固相萃取-气相色谱/质谱法同时检测动物组织中多种β-兴奋剂残留量的研究

The Analysis of β-agonists Residue in Animal Tissues by Gas Chromatography/Mass Spectrometry

建立了动物组织(肌肉、肝脏、肾脏)中妥洛特罗盐酸盐、异丙肾上腺素、硫酸特布他林、硫酸沙丁胺醇、盐酸克伦特罗、克伦潘特罗、波洛母特罗、盐酸羟苄羟麻黄碱、非诺特罗盐酸盐、莱克多巴胺等10种β-兴奋剂残留量的气相色谱-质谱法检测方法。样品经pH5.2乙酸钠溶液提取,提取液依次经乙酸乙酯-异丙醇(60∶40)混合溶剂和叔丁基甲醚-异丙醇(5∶1)萃取净化,再经Strata-X-C阳离子交换柱(500 mg,3cc)净化后,BSTFA∶TMCS(99∶1)衍生剂衍生,采用HP-5 MS(30 m×0.25 mm×0.25μm)色谱柱进行气相色谱-质谱法分析。10种β-兴奋剂类兽药检出限1μg/kg～5μg/kg,室内平均回收率59.1%～77.4%,变异系数(CV%)0.87～7.04。

The aim of this study was to develop an analytical method for the simultaneous determination of ten β-agonists residues of including ritodrine tulobuterol,clenbuterol,terbutaline,salbutamol,clenpenterol,DL-isoprenaline,fenoterol,bromobuterol and ractopamine in animal tissues by means of GC-MS.β-agonists were extracted with sodium acetate buffer solution of pH 5.2 followed by vortex and the ultrasound-assisted extraction,and was purified using ethyl acetate:isopropyl alcohol(60∶40) and tert-butyl ether:isopropanol(5∶1) two kinds mixed solvent to extract.The Strata-X-C solid phase extraction(SPE) column were used to clean up without any significant loss of growth β-agonists.The target components were derivatized with BSTFA∶TMCS(99∶1).The method detection limits were 1-5 μg/kg for all β-agonists.The average recoveries of ten β-agonists was determined as 59.1-77.4 %.Inter-precisions were 0.87%-7.04%.The detection limit was below the minimum required performance limits(MRPLs) established by the European Community(EC).The real sample tests showed this method can be used for the sensitive and accurate determination of multi-β-agonists residues in biological samples.