固相萃取-高效液相色谱串联质谱法测定原料奶中5种环境雌激素残留量的研究

Research of the determination of 5 kinds of environmental estrogens residues in raw milk by solid phase extraction-high performance liquid chromatography tandem mass spectrometry

摘要: 建立固相萃取-高效液相色谱串联质谱法测定原料乳中环境雌激素（雌酮、雌二醇、雌三醇、己烯雌酚、双酚A）的方法。原料乳用NH2-SPE固相萃取小柱进行富集,旋转蒸发浓缩后,采用高效液相色谱串联质谱法测定。实验结果表明:各待测物在0.01～0.5μg/mL范围内具有良好的线性关系,相关系数均大于0.9978,加标回收率为68.5%～105.6%,RSD为2.56%～7.59%,最低检出限为0.22～0.56μg/L（S/N=3）。本方法操作简便,快速灵敏,适合于牛奶中痕量环境雌激素的残留分析检测。

Abstract: A solid phase extraction-high performance liquid chromatography tandem mass spectrometry method for simultaneous determination of environmental estrogens including estrone, estradiol, estriol, diethylstilbestrol and bisphenol A in raw milk was established.5 kinds of environmental estrogens were extracted from the raw milk sample by a NH2-SPE column, and concentrated with a rotary evaporator.The extract was analyzed by high performance liquid chromatography tandem mass spectrometric.Results showed that a good linear range from 0.01⁰.5μg/mL with correlation coefficient of above 0.9978 was obtained.The extraction recovery were 68.5%¹05.6% and the relative standard deviation were 2.56%⁷.59%.The limit of detection was 0.22⁰.56μg/L (S/N=3) .The described method was simple, sensitive and accurate.