高效液相色谱-三重四极杆质谱法测定动物肌肉中73种兽药残留

doi:10.19894/j.issn.1000-0518.210026

摘要/Abstract

摘要： 建立了可同时对动物肌肉中73种兽药残留进行测定的高效液相色谱-串联三重四极杆质谱分析方法。依据食品基质三角,根据蛋白质、脂肪含量特点对动物食品基质进行分类,采用QuEChERS法制备待分析测试的样品,对提取溶剂、净化剂等进行优化,最终确定提取溶剂为含甲酸5%的乙腈,净化剂为C18。对仪器条件进行优化,确定各目标化合物测定的色谱条件和质谱参数。待测样品经前处理后,通过HSS T3色谱柱(2.1 mm×100 mm,1.8 μm)分离,用0.1%甲酸水溶液-乙腈梯度洗脱后,在正离子模式下检测,多反应监测模式进行分析。在不同的肉类基质中,73种化合物在0.1～10 ng/mL或0.5～10 ng/mL范围内线性关系良好,相关系数r＞0.9992;除马拉硫磷外,其余化合物的检出限均小于5 μg/kg;73种化合物在两种肉类基质中低、中和高3个添加水平的平均回收率为62.1%～128.5%;重复性RSD为0.8%～11.6%。方法灵敏度好,简单、快速,适合于多种类兽药残留的检测分析。

关键词: 兽药, 高效液相色谱, 三重四极杆质谱, 测定, 残留

Abstract: A high performance liquid chromatography-tandem mass spectrometric method is established for detection of residues of 73 veterinary drugs in animal muscle tissues. Animal food is classified based on the food matrix triangle. Samples are prepared for analysis by a quick, easy, cheap, effective, rugged, and safe (QuEChERS) method. After experimental conditions such as extraction solvent and purification agent are optimized, they are finally determined to be acetonitrile containing 5% formic acid and C18. Otherwise, instrumental conditions are optimized for the determination of 73 veterinary drugs. Samples are separated on a HSS T3 column (2.1 mm×100 mm, 1.8 μm) with the mobile phase of aqueous 0.1% formic acid and acetonitrile by gradient elution. Tandem mass spectrometry is operated in the positive ion mode. Multiple reaction monitoring is used for quantification. In pork and beef, the linear relationships are in the range of 0.1~10 ng/mL or 0.5~10 ng/mL with correlation coefficients r＞0.9992 for 73 veterinary drugs. The limits of detection for these veterinary drugs are not more than 5 μg/kg except malathion. The average recoveries at three spiked concentrations vary from 66.1% to 128.5% in pork and from 62.1% to 125.3% in beef. The repeatability is 0.8%~9.6% and 1.5%~11.6% in pork and beef, respectively. This method is simple, sensitive and fast, and could be used in multi-residue analysis of veterinary drugs.

Key words: Veterinary drugs, High performance liquid chromatography, Triple quadrupole mass spectrometry, Determination, Residues

中图分类号:

O657.6

王聪, 赵晓宇, 王海燕, 曹进, 王钢力. 高效液相色谱-三重四极杆质谱法测定动物肌肉中73种兽药残留[J]. 应用化学, 2021, 38(12): 1663-1675.

WANG Cong, ZHAO Xiao-Yu, WANG Hai-Yan, CAO Jin, WANG Gang-Li. Detection of 73 Veterinary Drugs Residues in Animal Muscle Tissues by High Performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry[J]. Chinese Journal of Applied Chemistry, 2021, 38(12): 1663-1675.

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