摘要
对用气相色谱质谱法(GC/MS)同时测定肝、肾和肉中11种β受体激动剂残留的方法进行研究。样品经pH5.2的乙酸钠缓冲溶液提取,提取液经β盐酸葡萄糖醛苷酶芳基硫酸酯酶水解,用高氯酸沉淀蛋白质,经异丙醇乙酸乙酯(6∶4,体积比)液液分配,再经阳离子交换树酯(SCX)小柱净化后,用N,O双(三甲基硅基)三氟乙酰胺衍生化。用美托洛尔为内标,同时测定11种β受体激动剂。对肝、肾和肉样品进行添加回收实验,平均回收率为71%~94%,变异系数为4.6%~18.7%,最低检测限(LOQ)为0.002~0.000mg/kg。
The method for the determination of β-agonist residues in liver, kidney and meat by gas chromatography-mass spectrometry (GC/MS) has been developed. The sample was extracted in acetate buffer of pH5.2 and the extraction was hydrolyzed by β-glucuronidase/ arylsulfatase, then the protein was precipitated with perchloricacid. The supernatant was passed through a SCX cation exchange column and derivatized with N,O-bis(trimethylsilyl) trifluoroacetamide (BSTFA). With metoprolol as internal standard, eleven β-agonists were determined at one time. The experimental results from of spiked liver, kidney and meat sample inditated that the average recoveries ranged from 71% to 94%, the variation coefficient was 4.6%0-18.7%, the limits of detection (LODs) were 0. 002-0. 005 mg/kg.
出处
《质谱学报》
EI
CAS
CSCD
2005年第3期129-137,共9页
Journal of Chinese Mass Spectrometry Society