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气相色谱-质谱法同时测定动物尿样中莱克多巴胺和克伦特罗

应永飞, 皮雄娥, 吴平谷, 陈慧华, 朱聪英, 陆春波

应永飞, 皮雄娥, 吴平谷, 陈慧华, 朱聪英, 陆春波. 气相色谱-质谱法同时测定动物尿样中莱克多巴胺和克伦特罗[J]. 质谱学报, 2006, 27(2): 74-78.
引用本文: 应永飞, 皮雄娥, 吴平谷, 陈慧华, 朱聪英, 陆春波. 气相色谱-质谱法同时测定动物尿样中莱克多巴胺和克伦特罗[J]. 质谱学报, 2006, 27(2): 74-78.
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YING Yong-fei, PI Xiong-e, WU Ping-gu, CHEN Hui-hua, ZHU Cong-ying, LU Chun-bo. Simultaneous Determination of Ractopamine and Clenbuterol Residues in Animal Urine with Gas Chromatography-Mass Spectrometry[J]. Journal of Chinese Mass Spectrometry Society, 2006, 27(2): 74-78.
Citation: YING Yong-fei, PI Xiong-e, WU Ping-gu, CHEN Hui-hua, ZHU Cong-ying, LU Chun-bo. Simultaneous Determination of Ractopamine and Clenbuterol Residues in Animal Urine with Gas Chromatography-Mass Spectrometry[J]. Journal of Chinese Mass Spectrometry Society, 2006, 27(2): 74-78.
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气相色谱-质谱法同时测定动物尿样中莱克多巴胺和克伦特罗

  • 1.

    浙江省畜产品质量安全检测中心,浙江 杭州 310020

  • 2.

    浙江省农业科学院植物保护与微生物所,浙江 杭州 310021

  • 3.

    浙江省疾病预防控制中心,浙江 杭州 310020

详细信息
    通讯作者:

    应永飞

  • 中图分类号: O657.63；R974.3

Simultaneous Determination of Ractopamine and Clenbuterol Residues in Animal Urine with Gas Chromatography-Mass Spectrometry

  • 1.

    Animal Products Quality Testing Center of Zhejiang Province, Hangzhou 310020, China

  • 2.

    Institute of Plant Protection and Microbiology, Zhejiang Academic of Agriculture Science, Hangzhou 310021, China

  • 3.

    Disease Prevent and Control Center of Zhejiang Province, Hangzhou 310020, China

More Information
    Corresponding author:

    YING Yong-fei

摘要

    摘要
  • 摘要: 建立了固相萃取-气相色谱-质谱法（SPE-GC/MS）同时测定动物尿样中的莱克多巴胺和克伦特罗的方法。试样中的药物经乙酸乙酯提取后，经SLH固相萃取柱净化，氮吹至干，衍生化后进行气相色谱-质谱测定。两种药物的检出限均为0.3 μg/L，定量限均为1.0 μg/L,线性范围为0.02～1.0 μg／mL。加标浓度在4.0～20.0 μg/L范围内，莱克多巴胺加标回收率为78.6％～101.2％，批内相对标准偏差≤7.0％；克伦特罗加标回收率为92.3％～112.2％，批内相对标准偏差≤6.9％。
    Abstract: A new solid phase extractiongas chromatographymass spectrometry （SPE-GC/MS） method for simultaneous determination of ractopamine and clenbuterol in animal urine was reported. The drugs were extracted with ethyl acetate from sample. The extraction was evaporated at 40 ℃. After the residue was dissolved in ethyl acetate, it was purified by passing through SLH solid-phase extraction （SPE） cartridges. The eluate was evaporated by nitrogen blow and derivatizated with BSTFA, and then assayed by GC/MS. The limits of detection (LOD) were 0.3 μg/L, and the limits of quantitation (LOQ) were 1.0 μg/L. The calibration curves were linear between 0.02 μg/mL and 1.0 μg／mL for ractopamine and clenbuterol. Recoveries of ractopamine and clenbuterol were 78.6％-101.2％and 92.3％-112.2％, and the intrarelative standard deviation (n=5) less than 7.0% and 6.9%, respectively, at spiked levels of 4.0～20 μg/L.
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    • 参考文献(13)
  • [1] EC Council directive 96/22/EC of 29 April 1996 (replacement of 88/146/EC). Concerning the Prohibition on the Use in Stock Farming of Substances Having β-Agonist Action, and Repealing Directives 81/602/EEC, 88/146/EEC and 88/299/EC[M]. Off J Eur Commun, 1996，L125：3.
    [2] 农业部,卫生部,国家药品监督管理局. 农业部176号公告[M] . 禁止在饲料和动物饮用水中使用的药物品种目录.
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    [6] 谢孟峡，刘 媛，蒋 敏. 固相萃取-气相色谱-质谱分析肉样中盐酸克伦特罗的残留量[J] . 分析化学, 2002, 30(11) ： 1 308-1 311.
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    [9] 贺利民，苏贻娟，张嘉慧. 气相色谱质谱法测定动物组织及饲料中克伦特罗[J] . 质谱学报，2005，26（3）：168-171.
    [10] Antignac J P, Marchand P, Bizec B L, et al. Identification of Ractopamine Residues in Tissue and Urine Samples at Ultra-trace Level Using Liquid Hromatography-Positive Electrospraytandem Mass Spectrometry[J]. J Chromatogr B，2002，774：59-66.
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    [12] Doerge D R, Churchwell M I, Holder C L, et al. Detection and Confirmation of β-Agonists in Bovine Retina Using LC/APCIMS[J]. Anal Chem，1996，68(11)：1 918-1 923.
    [13] 吴永宁，苗 虹，赵云峰,等. GB/T5009.192-2003. 动物性食品中克伦特罗残留量的测定[S]. 北京:中国标准出版社，2003.
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出版历程
  • 收稿日期:  2005-06-14
  • 修回日期:  2005-11-28
  • 刊出日期:  2006-05-14

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