同位素稀释结合固相萃取快速测定动物组织中β_2-兴奋剂

Comprehensive Multi-residue Analysis of Agonists in Animal Tissue Based on Isotope Dilution and Solid Phase Extraction

本文采用同位素稀释结合固相萃取技术,测定动物组织中特布他林、克伦特罗、沙丁胺醇、莱克多巴胺4种β2-兴奋剂。动物组织加同位素内标D3-沙丁胺醇和D9-克伦特罗,经甲醇提取后,正己烷脱脂,过SLS离子交换固相萃取柱净化,用BSTFA＋1%（φ）TMCS衍生,采用GC/MS进行测定,内标法定量。实验表明,动物组织中添加2.0-10.0μg/kg浓度水平的β2-兴奋剂,方法回收率在72.5%-97.9%,相对标准偏差1.0%~11.4%,线性范围为12.5-500μg/L,样品中特布他林、克伦特罗、沙丁胺醇、莱克多巴胺最低检出限分别为0.5μg/kg、1.0μg/kg、0.5μg/kg和1.0μg/kg。

A method for multi-residue analysis of terbutaline, clenbuterol, salbutamol and ractopamine in animal tissue has been developed by gas chromatography-mass spectrometry, based on isotope dilution and solid phase extraction. The homogenized samples were spiked with isotope-labeled internal standards D3-salbutamol and D9-clenbuterol, extracted with methanol, defatted using hexane. Further cleanup was performed on a SLS cartridge and the purified residue was derivatized with bis （trimethylsilyl） trifluoroacetamide （BSTFA） ＋ 1% （φ） trimethylchlorosilane （TMCS）, quantified using internal standard method. The calibration curves were linear between 2.5 μg/L and 500 μg/L. The experimental indicated that the rates of recovery were 72.5% - 97.9% , and the relative standard deviations were 1.0% - 11.4% spiked with 2.0 - 10.0 μg/kg of the above-mentioned agonists, the detection limits corresponding were 0. 5 μg/kg, 1.0 μg/kg, 0.5 μg/kg, 1.0 μg/kg, respectively.