超高效液相色谱-质谱法测定猪尿中15种β-受体阻断剂残留

Determination of 15β-blocker Residues in Pig Urine Using Ultra-high Performance Liquid Chromatography-Mass Spectrometry

为建立一种快速测定猪尿中15种β-受体阻断剂残留的超高效液相色谱-质谱(UPLC-MS/MS)确证方法,本试验优化了分子印迹固相萃取(MISPE)净化条件及色谱、质谱条件。猪尿样品经离心后加入MISPE柱上样,依次经水、乙腈淋洗,10%乙酸甲醇洗脱,N2吹干,0.1%甲酸水-乙腈(v:v=9:1)复溶;采用ESI正离子模式在多反应监测模式下进行离子扫描,外标法定量。结果显示,猪尿中15种药物在0.1~10μg/L范围内具有良好的线性关系(R2≥0.996),检出限和定量限分别为0.03和0.10μg/L;各药物回收率在76.7%~109.2%之间,批内、批间变异系数分别在2.2%~18.7%、2.1%~19.7%之间。结果表明,本方法操作简单快速、灵敏度高、特异性好。

In order to establish an ultra-high performance liquid chromatography-mass spectrometry(UPLC-MS/MS)to rapidly determine 15 kinds ofβ-blocker residues in pig urine,the conditions for purification of molecular imprinted solid phase extraction(MISPE)as well as chromatographic and mass spectrometry were optimized in the study.Pig urine samples were centrifuged and added in the MISPE column,then rinsed with water and acetonitrile successively,eluted with 10%acetic acid methanol,dried with N2,and redissolved with 0.1%formic acid water acetonitrile(V:V=9:1);ion scanning was carried out by ESI positive ion mode under multi-reaction monitoring mode(MRM),which was quantified by external standard method.The results showed that the 15 drugs were with a good linear relationship within 0.1~10μg/L(R2≥0.996),and the limits of detection(LOD)and quantification(LOQ)were 0.03 and 0.10μg/L,respectively;the recovery rate of all the drugs ranged from 76.7%to 109.2%,and the coefficients of variation ranged 2.2%~18.7%and 2.1%~19.7%,respectively.It was concluded that the method was simple,rapid,sensitive and specific.