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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。
A PRiME HLB solid-phase extraction / ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS) was developed for the rapid detection of 8 hormones, 6 β-agonists and 4 antibiotics in bovine liver Agent drug approach. Chromatographic separation conditions, MS / MS detection parameters and sample preparation were optimized. Samples were digested with β-glucuronidase / arylthioesterase and fractionated in methanol and acetonitrile-methanol (90:10, v / v). The samples were directly purified by PRiME HLB and the effluent nitrogen was collected and dried Reconstitute with acetonitrile-water (3: 7, volume ratio) for UPLC-MS / MS detection. The results showed that the linear range of the 18 compounds in the range of 1.0-100.0 μg / L was good, and the correlation coefficients were all greater than 0.990. The limits of detection (LOD) and the limit of quantitation (LOQ) of the 18 compounds ranged from 0.07 to 0.78 μg / kg. The recoveries were 67.5% -102.0% at 3 spiked levels (0.5, 1.0, 5.0 μg / kg) with relative standard deviations (RSDs) less than 15%. The method is simple, rapid and accurate and is suitable for simultaneous detection of various growth-promoting drugs in animal tissues.