色谱

色谱 ›› 2015, Vol. 33 ›› Issue (8): 838-842.DOI: 10.3724/SP.J.1123.2015.04016

• 研究论文 • 上一篇    下一篇

分子印迹固相萃取-超高效液相色谱-串联质谱法测定猪肉中5种 β2-受体激动剂残留

张学亮1, 罗云敬1, 姜洁2, 路勇2, 冯楠2   

  1. 1. 北京工业大学生命科学与生物工程学院, 北京 100124;
    2. 北京市食品安全监控和风险评估中心, 北京 100041
  • 收稿日期:2015-04-13 出版日期:2015-08-08 发布日期:2015-07-27
  • 通讯作者: 罗云敬
  • 基金资助:

    北京市科委计划基金项目(Z121100000312014).

Determination of five β2-agonist residues in pork by ultra-high performance liquid chromatography-tandem mass spectrometry with molecularly imprinted solid phase extraction

ZHANG Xueliang1, LUO Yunjing1, JIANG Jie2, LU Yong2, FENG Nan2   

  1. 1. College of Life Sciences & Bio-Engineering, Beijing University of Technology, Beijing 100124, China;
    2. Beijing Municipal Food Safety Monitoring and Risk Assessment Center, Beijing 100041, China
  • Received:2015-04-13 Online:2015-08-08 Published:2015-07-27

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摘要：

建立了一种分子印迹固相萃取-超高效液相色谱-串联质谱同时测定猪肉中5种 β2-受体激动剂残留的方法。样品经过均质处理后置于乙酸铵/乙酸缓冲液中,加入内标物和β-葡萄糖醛酸酶/芳基硫酸酯酶,于55 ℃酶解2 h,调节溶液pH后通过分子印迹固相萃取柱净化,然后采用BEH C18色谱柱分离,以甲醇-0.1%(v/v)甲酸水溶液为流动相,采用梯度洗脱,在电喷雾正离子多反应监测模式下用内标法定量。检出限(LOD, S/N=3)和定量限(LOQ, S/N=10)分别为0.005~0.009 μg/kg和0.015~0.025 μg/kg。在0~10 μg/kg范围内线性关系良好,相关系数≥0.9933。添加水平为0.25、1、5 μg/kg时,回收率为80.4%~92.9%,相对标准偏差为1.2%~6.3%。该方法具有灵敏度高、重复性好、回收率高等优点,适合同时进行多种 β2-受体激动剂残留的测定。

关键词: β2-受体激动剂, 残留, 超高效液相色谱-串联质谱, 分子印迹固相萃取, 猪肉

Abstract:

An ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method with molecularly imprinted solid phase extraction for the determination of five β2-gonists residues in pork has been developed. After the sample preparation, the ammonium acetate/acetic acid buffer was added, followed by the internal standard and β-glucuronidase/arylsulfatase enzyme. The solution was incubated at 55 ℃ for 2 h. After adjusting the pH of the solution, it was purified by a molecularly imprinted solid phase extraction column, then analyzed on a BEH C18 column with methanol-0.1% (v/v) formic acid aqueous solution as the mobile phases in gradient elution mode. The MS/MS analysis was in positive ion mode and multiple reaction monitoring mode. The analytes were quantified by the internal standard method. The limits of detection (LODs, S/N=3) and the limits of quantification (LOQs, S/N=10) were 0.005-0.009 μg/kg and 0.015-0.025 μg/kg, respectively. In the range of 0-10 μg/kg, the correlation coefficients of linear calibration curves were not less than 0.9933. At the spiked levels of 0.25, 1.0 and 5.0 μg/kg, the recoveries were 80.4%-92.9% with the relative standard deviations of 1.3%-6.3%. The method is of high sensitivity, good reproducibility, high recovery, and is useful for the simultaneous determination of multiple β2-agonists residues.

Key words: β2-gonists, molecularly imprinted solid phase extraction, pork, residues, ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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