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中国农学通报 ›› 2014, Vol. 30 ›› Issue (27): 299-303.doi: 10.11924/j.issn.1000-6850.2014-0741

所属专题: 畜牧兽医

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超高效液相色谱-串联质谱法测定猪肉中非甾体抗炎药残留量

李娜   

  1. 天津市农业质量标准与检测技术研究所
  • 收稿日期:2014-03-18 修回日期:2014-03-18 接受日期:2014-08-06 出版日期:2014-10-15 发布日期:2014-10-15
  • 通讯作者: 李娜
  • 基金资助:
    天津市农业科学院院长基金(11003)

Determination of Non-steroidal Anti-inflammatory Drugs in Porcine uscle by UPLC-MS/MS Method

  • Received:2014-03-18 Revised:2014-03-18 Accepted:2014-08-06 Online:2014-10-15 Published:2014-10-15

摘要: 研究建立了猪肉中美洛昔康、氟尼辛、卡洛芬和托芬那酸四种非甾体抗炎药残留量的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。样品中残留的药物经乙腈提取,提取液浓缩后用乙腈-0.1%甲酸水溶液溶解,正己烷液-液分配净化,最后采用电喷雾串联质谱仪在正离子多反应监测扫描(MRM)模式下进行测定,基质外标法定量。四种药物在各自的线性范围内,线性关系良好,相关系数均为0.999。对猪肉中美洛昔康、氟尼辛、卡洛芬和托芬那酸在定量限(LOQ)、2.5 倍定量限(2.5 LOQ)和5 倍定量限(5 LOQ)三个添加浓度水平下的回收率进行测定,其平均回收率在在72.1%和87.3% 之间,相对标准偏差在2.8%和6.7%之间。美洛昔康、氟尼辛、卡洛芬和托芬那酸的定量限(S/N≥10)分别为1.6、1.6、80 和8.0 μg/kg。该方法不使用固相萃取柱,简化了操作步骤,节约了检测成本,灵敏度、准确度和精密度均符合多残留检测技术的要求,可为猪肉中非甾体抗炎药残留量的测定提供技术支持。

关键词: 人为管理, 人为管理

Abstract: An ultra performance liquid chromatography-tandem mass spectrometric method was developed for the determination of the four non steroidal anti- inflammatory drugs (Meloxicam, Flunixin, Carprofen and Tolfenamic Acid) in porcine muscle. The drugs were extracted with acetonitrile, then cleaned-up by liquidliquid extraction with n-hexane, and finally analyzed by ultra performance liquid chromatography-tandem mass spectrometry (UPLC- MS/MS) in multiple reaction monitoring (MRM) mode via positive electrospray ionization. The method was validated at three fortification levels (LOQ, 2.5LOQ and 5LOQ) in porcine muscle. The validation results were as follows: the correlation coefficients of the standard calibration curves for the four non- steroidal anti- inflammatory drugs all were 0.999 over their own concentration range; the average recoveries of the four drugs were between 72.1% and 87.3% , with the relative standard deviation (RSD) between 2.8% and 6.7% ; the limits of quantification (S/N≥10) of Meloxicam, Flunixin, Carprofen and Tolfenamic Acid were 1.6, 1.6, 80 and 8.0 μg/kg. It was indicated that the method developed in this study is cheap,easy and has a good purification effect. The sensitivity, accuracy and precision of the method were all acceptable, and it can meet the requirements of the multiple residue analysis. So, this method can be further applied to investigate the anti-inflammatory residue status in porcine muscle.