气相色谱-串联质谱测定乳粉中6种雌激素

建立了乳粉中6种雌激素残留(己烯雌酚、α-雌二醇、β-雌二醇、雌三醇、雌酮、双酚A)的气相色谱-串联质谱的检测方法.样品经酶解、提取、衍生后经气相色谱-串联质谱测定,在多反应监测模式下进行定性定量分析.结果表明,6种雌激素的校准曲线均呈现良好的线性,相关系数大于0.999.双酚A的定量限为0.03μg/kg,其余5种的定量限为0.3μg/kg,平均回收率93.93％,平均相对标准偏差6.05％,符合方法学要求,并己成功应用于市售乳粉中6种雌激素残留的检测.

Simultaneous Analysis of Six Estrogens in Milk Powder by GC-MS-MS

An efficient method was developed for the simultaneous analysis of six estrogens including diethylstilbestrol, α-estradiol, β-estradiol, estriol, estrone and bisphenol A in milk powder using gas chromatography-tandem mass spectrometry （GC-MS-MS）. Samples were enzymatically hydrolyzed and extracted with acetonitrile. The extract was then derivatized with pentafluoropropionic anhydride before being injected into the GC-MS-MS system. Qualitative and Quantitative analysis was carried out under the multiple reaction monitoring （MRM） mode. The results indicated that all six estrogens displayed a good linear relationship with R2 〉 0.999. The limits of quantification for bisphenol A and the other fiv~ estrogens were 0.03 and 0.3 μg/kg, respectively. The average recovery of six estrogens was 93.93%, with RSD of 6.05%, meeting the methodological requirements. The method developed in this study can be successfully applied in the determination of six estrogens in milk powder.