气相色谱-质谱法测定动物组织中残留的10种β2-兴奋剂

Multi-residue analysis of 10 β_2-agonists in animal tissues using gas chromatography-mass spectrometry

采用同位素稀释法并结合固相萃取技术,建立了动物组织中马布特罗、特布他林、卡布特罗、克伦特罗、西马特罗、沙丁胺醇、clenpenterol、苯氧丙酚胺、班布特罗、莱克多巴胺等10种β2-兴奋剂残留的气相色谱-质谱（GC-MS）检测方法。动物组织中添加同位素内标D9-克伦特罗、D3-沙丁胺醇、D5-莱克多巴胺,经无水乙醇提取、正己烷脱脂、SLS离子交换固相萃取柱净化后,用双三甲基硅基三氟乙酰胺＋1%三甲基氯硅烷衍生,再进行GC-MS测定,内标法定量。结果表明,动物组织中添加2.0-10.0μg/kg水平的β2-兴奋剂,回收率为72.8%-110.3%,相对标准偏差为1.2%-11.3%,最低检测限为0.5-1.0μg/kg。

A method for multi-residue analysis of β2-agonists, mabuterol, terbutaline, carbuterol, clenbuterol, cimaterol, salbutamol, clenpenterol, isoxsuprine, bambuterol and ractopamine in animal tissues using gas chromatography-mass spectrometry, based on isotope dilution and solid phase extraction has been developed. The homogenized sample was spiked with isotope-labeled internal standards, D9-clenbuterol, D3-salbutamol and D5-ractopamine, extracted with anhydrous alcohol, defatted using hexane, and cleaned-up on an SLS cartridge, and derivatized with N, O-bis（trimethylsilyl） trifluoro acetamide （BSTFA） ＋ 1% trimethylchlorosilane （TMCS）. The experimental results indicated that the recoveries were 72.8% - 110.3%, and the relative standard deviations were 1.2% - 1 1. 3% in blank samples spiked with the above mentioned agonists at 2.0 - 10.0 μg/kg, and the corresponding detection limits were 0.5 - 1.0 μg/kg.