色谱

色谱

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气相色谱-质谱法测定鸡肉组织中残留的氯羟吡啶

刘祥国1,苏贻娟2,方炳虎1,丁焕中1,贺利民1*,曾振灵1,陈杖榴1   

  1. 1.Department of Pharmacology and Toxicology, College of Veterinary Medicine, South China Agricultural University, Guangzhou 510642, China; 2.Department of Ecology, College of Agriculture, South China Agricultural University, Guangzhou 510642, China
  • 收稿日期:2008-07-06 修回日期:2008-09-15 出版日期:2009-01-30 发布日期:1983-03-25
  • 通讯作者: 贺利民
  • 基金资助:
    农业行业标准制定专项(No. 070106-69)和“十一五”国家科技支撑计划重点项目(No. 2006BAD31B06).

Determination of clopidol residues in chicken muscle by gas chromatography-mass spectrometry

LIU Xiangguo1, SU Yijuan2, FANG Binghu1, DING Huanzhong1, HE Limin1*, ZENG Zhenling1, CHEN Zhangliu1   

  1. 1.Department of Pharmacology and Toxicology, College of Veterinary Medicine, South China Agricultural University, Guangzhou 510642, China; 2.Department of Ecology, College of Agriculture, South China Agricultural University, Guangzhou 510642, China
  • Received:2008-07-06 Revised:2008-09-15 Online:2009-01-30 Published:1983-03-25
  • Contact: HE Limin

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590

被引次数

29

摘要： 建立了气相色谱-质谱(GC-MS)测定鸡肉组织中氯羟吡啶残留的确证方法。采用乙腈提取鸡肉组织中的待测物,经碱性氧化铝层析柱净化,Sylon BFT衍生剂衍生后,采用选择离子监测(SIM)模式检测。对氯羟吡啶三甲基硅烷化衍生物的电子轰击（EI）质谱碎片进行解析,选择m/z 212,214,248和263等4个特征离子作为定性离子,其中m/z 248为定量离子。同时还考察了检测过程中的基质效应。氯羟吡啶衍生物的响应与其质量浓度在5.0～500 μg/L范围内呈良好的线性关系,相关系数大于0.998;以3倍信噪比(S/N)计算方法的检出限达0.5 μg/kg;在5，10和20 μg/kg添加水平下鸡肉组织中待测物的平均回收率分别为77.0%,84.5%及89.4%,相对标准偏差小于6.9%。结果表明,该方法简单、灵敏、可靠,适用于鸡肉组织中氯羟吡啶残留的分析确证。

关键词: 残留, 鸡肉 , 氯羟吡啶, 气相色谱-质谱法

Abstract: A confirmative method to determine clopidol residues in chicken muscle by gas chromatography-mass spectrometry (GC-MS) was developed. The analyte was extracted with acetonitrile, and then purified with an Alumina-B cartridge column. The drug was derived at 80 ℃ for 60 min with Sylon BFT, and more toluene was added and then applied to GC-MS. The mass spectral characteristics of trimethylsilyl derivative of clopidol were interpreted, and selected ion monitoring (SIM) mode was performed at m/z 212, 214, 248 and 263. The clopidol was qualitatively identified by the ratio of relative abundance of the selected ions and determined quantitatively by SIM mode at m/z 248. In the meantime, the matrix effect was evaluated. The range of linearity was 5.0-500 μg/L with the correlation coefficients better than 0.998, and the detection limit was 0.5 μg/kg (S/N=3) for clopidol. The average recoveries from chicken muscle fortified at 5, 10 and 20 μg/kg were 77.0%, 84.5% and 89.4%, respectively, and the relative standard deviations (RSD) were less than 6.9%. The established method is simple, sensitive and reproducible for the identification and quantification of clopidol residues in chicken muscle tissue.

Key words: chicken muscle , clopidol, residue, gas chromatography-mass spectrometry (GC-MS)