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目的建立牛奶中雌三醇、17β-雌二醇、17α-炔雌醇、雌酮、己烯雌酚、己二烯雌酚、己烷雌酚7种雌激素类药物残留的高效液相色谱-串联质谱(LC-MS/MS)同时测定方法。方法均质样品用水分散后加乙腈提取雌激素,采用正己烷除脂,NH2柱净化后,经Atlantis T3色谱柱分离,在电喷雾负离子模式下以多反应监测(MRM)方式检测,采用同位素内标法定量。结果 7种雌激素在1.0~50μg/L范围内线性良好,相关系数均大于0.998,检出限和定量限分别为0.1~0.3μg/kg和0.2~0.9μg/kg。在1、10、50μg/kg三个浓度水平下的平均回收率为75.3%~120.0%,相对标准偏差(RSD)为3.4%~19.6%。结论该方法操作简便、快速、灵敏度高、定量准确,适合于牛奶中雌激素类药物残留的同时快速分析。
OBJECTIVE To establish a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) method for the determination of estrogen, 17β-estradiol, 17α-ethinylestradiol, estrone, diethylstilbestrol, diethylstilbestrol and hexestrol in milk (LC-MS / MS) simultaneous determination method. METHODS Homogenized samples were extracted with water and acetonitrile was used to extract estrogen. The samples were denaturalized with n-hexane, purified with NH2 column, separated by Atlantis T3 column and detected by MRM in electrospray negative ion mode. Standard method of quantitative. Results The linearity of the seven estrogens in the range of 1.0-50 μg / L was good with the correlation coefficients greater than 0.998. The limits of detection and quantification were 0.1-0.3 μg / kg and 0.2-0.9 μg / kg, respectively. The average recoveries at three concentration levels of 1, 10 and 50 μg / kg ranged from 75.3% to 120.0% and the relative standard deviations (RSDs) ranged from 3.4% to 19.6%. Conclusion The method is simple, rapid, sensitive and accurate. It is suitable for simultaneous rapid analysis of estrogenic drug residues in milk.