摘要
建立了气相色谱-质谱（GC-MS）测定鸡蛋、牛奶中氯羟吡啶残留的检测方法.采用甲醇提取鸡蛋、牛奶中待测物,经碱性氧化铝层析柱净化,Sylon BFT衍生剂80℃衍生60 m in,对氯羟吡啶三甲基硅烷化衍生物采用选择离子监测模式（SIM）进行检测.氯羟吡啶衍生物的响应信号与其质量浓度在5.00~500.00μg/L范围内呈良好的线性关系,相关系数大于0.99;在5、10和20μg/kg添加水平下,鸡蛋中待测物的平均回收率分别为68.4%、75.2%和80.1%,牛奶中待测物的平均回收率分别为79.5%、87.1%和90.0%,批内、批间相对标准偏差均小于10%;以3倍信噪比（S/N）计算方法的检出限达2.0μg/kg;以10倍信噪比（S/N）计算方法的定量限为5.0μg/kg.
A confirmative method to determine clopidol residues in egg and milk by gas chromatography-mass spectrometry（GC-MS） was established.The analyte was extracted with methanol,and then purified with a Bond Elut Alumina-B.The drug was derived at 80 ℃ for 60 min with Sylon BFT,and more toluene was added and then applied to GC-MS.The selected ion monitoring（SIM） mode was performed at m/z 212,214,248 and 263.The linearity was good in the range of 5.00 and 500.00 μg/L with the correlation coefficients better than 0.99.The average recoveries fortified at 5,10 and 20 μg/kg were 68.4%,75.2% and 80.1% in egg and 79.5%,87.1% and 90.0% in milk,respectively.The relative standard deviations（RSD） of intra-day and inter-day were less than 10%.The limit of detection（S/N=3） was 2.0 μg/kg and the limit of quantification（S/N=10） was 5.0 μg/kg for clopidol in egg and milk.
出处
《华南农业大学学报》
CAS
CSCD
北大核心
2010年第4期108-111,共4页
Journal of South China Agricultural University
基金
农业部2007年农业行业标准项目(070106)
关键词
气相色谱-质谱法
氯羟吡啶
残留
鸡蛋
牛奶
gas chromatography-mass spectrometry（GC-MS）
clopidol
residue
egg
milk
