气相色谱-质谱法测定鸡肉组织中残留的氯羟吡啶  

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

作　　者：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] 

机构地区：[1]华南农业大学兽医学院兽医药理研究室,广东广州510642 [2]华南农业大学农学院化学生态研究室,广东广州510642

出　　处：《色谱》2009年第1期86-90,共5页Chinese Journal of Chromatography

基　　金：农业行业标准制定专项(No.070106-69);"十一五"国家科技支撑计划重点项目(No.2006BAD31B06)

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5．0～500μg／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0．5μ/kg；在5，10和20μg／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。A confirmative method to determine clopidol residues in chicken muscle by gas chro- matography-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 253. 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 0.5μg/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 5.9%. The established method is simple, sensitive and reproducible for the identification and quantification of clopidol residues in chicken muscle tissue.

关 键 词：气相色谱-质谱法 氯羟吡啶 残留 鸡肉 

分 类 号：O658[理学—分析化学]