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采用QuEChERS结合超高效液相色谱-串联质谱法(UPLC-MS/MS)测定动物源性食品中的兽药。

Determination of veterinary drugs in foods of animal origin by QuEChERS coupled with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).

作者信息

Sun Qianran, Liu Jun, Gou Yuan, Chen Tieyuan, Shen Xiaofang, Wang Tao, Li Yongli, He Huizhen, Deng Huidan, Hua Yi

机构信息

Technology Center, Chengdu Customs, Chengdu 610041, China.

Technology Center, Chengdu Customs, Chengdu 610041, China.

出版信息

J Chromatogr A. 2025 Mar 15;1744:465726. doi: 10.1016/j.chroma.2025.465726. Epub 2025 Jan 26.

DOI:10.1016/j.chroma.2025.465726
PMID:39893914
Abstract

A method using QuEChERS coupled with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for the determination of the residues of 19 veterinary drugs in ten animal-derived matrices, including beef, pork, sheep, horse, chicken, prawn, fish, liver, milk, and fat. This method was based on the enactment of veterinary drug compounds by Korea, Canada, the United States, and the European Union in recent years. The samples were extracted using 85% acetonitrile and separated on an ACQUITY UPLC HSS T3 column (2.1 mm × 100 mm, 1.8 μm) with a gradient elution of methanol-0.2% formic acid water as the mobile phase. The detection of the analytes was achieved through the use of positive ion electrospray ionization (ESI) and multiple reaction monitoring (MRM) modes, while the quantification was conducted via the matrix-matched external standard method. Following optimization, the linearity of the target veterinary residues in the ten matrices was observed to be satisfactory, having a range of 0.5-50.0 ng/mL (R > 0.991). The limits of detection (LOD) were in the range of 0.01-1.29 μg/kg, while the limits of quantification (LOQ) were in the range of 0.02-4.31 μg/kg. The recoveries were observed to be in the range of 60.6-117.7 %, with relative standard deviations (RSDs) of ≤20.6 %. The method is straightforward and highly sensitive, and it satisfies the maximum limits set by the relevant standards of Korea, Canada, the USA, and the EU. It is well-suited for the rapid screening, qualitative, and quantitative analyses of metomidate, acetanilide, dl-methylephedrine, and other substances in foods of animal origin, providing technical assistance for cross-border food safety and testing.

摘要

建立了一种采用QuEChERS结合超高效液相色谱-串联质谱法(UPLC-MS/MS)测定牛肉、猪肉、羊肉、马肉、鸡肉、对虾、鱼肉、肝脏、牛奶和脂肪等10种动物源性基质中19种兽药残留的方法。该方法基于韩国、加拿大、美国和欧盟近年来颁布的兽药化合物。样品用85%乙腈提取,在ACQUITY UPLC HSS T3柱(2.1 mm×100 mm,1.8μm)上分离,以甲醇-0.2%甲酸水为流动相进行梯度洗脱。通过正离子电喷雾电离(ESI)和多反应监测(MRM)模式检测分析物,采用基质匹配外标法进行定量。经过优化,观察到10种基质中目标兽药残留的线性良好,范围为0.5 - 50.0 ng/mL(R>0.991)。检测限(LOD)在0.01 - 1.29μg/kg范围内,定量限(LOQ)在0.02 - 4.31μg/kg范围内。回收率在60.6% - 117.7%之间,相对标准偏差(RSD)≤20.6%。该方法操作简便、灵敏度高,满足韩国、加拿大、美国和欧盟相关标准设定的最大限量要求。适用于动物源性食品中米托咪酯、乙酰苯胺、dl-甲基麻黄碱等物质的快速筛查、定性和定量分析,为跨境食品安全检测提供技术支持。

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