食品科学 ›› 2009, Vol. 30 ›› Issue (18 ): 282-284.doi: 10.7506/spkx1002-6630-200918063

• 分析检测 • 上一篇    下一篇

GC-MS 法测定速冻调制食品中6 种β - 兴奋剂残留

冉晓占1,吕 品2,范 斌3,张会军3,张 岩3,4,*,刘敬泽4   

  1. 1. 河北师范大学体育学院 2 河北医科大学基础医学院 3. 河北省食品安全重点实验室 4. 河北师范大学生命科学学院
  • 收稿日期:2009-06-30 出版日期:2009-09-15 发布日期:2010-12-29
  • 通讯作者: 张 岩3,4,*, E-mail:snowwinglv@126.com
  • 基金资助:

    河北省科技支撑计划项目(07276709D;09276906D)

GC-MS Determination of Six Beta-agonists in Prepared Frozen Foods

RAN Xiao-zhan1,LU Pin2,FAN Bin3,ZHANG Hui-jun3,ZHANG Yan3,4,*,LIU Jing-ze4   

  1. (1. College of Physical Education and Sport Science, Hebei Normal University, Shijiazhuang 050016, China;
    2. School of Basic Medical Sciences, Hebei Medical University, Shijiazhuang 050017, China;3. Hebei Key Laboratory of Food
    Safety, Shijiazhuang 050051, China;4. College of Life Science, Hebei Normal University, Shijiazhuang 050016, China)
  • Received:2009-06-30 Online:2009-09-15 Published:2010-12-29
  • Contact: ZHANG Yan3,4,*, E-mail:snowwinglv@126.com

摘要:

建立了气相色谱- 质谱法同时测定速冻调制食品中6 种β- 兴奋剂残留的检测方法。样品经β- 盐酸葡萄糖醛苷酶水解,用高氯酸沉淀蛋白质,经乙酸乙酯提取,再经MCX 固相萃取柱净化后,用N,O- 双(三甲基硅基)- 三氟乙酰胺(BSTFA)衍生化,以美托洛尔为内标,气相色谱质谱离子选择模式检测。对样品进行添加回收实验,平均回收率为80.1%~94.5%,相对标准偏差为4.3%~11.2%,检出限(LOD)为5μg/kg。

关键词: 气相色谱- 质谱, 速冻调制食品, β- 兴奋剂

Abstract:

A GC-MS method was developed for the determination of residues of 6 β -agonists such as clorprenaline, tulobuterol, penbutolol, propranolol, fenoterol, and ractopamine in prepared frozen foods. Minced beef cutlet samples were hydrolyzed by β-glucuronidase in sodium acetate buffer, and the centrifugation supernatant was then subjected to protein precipitation using perchloric acid, extraction using ethyl acetate, and clean up using an MCX column, followed by derivatization with bis (trimethylsilyl)trifluoroacetamide (BSTFA). The analysis was conducted with metoprolol as an internal standard in selected ion monitoring mode. The spiked recoveries of the 6β-agonists ranged 80.1%-94.5%, with a RSD from 4.3% to 11.2%, and their LODs all were 5 μg/kg.

Key words: GC-MS, prepared frozen food, β-agonists

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