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液相色谱-串联质谱法(LC-MS/MS)测定畜禽和水产品中氟尼辛及5-羟基氟尼辛残留量

Determination of Flunixin and 5-Hydroxy Flunixin Residues in Livestock and Fishery Products Using Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS).

作者信息

Park Dahae, Choi Yong Seok, Kim Ji-Young, Choi Jang-Duck, Moon Gui-Im

机构信息

Pesticides & Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation, Cheongju 28159, Korea.

College of Pharmacy, Dankook University, Cheonan 31116, Korea.

出版信息

Food Sci Anim Resour. 2024 Jul;44(4):873-884. doi: 10.5851/kosfa.2024.e24. Epub 2024 Jul 1.

Abstract

Flunixin is a veterinary nonsteroidal anti-inflammatory agent whose residues have been investigated in their original form within tissues such as muscle and liver. However, flunixin remains in milk as a metabolite, and 5-hydroxy flunixin has been used as the primary marker for its surveillance. This study aimed to develop a quantitative method for detecting flunixin and 5-hydroxy flunixin in milk and to strengthen the monitoring system by applying to other livestock and fishery products. Two different methods were compared, and the target compounds were extracted from milk using an organic solvent, purified with C, concentrated, and reconstituted using a methanol-based solvent. Following filtering, the final sample was analyzed using liquid chromatography- tandem mass spectrometry. Method 1 is environmentally friendly due to the low use of reagents and is based on a multi-residue, multi-class analysis method approved by the Ministry of Food and Drug Safety. The accuracy and precision of both methods were 84.6%-115% and 0.7%-9.3%, respectively. Owing to the low matrix effect in milk and its convenience, Method 1 was evaluated for other matrices (beef, chicken, egg, flatfish, and shrimp) and its recovery and coefficient of variation are sufficient according to the Codex criteria (CAC/GL 71-2009). The limits of detection and quantification were 2-8 and 5-27 μg/kg for flunixin and 2-10 and 6-33 μg/kg for 5-hydroxy flunixin, respectively. This study can be used as a monitoring method for a positive list system that regulates veterinary drug residues for all livestock and fisheries products.

摘要

氟尼辛是一种兽用非甾体抗炎药,其在肌肉和肝脏等组织中的残留已按原始形式进行过研究。然而,氟尼辛会以代谢物的形式残留在牛奶中,5-羟基氟尼辛已被用作其监测的主要标志物。本研究旨在开发一种定量检测牛奶中氟尼辛和5-羟基氟尼辛的方法,并通过应用于其他畜禽和水产品来加强监测系统。比较了两种不同的方法,目标化合物先用有机溶剂从牛奶中提取,再用C进行净化、浓缩,并用甲醇基溶剂复溶。过滤后,最终样品采用液相色谱-串联质谱法进行分析。方法1由于试剂使用量少而环保,且基于食品药品安全部批准的多残留、多类别分析方法。两种方法的准确度和精密度分别为84.6%-115%和0.7%-9.3%。由于牛奶中的基质效应较低且操作方便,对方法1在其他基质(牛肉、鸡肉、鸡蛋、比目鱼和虾)中进行了评估,根据食品法典标准(CAC/GL 71-2009),其回收率和变异系数均足够。氟尼辛的检测限和定量限分别为2-8μg/kg和5-27μg/kg,5-羟基氟尼辛的检测限和定量限分别为2-10μg/kg和6-33μg/kg。本研究可作为一种监测方法,用于对所有畜禽和水产品的兽药残留进行监管性的肯定列表制度。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/2ebe/11222691/bd657ca637bb/kosfa-44-4-873-g1.jpg

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