建立了婴幼儿配方奶粉中6种雌激素残留(己烯雌酚diethylstilbesterol,17α-乙炔基雌二醇17α-ethynylestradiol,17α-雌二醇17α-estradiol,17β-雌二醇17β-estradiol,雌三醇estriol,雌酮estrone)的气相色谱-质谱(GC-MS)的检测方法.样品经酶解后,用乙腈超声提取.提取液蒸发至近干,五氟丙酸酐(PFPA)衍生化后,经HP-5MS弱极性色谱柱分离,在SIM模式下进行定性分析和定量检测.结果表明:在0.1～50 ng/mL内,6种药物的校准曲线呈现良好的线性,相关系数(r)大于0.999.17α-乙炔基雌二醇的定量限为0.8 μg/kg,其余5种的定量限为0.1 μg/kg.6种药物在3.0,5.0,10.0μg/kg质量浓度添加水平 下,其平均回收率为60.6％～120.6％；相对标准偏差(RSD)为7.8％～19.6％.该方法已成功应用于婴幼儿配方奶粉中6种雌激素残留的定性定量检测.
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