Determination of 90 Prohibited Drugs Residues in Poultry Eggs by QuEChERS/Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

CHEN Rong; LIU Yu-xing; WANG Ze-lin; LI Shu-cai; ZHANG Jing; SHAO Bing

doi:10.19969/j.fxcsxb.23070301

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Determination of 90 Prohibited Drugs Residues in Poultry Eggs by QuEChERS/Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

Scientific Papers | 更新时间：2023-10-18

- Determination of 90 Prohibited Drugs Residues in Poultry Eggs by QuEChERS/Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
- Journal of Instrumental Analysis Vol. 42, Issue 10, Pages: 1291-1300(2023)
- 作者机构：
  
  1.北京市疾病预防控制中心食物中毒诊断溯源技术北京市重点实验室，北京 100013
  2.四川省食品检验研究院，四川成都 611731
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.23070301
  CLC：
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陈容,刘育形,王泽林等.QuEChERS/超高效液相色谱-串联质谱法测定禽蛋中90种禁用药物残留[J].分析测试学报,2023,42(10):1291-1300.

CHEN Rong,LIU Yu-xing,WANG Ze-lin,et al.Determination of 90 Prohibited Drugs Residues in Poultry Eggs by QuEChERS/Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(10):1291-1300.
陈容,刘育形,王泽林等.QuEChERS/超高效液相色谱-串联质谱法测定禽蛋中90种禁用药物残留[J].分析测试学报,2023,42(10):1291-1300. DOI： 10.19969/j.fxcsxb.23070301.

CHEN Rong,LIU Yu-xing,WANG Ze-lin,et al.Determination of 90 Prohibited Drugs Residues in Poultry Eggs by QuEChERS/Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(10):1291-1300. DOI： 10.19969/j.fxcsxb.23070301.

摘要

建立了禽蛋中90种禁用药物的QuEChERS/超高效液相色谱-三重四极杆串联质谱（UPLC-QqQ-MS）检测方法。样品以0.2%甲酸-乙腈水溶液（3∶1，体积比）超声提取，加入25 mg Na,2,EDTA螯合基质中的金属离子，用EMR-lipid 填料净化后采用ACQUITY UPLC HSS T3柱（2.1 mm×100 mm，1.8 μm）分离，正离子模式以0.1%甲酸水-甲醇为流动相，负离子模式以水-乙腈为流动相进行梯度分离，以多反应监测（MRM）方式扫描，标准曲线内标法定量。结果表明：目标物在各自质量浓度范围内呈良好的线性关系，相关系数（,r,2,）不小于0.99，检出限（LOD）和定量下限分别为0.05~1 μg/kg和0.1~3 μg/kg，鸡蛋的回收率为60.8%~111%，相对标准偏差为1.6%~18%，106件实际样品共检出7种药物。该方法操作简捷、准确性高，可实现禽蛋中违禁药物残留的高通量快速检测。

Abstract

To establish a method for the determination of prohibited drugs in poultry eggs by ultra performance liquid chromatography-tandem triple quadrupole mass spectrometry（UPLC-QqQ-MS），samples were extracted and purified using QuEChERS method. The drugs were extracted with 0.2% formic acid-acetonitrile solution（3∶1，by volume），and 25 mg of Na,2,EDTA was added to chelate the metal ions in the matrix，and the separation was performed on an ACQUITY UPLC HSS T3 column（2.1 mm×100 mm，1.8 μm） after cleanup with EMR-lipid packing. The separation was carried out by gradient separation with 0.1% formic acid aqueous solution-methanol as mobile phase in positive ion mode and water-acetonitrile as mobile phase in negative ion mode，which was scanned by multi-reaction monitoring（MRM） mode and quantified by the standard curve internal standard method. The results showed that target compounds obtained good linear relationship in their respective mass concentration ranges，with correlation coefficients（,r,2,） not less than 0.99. The limits of detection（LODs） and the limits of quantitations（LOQs） for the 90 compounds were determined to be 0.05-1 μg/kg and 0.1-3 μg/kg，respectively. Average recoveries of these compounds in eggs were 60.8%-111%，and the relative standard deviations were 1.6%-18%，which met the requirements of multiple veterinary drug residues. A total of 7 prohibited drugs were detected in 106 samples. This method can be used for the high-throughput rapid detection of prohibited drug residues in poultry eggs with a simple，accurate and low-cost procedure.

关键词

QuEChERS超高效液相色谱-串联质谱违禁药物禽蛋

Keywords

QuEChERSultra performance liquid chromatography-tandem mass spectrometryprohibited drugspoultry eggs

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