气相色谱-质谱法同时测定饲料中6种雌激素类药物  

Simultaneous Determination of Six Estrogens in Feed by Gas Chromatography- Mass Spectrometry

作　　者：林小莉 李宁 霍峰 董艳峰 彭玮 

机构地区：[1]哈尔滨市兽药饲料监察所,黑龙江哈尔滨150010

出　　处：《分析测试学报》2016年第3期322-326,共5页Journal of Instrumental Analysis

基　　金：哈尔滨市科技攻关计划(2014AB3BN041)

摘　　要：建立了固相萃取/气相色谱-质谱法（GC-MS）同时测定饲料中己烷雌酚、己烯雌酚、双烯雌酚、雌酮、17β-雌二醇、雌三醇的检测方法。饲料样品经乙醚提取后,HLB固相萃取柱净化、衍生化后用气相色谱-质谱仪进行检测,外标法定量。结果表明,己烷雌酚在2.5-250 ng/mL,其它5种雌激素类药物在5-500ng/mL范围内具有良好的线性关系,相关系数不小于0.99,检出限为3-8μg/kg,样品的平均加标回收率为75.9%-96.3%。该方法检出限低,能够准确进行定性和定量测定,可同时测定饲料中的6种雌激素类药物。A method was developed for the simultaneous determination of hexoestrolum,diethylstilbestrol,dienestrol,estrone,17β-estradiol and estriol in feed by solid phase extraction and gas chromatography- mass spectrometry（ GC- MS）. After extracted with ethyl ether and cleaned-up on an HLB phase extraction column,six kinds of estrogens were derived and quantified by GC- MS. The external standard calibration curves were used for the quantification. The results showed that the high linear ranges from 2. 5 ng / mL to 250 ng / mL for hexoestrolum and from 5 ng / mL to 500 ng / mL for five other estrogens were obtained with correlation coefficients（ r^2） not less than 0. 99. The limits of detection were in the range of 3- 8 μg / kg and the average recoveries were 75. 9%- 96. 3%. The results demonstrated that the developed method could be applied in the qualitative and quantitative determination of six kinds of estrogens in feed with low limit of detection and high accuracy.

关 键 词：气相色谱-质谱 己烷雌酚 己烯雌酚 双烯雌酚 雌酮 雌二醇 雌三醇 饲料 

分 类 号：O657.63[理学—分析化学] O629.8[理学—化学]