气相色谱-质谱法测定牛奶中的8种环境雌激素和内源性雌激素  

Determination of environmental estrogens in milk by gas chromatography-mass spectrometry

作　　者：张红英[1] 张宏[1] 王淑惠[1] 杨立学[1] 陈杏琴[1] 

机构地区：[1]石家庄市疾病预防控制中心,石家庄050011

出　　处：《中国卫生检验杂志》2009年第8期1713-1715,共3页Chinese Journal of Health Laboratory Technology

基　　金：石家庄市科技局指令性课题(04146403A)

摘　　要：目的：建立气相色谱-质谱法测定牛奶中环境雌激素（4-壬基酚、双酚A、已烯雌酚、17α-乙炔基雌二醇）和内源性雌激素（17α-雌二醇、17β-雌二醇、雌三醇、雌酮）方法。方法：样品经乙腈提取和沉淀蛋白后,浓缩上清液,经五氟丙酸酐（PFPA）衍生化后用GC/MS检测。结果：该法测定的峰面积的日内相对标准偏差为1.25%-5.85%,检出限为0.024-1.40μg/kg。牛奶中被测组分的加标回收率在74.7%-111.8%之间。结论：该方法准确、灵敏,精密度好,适于牛奶中环境雌激素和内源性雌激素的测定。Objective： A gas chromatography-mass spectrometry（GC/MS） method for simultaneous determination of environmental estrogens including 4-nonylphenol,bishphenol A,diethylstilbestrol and 17-ethinylestradiol and endogenic estrogens including 17α-estradiol,17β-estradiol,estriol and estrone in milk was established.Methods：Acetonitrile was used as extracted solution and albumen precipitator.Milk and powdered milk were extracted with acetonitrile.The extract was gently evaporated just to dryness with nitrogen and then derivated with pentafluoropropionic anhydride（PFPA）,the derivatives were determined by GC-MS.Results：The intra-day relative standard deviations of the peak area were 1.25% to 5.85% and the detection limits ranged from 0.024 to 1.40 μg/kg and the recoveries from 74.7% to 111.8%.Conclusion：This method is simple,rapid,accurate and applicable to the determination of trace environmental estrogens in milk.

关 键 词：气相色谱-质谱法 环境雌激素 牛奶 

分 类 号：O657.63[理学—分析化学]