蛋白受体结合筛选-气质联用法测定动物组织中的氯霉素残留

Analysis of chloramphenicol residues in animal tissues with protein receptor binding screening and GC/MS method

建立了动物组织中氯霉素残留的蛋白受体结合筛选和GC MS分析方法。受体结合生物筛选的筛选限为0.1μg kg,假阴性率为零,其它常用抗生素的交叉反应率均<0.1%。筛选阳性样本经液液分配萃取、C18SPE固相萃取净化后衍生进行GC MS的NCI选择离子监测分析。其定量检出限为0 1μg kg,样品添加水平0 1～10μg kg时,回收率为76 2%～103 5%,相对标准偏差为7 5%～10 6%。

A protein receptor binding screening system and GC/MS confirmatory method were exploited to determine the chloramphenical (CAP) residues in animal tissues. The screening limit of the receptor binding system was 0.1 μg/kg, false negative rate was zero, and the cross-reaction rate of other commonly used antibiotics was under 0.1%. The suspected screening positive samples continued to be analyzed by GC/MS. After liquid-liquid extraction, C_(18) solid phase extraction and derivatization, the CAP-TMS were tested under selected ion monitoring mode with a negative chemical ionization source. The limit of quantification was 0.1 μg/kg. The recoveries were in the range of 76.2%～103.5% at the spiked level of 0.1～1.0 μg/kg, and the relative standard deviations were 7.5%～106%.