UPLC-MS/MS法测定鸡蛋中 13种性激素残留量

Determination of 13 sex hormone residues in eggs by UPLC-MS/MS

采用超高效液相色谱-串联质谱法(UPLC-MS/MS)优化提取净化条件,利用外标法进行定量,建立鸡蛋中13种性激素残留量的定量分析方法。样品经乙腈提取后,用Waters Oasis PRiME HLB柱净化,UPLC-MS/MS法检测,经正负离子模式采集,多反应监测方式(Multiple reaction monitoring,MRM)检测,基质匹配外标法分析鸡蛋中雌二醇、雌三醇、雌酮等13种性激素的残留量。结果显示,13种性激素在鸡蛋基质中的线性良好,定量限在1.50~41.00μg/kg范围内,回收率RSD为0.21%~14.08%,在鸡蛋中50.00、100.00、200.00μg/kg添加水平上的回收率平均值为62.60%~117.20%。该方法分析速度快、特异性强、准确度高及操作简便,适合用于检测分析鸡蛋中性激素的残留筛查。

The ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was used to optimize the extrac⁃tion and purification conditions,and the external standard method was used to quantify the 13 kinds of sex hormone residues in eggs.The samples were extracted with acetonitrile,purified by Waters Oasis PRiME HLB column,and detected by UPLC-MS/MS.The sam⁃ples were collected in positive and negative ion mode,and detected by multiple reaction monitoring(MRM).The residues of 13 kinds of sex hormones such as estradiol,estriol,and esterone in eggs were analyzed by matrix matching external standard method.The re⁃sults showed that the linearity of 13 sex hormones in egg matrix was good.The limit of quantification was 1.50~41.00μg/kg,and the RSD of recovery(RSD)was 0.21%~14.08%.The average recovery at the spiked levels of 50.00,100.00 and 200.00μg/kg in eggs was 62.60%~117.20%.The method used in this study is fast,specific,accurate and easy to operate,which is suitable for the detection and analysis of residual sex hormones in eggs.