同时检测动物肌肉中26种β2-兴奋剂和激素残留  

Multi-Residue Analysis of 26 Types of β_2-Agonists and Steroids in Animal Tissues

作　　者：吴平谷[1] 王强[2] 陈慧华[3] 应永飞[3] 赵永信[1] 沈向红[1] 宋国良[1] 徐小民[1] 

机构地区：[1]浙江省疾病预防控制中心,杭州310009 [2]浙江省农业科学院,杭州310020 [3]浙江省畜产品质量安全检测中心,杭州310020

出　　处：《分析化学》2008年第11期1476-1482,共7页Chinese Journal of Analytical Chemistry

基　　金：浙江省卫生厅优秀青年人才基金(No.2006QN007);浙江省重点科研农业基金(No.2005C22029);浙江省重大科技攻关基金(No.2005C12007)资助项目

摘　　要：建立了动物肌肉中10种β2-兴奋剂、16种激素共26种促蛋白合成剂的固相萃取样品前处理方法,用同位素内标结合气相色谱-质谱联用法进行分析。动物肌肉经过β-葡萄糖醛苷酶/芳基硫酸酯酶酶解,酶解液通过SLW固相萃取柱浓缩净化,先用甲醇洗脱16种激素,然后用5%氨化乙酸乙酯洗脱10种β2-兴奋剂,后者经过双三甲基硅基三氟乙酰胺＋1%（φ）三甲基氯硅烷衍生后,用GC/MS测定β2-兴奋剂;前者再用SLH固相萃取柱净化,七氟丁酸酐衍生后用GC/MS测定激素。结果表明,SLW固相萃取柱能够很好地分离动物肌肉酶解液中10种β2-兴奋剂、16种激素,结合GC/MS测定,本方法检出浓度为0.5-1.0μg/kg,回收率在68.2%-103.2%之间,相对标准偏差1.5%-12.4%。A sample pretreatment method has been developed for the multi-residue analysis of 26 types anabolic agents including 10 types agonists and 16 types steroids in animal tissues by gas chromatography-mass spectrometry, based on isotope-labeled internal standards and solid phase extraction. The homogenized animal muscle was hydrolyzed by β-glucuronidase/arylsulfatase, then passed through SLW solid phase extraction column. The steroid fraction was obtained by eluting the column with methanol and the agonist fraction was eluted with 5% ammonia in ethyl acetate. The agonist fraction was derivatized with bis（trimethylsilyl ）trifluoroaeetamide ＋ 1% （m/V） trimethylchlorosilane. The steroid fraction was further cleanuped on a SLH cartridge and the purified residue was derivatized with heptafluorobutyrate. Both fractions were analyzed by gas chromatography-mass spectrometry. The experimental results indicated that the 10 types β2-agonists and 16 types steroids could be separated using SLW solid phase extraction column. The detection limits were 0.5 - 1.0μg/kg, the rates of recovery were 68.2% - 103.2% , and the relative standard deviations were 1.5% - 12.4%.

关 键 词：促蛋白合成剂 β2-兴奋剂 激素 多种残留 气相色谱-质谱 

分 类 号：TS207.53[轻工技术与工程—食品科学]