PRiME HLB固相萃取/超高效液相色谱-串联质谱法快速检测牛肝中18种促生长剂类药物残留

建立了PRiME HLB固相萃取/超高效液相色谱-串联质谱(UPLC-MS/MS)高通量快速检测牛肝中8种激素、6种β-受体激动剂及4种抗生素类促生长剂药物的方法。分别对色谱分离条件、MS/MS检测参数及样品前处理进行了优化。样品经β-葡萄糖醛苷酶/芳基硫酯酶酶解后,以甲醇和乙腈-甲醇(90∶10,体积比)分步提取后,直接通过PRiME HLB净化,收集流出液氮气吹干后以乙腈-水(3∶7,体积比)复溶,供UPLC-MS/MS检测。结果表明18种化合物在1.0~100.0μg/L范围内线性关系良好,相关系数均大于0.990;方法检出限(LOD)为0.07~0.78μg/kg,定量下限(LOQ)为0.23~2.58μg/kg。在3个加标水平下(0.5、1.0、5.0μg/kg)的回收率为67.5%~102.0%,相对标准偏差(RSD)均小于15%。该方法简单、快速、准确,适用于动物组织中多种促生长剂类药物的同时检测。

Rapid Determination of 18 Growth Promoting Agents in Bovine Liver by UPLC-MS/MS Coupled with PRiME HLB SPE Clean-up

A method was developed for the rapid detection of 8 hormones,6 β-receptor agonists and 4 antibiotics growth promoting agents in bovine liver by PRiME HLB solid-phase extraction/ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS).The chromatographic separation conditions,MS/MS detection parameters and sample pretreatment were optimized,respectively.The sample was firstly added NH4OAc buffer solution(pH 5.2),and hydrolyzed with a mixed solution ofβ-glucuronidase/sulfatase,then extracted with methanol(MeOH) and acetonitrile (ACN)-MeOH(90 ∶ 10,by volume) step by step,finally purified with PRiME HLB.The effluent was collected and concentrated to dryness,and redissolved with ACN-water(3 ∶ 7,by volume) for UPLC-MS/MS detection.The results showed that 18 kinds of compounds had good linear relationships in the range of 1.0-100.0 μg/L with their correlation coefficients higher than 0.990.The detection limits(LODs) ranged from 0.07-0.78 μg/kg,and the quantitation limits(LOQs) ranged from 0.23 -2.58 μg/kg.The average recoveries of 18 compounds at three spiked levels(0.5,1.0,5.0 μg/ kg) were in the range of 67.5％-102.0％ with relative standard deviations(RSDs) less than 15％.The method was simple,rapid and accurate,and was suitable for the simultaneous detection of 18 growth promoting agents in animal tissues.