PDF(Pubmed)
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 C18, 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：
Flunixin是一种兽用非甾体抗炎剂，其残留物已在肌肉和肝脏等组织中以其原始形式进行了研究。然而,氟尼辛作为代谢产物留在牛奶中，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牧和渔业产品来加强监测系统。比较了两种不同的方法，用有机溶剂从牛奶中提取目标化合物，用C18纯化，浓缩，并使用甲醇基溶剂重构。过滤后，使用液相色谱-串联质谱法分析最终样品。方法1是环境友好的，由于试剂的低使用，并且基于多残基，经食品药品安全部批准的多类分析方法。两种方法的准确度和精密度分别为84.6%-115%和0.7%-9.3%,分别。由于牛奶中的基质效应较低，因此它的便利性，方法1对其他基质(牛肉，鸡肉,鸡蛋,比目鱼,和虾），其回收率和变异系数根据Codex标准（CAC/GL71-2009）是足够的。氟尼辛的检测限和定量限为2-8和5-27μg/kg，5-羟基氟尼辛的检测限和定量限为2-10和6-33μg/kg，分别。该研究可用作对所有牲畜和渔业产品的兽药残留进行监管的阳性列表系统的监测方法。
