食品科学 ›› 2012, Vol. 33 ›› Issue (8): 252-255.doi: 10.7506/spkx1002-6630-201208056

• 分析检测 • 上一篇    下一篇

基质固相分散- 超高效液相色谱- 串联质谱法同时测定畜禽肉中残留的13 种镇静药物

渠 岩1,路 勇2,冯 楠2,赵俊平2,金伟伟1,王贵双1   

  1. 1.北京市食品酿造研究所 2.北京市食品安全监控中心
  • 出版日期:2012-04-25 发布日期:2012-03-31
  • 基金资助:
    北京市科委计划项目(D101110047710004)

Determination of Thirteen Sedative Residues in Meat by Matrix Solid Phase Dispersion-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

QU Yan1,LU Yong2,FENG Nan2,ZHAO Jun-ping2,JIN Wei-wei1,WANG Gui-shuang1   

  1. (1. Beijing Food Brewing Institute, Beijing 100050, China; 2. Beijing Municipal Center for Food Safety Monitoring, Beijing 100041, China)
  • Online:2012-04-25 Published:2012-03-31

摘要: 建立同时测定畜禽肉中13种镇静药物(阿普唑仑、咪达唑仑、三唑仑、艾司唑仑、奥沙西泮、地西泮、硝西泮、氯硝西泮、卡马西平、利多卡因、苯巴比妥、异戊巴比妥、司可巴比妥)残留量的基质固相分散-超高效液相色谱-串联质谱方法。样品经基质固相分散样品制备试剂盒净化后,进行超高效液相色谱-串联质谱分析,采用多反应监测模式,外标法定量。采用BEH C18液相色谱柱分离,以10mmol/L乙酸铵溶液-甲醇为流动相进行梯度洗脱。结果表明:13种镇静药物的方法检出限为0.05~3μg/kg,线性范围内低、中、高3个添加水平的回收率为77.4%~100.2%,相对标准偏差为1.3%~14.8%。该方法具有简便快捷、灵敏度高、结果准确等特点,适用于对上述镇静药物在畜禽肉中残留的检测。

关键词: 镇静药, 超高效液相色谱-串联质谱, 基质固相分散, 畜禽肉

Abstract: A matrix solid phase dispersion (MSPD) and ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method has been developed for the simultaneous determination of alprazolam, midazolam, triazolam, estazolam, oxazeoam, diazepam, nitrazepam, clonazepam, carbamazepin, lidocaine, phenobarbita, amobarbital and secobarbita residues in meat. Sample extract was cleaned up using an MSPD kit before UPLC-MS/MS. The analytes were monitored under multi-reaction monitoring (MRM) mode and quantified by an external standard method. The chromatographic separation was achieved on a BEH C18 column using a mobile phase composed of 10 mmol/L ammonium acetate and methanol through gradient elution. The results showed that the limits of detection for 13 sedatives ranged between 0.05 and 3 μg/kg. The average spike recoveries for the sedatives in a blank pork sample at three spike levels were 77.4%-100.2% with relative standard deviation (RSD) of 1.3%-14.8% (n =3). The method was simple, rapid, sensitive, accurate and applicable for the determination of 13 sedative residues in meat.

Key words: sedative drug, ultra performance liquid chromatography-tandem mass spectrometry, matrix solid phase dispersion (MSPD), meat

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