全自动固相萃取-高效液相色谱-串联质谱法测定食糖中的雌二醇

摘要

A high performance liquid chromatography-tandem mass spectrometry ( HPLC-MS/MS)method was established for the determination of estradiol in table sugar. Sugar sam-ples were dissolved in water,and extracted by alkaline acetonitrile,then cleaned-up using an HLB column. The resulting samples were detected under negative multiple reactions monitoring (MRM)mode,and quantified by the internal standard method. As the results showed,the matrix effects were depressed obviously after the purification. The limit of determination and the limit of quantification of the method were 0. 1 μg/kg and 0. 5 μg/kg,respectively. For all the tested samples,the average spiked recoveries ranged from 83. 9% to 95. 1%,and the rela-tive standard deviations( RSDs,n=6)were lower than 10%. The method is quick,easy,effec-tive,sensitive and accurate,and can meet the requirements of the determination of estradiol in table sugar.%建立了全自动固相萃取-高效液相色谱-串联质谱检测食糖中雌二醇含量的方法。食糖样品经水溶解后，用碱化乙腈提取，经 HLB固相萃取柱净化，采用高效液相色谱-串联质谱分析，内标法定量。质谱分析采用电喷雾电离（ ESI）负离子扫描，多反应监测（ MRM）模式。雌二醇定量离子对为271.1／144.8和271.1／183.2，内标 D2-雌二醇定量离子对为273.2／147.0。实验表明，经 SPE 柱净化后基质效应明显降低，样品中添加0.5~10μg／kg 的雌二醇，其回收率为83.9％~95.1％，相对标准偏差（ n＝6）小于10％。雌二醇的检出限为0.1μg／kg，定量限为0.5μg／kg。该方法提取效果好，具有良好的灵敏度、回收率和重复性。