液相色谱-串联质谱法检测牛奶中的雌二醇

Determination of estradiol in milk products by LC-MS /MS

目的建立液相-串联质谱法(LC-MS/MS)测定牛奶中雌二醇残留的分析方法。方法样品经甲醇提取,离心,过CARB/NH2复合柱净化,氮吹至干,用1 ml乙腈-水(4∶6,V∶V)定容后经超高效液相色谱分离,电喷雾串联四级杆质谱进行检测,内标法定量。结果本法雌二醇在3.0μg/L^60μg/L的范围内线性关系良好,r=0.9992,平均回收率为91.2%~109.5%,相对标准偏差为3.45%~6.21%。方法定量限1.0μg/kg。结论该方法快速、灵敏,适用于批量实际样品检测。

Objective To establish a liquid chromatography-mass spectrometry（LC-MS /MS） method for determination of estradiol in milk.Methods Estradiol in milk was extracted with methanol,then the extract was centrifuged and purified on a CARB /NH2 column.The eluant was evaporated under nitrogen.The residue was dissolved in acetonitrile-water（4∶6,V /V）,then determined by LC-MS /MS and quantified by internal standard method.Results The linear range of the method was3.0 μg /L - 60 μg /L,with r = 0.9992.The average recoveries of the method were 91.2% - 109.5%,the relative standard deviations were 3.45% - 6.21%,the limit of quantification was 1.0 μg /kg.Conclusion The method is rapid,sensitive and suitable for analysis of estradiol in practical samples in batches.