GC-MS法测定奶与奶制品中雌二酮残留量的研究  

Determination of estrone in milk and milk product with Gas Chromatography-Mass Spectrometry

作　　者：刘勇军[1] 刘创基[1] 姜艳彬[1] 吴银良 雷春娟[1] 

机构地区：[1]中国动物疫病预防控制中心,北京100125 [2]宁波市农业科学院,浙江宁波315000

出　　处：《中国乳品工业》2011年第1期45-47,52,共4页China Dairy Industry

摘　　要：通过液液萃取和固相萃取提取、净化奶与奶制品中添加的雌酮,以TMS衍生化试剂BSTFA衍生化,气相色谱-质谱联用(选择离子模式,选择离子为m/z218、m/z244、m/z257、m/z342)对衍生物检测分析,确定了样品中雌酮的定性、定量分析方法,该法检出限为0.2μg/kg,定量限为0.8μg/kg。衍生物的峰面积与样品质量浓度在0.5～1000μg/L范围内呈良好的线性关系,线性回归系数为0.999。雌酮不同加入量的添加回收率为70.1%～93.6%,变异系数为2.0%～3.7%。该方法可实现对样品进行灵敏、准确的定性定量分析。The residual veterinary drug of estrone in milk and milk product was extracted and purified by the method of liquid-liquid partition and solid phase extraction.The estrone was separated and validated by gas chromatography spectrometry（selected ion mode,the selected ions m/z 218,m/z 244,m/z 257 and m/z 342） after derivatization of the purified sample with the TMS derivative reagent of BSTFA,and the qualitative and quantitative analysis method was developed.Its LOD and LOQ is 0.2 μg/L and 0.8 μg/kg,respectively.and there was a good linear correlation between the ratio of peak areas and the concentration of estrone in the add range of 0.5～1000 μg/L,the correlative coefficient is 0.999,the recoveries of different concentration of estrone was 70.1%～93.6%.The RSD of the method was between 2.0% and 3.7%.The method is suitable for the qualitative and quantitative analysis of estrone in the milk and milk product.

关 键 词：固相萃取 气质联用 雌酮 选择离子监测 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程]