【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%。 (w#)|9Cxm
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MultiResidue Analysis of 26 Types of β2Agonists adn Steroids in Animal Tissues b@Dt]6_UL
WU PingGu, WANG Qiang, CHEN HuiHua, YING YongFei, ZHAO YongXin,SHEN XiangHong, SONG GuoLiang, XU XiaoMin tqCwbi
1(Zhejiang Provincial Center For Disease Control adn Prevention, Hangzhou 310009) $=ESY>MO
2【Zhejiang Provincial Agricultural Scientific Academy, Hangzhou 310020】 *2}f $8
3【Zhejiang Provincial Inspection Center for Animal Products QualITy, Hangzhou 310020】 }I MV@z B
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%. +sTPTCLE
Keywords Anabolic agents, β2agonists, steroids, multiresidue, gas omatographymass spectrometry WMW=RgiW\
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 uL@%M8n
1 引 言 C@[U:\
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。 &c