超高效液相色谱-串联质谱法检测卤肉中36种兽药残留

张飞; 王远; 马小宁; 张金磊; 巩婧婷; 付明鑫

doi:10.13386/j.issn1002-0306.2022080155

超高效液相色谱-串联质谱法检测卤肉中36种兽药残留

Determination of 36 Veterinary Drug Residues in Cooked Meat by Ultra Performance Liquid Chromatography-tandem Mass Spectrometry

摘要

摘要: 建立了卤肉中金刚烷胺、磺胺类、喹诺酮类及氯霉素类等36种兽药残留的检测方法。卤肉样品通过乙腈-水溶液（V:V=8:2）提取，PRiME HLB固相萃取柱净化，配有电喷雾离子源（ESI±）的超高效液相色谱-串联质谱（UPLC-MS/MS），在正负离子多反应监测（MRM）模式下同时测定，基质匹配标准曲线定量。结果表明，所研究的36种兽药在0.5~20.0 ng/mL浓度范围内均呈良好线性关系（R²>0.999）。本方法中36种药物的检出限均为0.10 μg/kg，定量限均为0.33 μg/kg，在高中低3个不同浓度（0.5，1.0和5.0 μg/kg）36种兽药的添加回收率为70.8%~106.9%，相对标准偏差（RSD, n=6）0.2%~6.2%。该研究建立的方法操作简单、准确性高、回收率和重现性好，可同时对卤肉中的36种兽药残留进行测定。

Abstract: A method was developed for the determination of amantadine sulfonamides, quinolones and chloramphenicols in cooked meat. The samples were extracted with acetonitrile-water mixtures (V:V=8:2), purified with PRiME HLB solid phase extraction column. 36 veterinary drugs were determined by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with an electrospray ion source (ESI±) in positive and negative ion switching scanning mode. The results showed that the 36 veterinary drugs showed a good linear relationship in the concentration range of 0.5~20.0 ng/mL (R²>0.999). The limits of detection were 0.10 μg/kg and the limits of quantitation were 0.33 μg/kg. The average recovery was 70.8%~106.9% in the range of high, medium and low concentrations (0.5, 1.0 and 5.0 μg/kg). The relative standard deviations (RSD, n=6) was 0.2%~6.2%. The method is simple, sensitive and accurate, and could be used for the determination of 36 veterinary drug residues in cooked meat.