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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: To establish a gas chromatography-mass spectrometry method for the determination of environmental estrogens (4-nonylphenol, bisphenol A, diethylstilbestrol, 17α-ethynyl estradiol) and 17α-estradiol , 17β-estradiol, estriol, estrone) method. Methods: After the sample was extracted with acetonitrile and the protein was precipitated, the supernatant was concentrated and derivatized with pentafluoropropionic anhydride (PFPA) and detected by GC / MS. Results: 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 spiked recoveries of the tested components in milk ranged from 74.7% to 111.8%. Conclusion: The method is accurate, sensitive and accurate. It is suitable for the determination of environmental estrogen and endogenous estrogen in milk.