您现在的位置:标准库>> 检验方法>> 肉制品>>正文内容

同时检测动物肌肉中26种β2兴奋剂和激素残留

点击数: 【字体: 打印文章 双击鼠标滚动屏幕
 


 
【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0.5~1.0 μg/kg,回收率在68. 2%~103.2%之间,相对标准偏差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

MultiResidue Analysis of 26 Types of β2Agonists adn Steroids in Animal Tissues

WU PingGu, WANG Qiang, CHEN HuiHua, YING YongFei, ZHAO YongXin,SHEN XiangHong, SONG GuoLiang, XU XiaoMin

1(Zhejiang Provincial Center For Disease Control adn Prevention, Hangzhou 310009)

2【Zhejiang Provincial Agricultural Scientific Academy, Hangzhou 310020】

3【Zhejiang Provincial Inspection Center for Animal Products Quality, Hangzhou 310020】

Abstract   A sample pretreatment method has been developed for the multiresidue analysis of 26 types anabolic agents including 10 types agonists adn 16 types steroids in animal tissues by gas omatographymass spectrometry, based on isotopelabeled internal stadnards adn solid phase extraction. The homogenized animal muscle was hydrolyzed by βglucuronidase /arylsulfatase, then passed through SLW solid phase extraction column. The steroid fraction was obtained by eluting the column with methanol adn the agonist fraction was eluted with 5% ammonia in ethyl acetate. The agonist fraction was derivatized with bis【trimethylsily1】trifluoroacetamdie+1%【m/V】 trimethylchlorosilane. The steroid fraction was further cleanuped on a SLH cartridge adn the purified residue was derivatized with heptafluorobutyrate. Both fractions were analyzed by gas omatographymass spectrometry. The experimental results indicated that the 10 types β2agonists adn 16 types steroids could be separated using SLW solid phase extraction column. The detection limits were 0.5-1.0 μg/kg, the rates of recovery were 68.2%-103.2%, adn the relative stadnard deviations were 1.5%-12.4%.

Keywords   Anabolic agents, β2agonists, steroids, multiresidue, gas omatographymass spectrometry

本文系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)和浙江省重大科技攻关基金(No.2005C12007)资助项目 Email:pgwu@cdc.zj.cn

1 引 言

畜产品生产过程滥用促蛋白合成剂(主要有激素、β2兴奋剂)对食品安全、生态环境造成直接及潜在的危害。20世纪80年代以来许多国家或组织通过立法来限制或禁止在食用动物养殖中使用促蛋白合成剂。我国也禁止将促蛋白合成剂用于动物促生长目的。由于利益驱动,在世界范围内激素和β2兴奋剂仍被大量滥用。
    
国内外对动物肌肉中激素、β2兴奋剂多残留确认检测技术文献报道很多,主要有气相色谱质谱法【GC/MS】[1~8]、液相色谱质谱法【LC/MS】[9~12],但所采用的方法很少涉及上述两大类药物多残留的同时检测。动物性食品中兽药残留由于残留物水平很低,样品基质复杂,干扰物质多,要尽可能除去与目标物同时存在的杂质,减少色谱干扰峰,避免检测器和色谱柱污染,因此样品预处理约占工作量的70%,样品的分离纯化是兽药残留分析中费时和费力的步骤,多类兽药残留集成化检测技术和兽药提取净化技术是今后研究的热点,固相萃取技术、同位素稀释技术近年来在复杂样品药物残留检测中得到广泛应用[1~12]。
    
本研究考虑到动物肌肉中激素、β2兴奋剂检测均需要先用β葡萄糖醛苷酶/芳基硫酸酯酶酶解,因此考虑两大类药物残留的同时检测。本研究采用SLW混合型固相萃取柱作为动物肌肉中促蛋白合成剂多残留测定前处理技术,先将上述两类药物在SLW柱上富集后分别洗脱,然后用GC/MS分别测定26种促蛋白合成剂【10种β2兴奋剂、16种激素】残留,结合同位素内标进行定量分析。