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[目的]建立奶粉中的环境雌激素(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)的气相色谱-质谱(GC-MS)测定方法。[方法]样品经乙腈沉淀蛋白质后取上清液氮气流浓缩至干,经五氟丙酸酐(PFPA)衍生化后用GC-MS进行检测。[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。回收率为72.2%～102.5%。[结论]该方法准确、灵敏,精密度好,适于奶粉中环境雌激素的测定。
[Objective] To establish the environmental estrogen (4-nonylphenol, bisphenol A, diethylstilbestrol, 17α-ethinyl estradiol) and endogenous estrogen (17α-estradiol, 17β- Diol, estriol, estrone) by gas chromatography-mass spectrometry (GC-MS) determination method. [Method] After the sample was precipitated by acetonitrile, the supernatant was extracted by nitrogen and concentrated to dryness. The sample was derivatized with pentafluoropropionic anhydride (PFPA) and detected by GC-MS. [Result] The relative standard deviation (RSD) of peak area measured by this method was 1.25% ~ 5.85% with the detection limit of 0.024 ~ 1.40μg / kg. The recovery rate was 72.2% ~ 102.5%. [Conclusion] The method is accurate, sensitive and precise, suitable for the determination of environmental estrogen in milk powder.