基质匹配校准曲线，相关系数均大于 0.9935。在 5、10 和 20μg/kg 三个加标水平下，回收率在 61.58%至 119.37%之间，相对标准偏差不超过 19.05%。检测限在 0.3-1.6μg/kg 之间，定量限在 1.0-5.0μg/kg 之间。基质效应中等，范围为-99.47%至 51.98%。从大型市场采集的基质检测结果均为阴性。该方法适用于实际样品检测，可用于同时测定水产品中的目标分析物。
