固相萃取净化高效液相色谱串联质谱法测定林蛙油中4种环境雌激素的含量

Simultaneous Determination of 4 Kinds of Environmental Estrogens Residues in Rana Oviduct by Solid-Phase Extraction High Performance Liquid Chromatography-Tandem Mass Spectrometry

为建立一种简单、快速测定林蛙油中4种环境雌激素的固相萃取净化-液相色谱串联质谱的分析方法,样品经乙腈提取,Carb/NH2固相萃取柱净化后,采用HPLC-MS/MS,选择反应监测(SRM)负离子模式测定进行定性、定量分析.结果表明:在0.5~100μg/L范围内,峰面积与浓度线性良好,相关系数均大于0.997;方法的检出限(LOD)为0.36~0.42 ng/g,定量限(LOQ)为1.16~1.23 ng/g,检测结果的相对标准偏差为2.41%~13.4%(n=5),平均加标回收率达到87.3%~96.3%.该方法具有较高的重现性和选择性,适用于林蛙油中痕量环境雌激素的残留分析检测.

In this work,a simple and quick analysis method was established for the determination of four environmental estrogens in Rana oviduct by liquid chromatography-tandem mass spectrometry. The sample was extracted with acetonitrile and cleaned by Carb/NH2 solid phase extraction column. The mass spectrometer was operated in the negative ion mode using selected reaction monitoring for the qualitative and quantitative analyses. The external standard calibration curves were used for the quantification. The linear range was from 0. 5 to 100 μg/L with a good linear relationship（ R20.997）. The detection limit of this method was 0.36 ~ 0.42 ng/g,and the limit of quantification was 1.16 ~ 1.23 ng/g. The relative standard deviation ranged from 2.41% ~ 13.4%（ n = 5） and the average recovery rate was from 87.3% ~ 96.3%. This method should be suitable for the identification and quantification of environmental estrogens in Rana oviduct due to its high predictability and selectivity.