色谱

色谱 ›› 2014, Vol. 32 ›› Issue (8): 867-873.DOI: 10.3724/SP.J.1123.2014.03029

• 技术与应用 • 上一篇    下一篇

QuEChERS结合高效液相色谱-串联质谱法测定饲料中的18种β-兴奋剂

郑玲, 吴玉杰, 赵永锋, 李丽华, 马燕娟   

  1. 广西出入境检验检疫局, 广西 南宁 530021
  • 收稿日期:2014-03-19 修回日期:2014-04-22 出版日期:2014-08-08 发布日期:2014-08-01
  • 通讯作者: 吴玉杰，E-mail：wyjhappy_2001@163.com
  • 基金资助:

    广西科技厅2012重大专项课题（桂科重：1222003-2-1）.

Simultaneous determination of 18β-agonist residues in feed using QuEChERS sample preparation and high performance liquid chromatography-tandem mass spectrometry

ZHENG Ling, WU Yujie, ZHAO Yongfeng, LI Lihua, MA Yanjuan   

  1. Guangxi Entry-Exit Inspection and Quarantine Bureau, Nanning 530021, China
  • Received:2014-03-19 Revised:2014-04-22 Online:2014-08-08 Published:2014-08-01

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摘要：

建立了饲料中克仑特罗、莱克多巴胺、喷布特罗、妥布特罗等18种β-兴奋剂的QuEChERS结合高效液相色谱-串联质谱的检测方法。饲料样品加水分散后经4%（v/v）氨水乙腈提取，加入25 mg十八烷基硅烷（C18）和50 mg N-丙基乙二胺（PSA）吸附剂分散固相萃取净化后，以高效液相色谱-串联质谱进行定性和定量分析。采用Agilent Zorbax Eclipse XDB-C18 （50 mm×4.6 mm，1.8 μm）分析柱，以甲醇-0.1%（v/v）甲酸水溶液为流动相进行梯度洗脱，串联质谱在多反应监测（MRM）正离子模式下进行检测，基质外标法定量。结果表明，18种待测物在质量浓度为5~200 μg/L范围内线性关系良好，相关系数为0.9912~0.9995；在0.05、0.1、0.5 mg/kg 3个浓度加标水平下，饲料中18种β-兴奋剂的平均回收率为78.4%~107.1%，相对标准偏差（RSD）为3.5%~12.3%，定量限（以信噪比≥10计）均为0.05 mg/kg。该方法准确、灵敏，前处理简单，可作为饲料中克仑特罗等18种β-兴奋剂筛选和确认的检测方法。

关键词: β-兴奋剂, QuEChERS, 高效液相色谱-串联质谱, 饲料

Abstract:

A multi-residue method was developed for the simultaneous determination of 18 β-agonist residues (clenbuterol, ractopamine, penbutolol, tulobuterol, etc) in feed by using QuEChERS sample preparation and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The feed samples were dispersed by water, then the analytes were extracted with acetonitrile containing 4%(v/v) ammonia and cleaned up by QuEChERS method with 25 mg octadecylsilyl (C18) and 50 mg primary secondary amine (PSA) adsorbents. The separation of compounds was carried on an Agilent ZORBAX Eclipse XDB-C18 column (50 mm×4.6 mm, 1.8 μm) by a gradient elution using methanol-0.1%(v/v) formic acid aqueous solution as mobile phase. The analytes were detected by tandem mass spectrometry under multiple reaction monitoring (MRM) mode with positive electrospray ionization (ESI+) and quantified by the matrix-matched external standard method. The results showed that the calibration curves of the 18 β-agonists were linear in the range of 5-200 μg/L with correlation coefficients of 0.9912-0.9995. The average recoveries of the 18 analytes at three spiked levels of 0.05, 0.1 and 0.5 mg/kg ranged from 78.4% to 107.1% with the relative standard deviations (RSDs) of 3.5%-12.3%. The limit of quantification (LOQ, S/N≥10) was 0.05 mg/kg for each analyte . The developed method is simple and sensitive, and can be applied as a screen and confirmatory method for the analysis of β-agonists in feed.

Key words: &beta, -agonists, feed, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), QuEChERS

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