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

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

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。

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.