猪组织中10种β-兴奋剂类兽药残留量的气相色谱-质谱法检测

Determination of β-Agonists Residue in Pork Tissues by Gas Chromatography-Mass Spectrometry

利用气相色谱-质谱检测技术,建立了猪组织（猪肉、猪肝、猪肾）中10种β-兴奋剂类兽药残留量的检测方法。样品经乙酸钠缓冲溶液提取后,依次经液-液萃取、阳离子交换柱净化,再经双（三甲基硅烷基）三氟乙酰胺-三甲基氯硅烷（BSTFA-TMCS）衍生,气相色谱-质谱检测。在相应的质量浓度范围内,10种β-兴奋剂的质量浓度与峰面积有良好的线性关系,相关系数r2大于0.996,检出限为1~5μg/kg。对猪组织样品的室内平均回收率为59%~77%,相对标准偏差为0.87%~7.0%;室间平均回收率为63%~76%,相对标准偏差为1.5%~12.6%。方法具有简便快速、准确度和灵敏度高、重复性好等特点,适合于动物组织中β-兴奋剂的测定。

A GC-MS method was developed for the simultaneous determination of ten β-agonists residues including ritodrine,tulobuterol,clenbuterol,terbutaline,salbutamol,clenpenterol,isoprenaline,fenoterol,bromobuterol and ractopamine in animal tissues.The sample was extracted with sodium acetate buffer solution,and purified by liquid-liquid extraction and Strata-X-C cation exchange column.The target compounds were derivatized with BSTFA-TMCS and detected by GC-MS.There was a good linear relationship between peak areas and concentrations of 10 β-agonists in certain mass concentration range.The correlation coefficients（r2） were greater than 0.996.The method detection limits ranged from 1 μg/kg to 5 μg/kg for all β-agonists.The interion recoveries of ten β-agonists from spiked pork,pig liver and pig kidney samples were 59%-77%with RSDs of 0.87%-7.0%.The external recoveries were in the range of 63%-76% with RSDs of 1.5%-12.6%.The method was simple,rapid and accurate,and was suitable for the simultaneous determination of β-agonists in animal tissues.