氘代同位素内标QuEChERS法测定动物尿液中3种β_2-兴奋剂药物残留量  

Determination of 3 β_2-Agonist Residues in Animal Urine by QuEChERS Method with Deuterated Isotope Internal Standard

作　　者：黄子敬 符靖雯 陈孟君 罗汉金[2] 

机构地区：[1]惠州市农产品质量安全监督检测中心,广东惠州516008 [2]华南理工大学环境与能源学院,广东广州510006

出　　处：《分析测试学报》2015年第8期880-886,共7页Journal of Instrumental Analysis

基　　金：国家自然科学基金项目(40973074);广东省科技计划项目(2005B26001118)

摘　　要：采用氘代同位素内标Qu ECh ERS法制备分析样品,气相色谱-质谱法检测动物尿液中的盐酸克伦特罗、沙丁胺醇及莱克多巴胺3种β2-兴奋剂残留量。样品经β-葡萄糖醛酸苷酶酶解后,用氨化乙酸乙酯提取,上清液经无水Mg SO4和N-丙基乙二胺（PSA）吸附剂净化后吹干衍生,气相色谱-质谱进行测定。3种β2-兴奋剂的线性良好,相关系数均大于0.998,在3个加标水平下的平均回收率为95.0%-101.0%,相对标准偏差为2.5%-6.2%,检出限（LOD）为0.3-0.6μg/L,定量下限（LOQ）为1.0-2.0μg/L。该方法操作简单、快速、稳定、精密度高,适用于动物尿液中3种β2-兴奋剂残留的快速测定。Illegal drugs added in the process of livestock production would seriously affect the food safety in our country. The residues of 3 β2-agonists （ e. g. , clenbuterol, salbutamol and ractopamine） in animal urine were prepared with deuterated isotope internal standard QuEChERS method , and analyzed by gas chromatographymass spectrometry（ GC -MS）. Samples were enzymaticed with β- glucuronidase, and extracted with ammoniation ethyl acetate, then cleansed with anhydrous MgSO4 and primary secondary amine （PSA）sorbent. After supernatant was dried and derivatized, the analysis of target compounds was performed with GC - MS. The results indicated that good linear relationships were obtained for three β2-agonists in the certain concentration with correlation coefficients greater than 0. 998. The average recoveries of 3 analytes at three spiked concentration levels ranged from 95.0% to 101.0% , with relative standard deviations（RSDs） of 2. 5% - 6. 2%. The limits of detection（LOD） were in the range of 0. 3 -0.6μg/L and the limits of quantitation（LOQ） were 1.0 -2. 0 μg/L. This method has the advantages of simplicity, rapidness, stable operation, high precision, and is suitable for the determination of three kinds of β2-agonists residues in animal urine.

关 键 词：氘代同位素内标 QUECHERS β2-兴奋剂 气相色谱-质谱 动物尿液 

分 类 号：O657.63[理学—分析化学] TQ460.72[理学—化学]