分散固相萃取结合HPLC-MS/MS检测鸡蛋中16种全氟化合物

Determination of Sixteen Perfluorinated Compounds in Egg by High Performance Liquid Chromatography- Tandem Mass Spectrometry Combined with Dispersive Solid Phase Extraction

建立了分散固相萃取净化结合 HPLC -MS/MS 测定鸡蛋中16种全氟化合物（ Perfluorinated com-pounds，PFCs）的方法。样品经乙腈40℃下超声萃取，氮吹浓缩，石墨化碳黑分散萃取净化后，采用HPLC-MS/MS进行测定，基质曲线-内标法定量。结果显示，16种PFCs在0.50-10.0μg/L浓度范围内呈良好线性，相关系数（ r）为0.9962-0.9999，检出限为0.001-0.093μg/kg，定量下限为0.003-0.310μg/kg。在0.5，1.0，2.0μg/kg 3个加标浓度水平下，16种PFCs的加标回收率为79％-125％，相对标准偏差（ RSDs， n=6）为0.26％-14％。该方法具有净化效果好、定量准确、灵敏度高的特点，适用于鸡蛋样品中16种常见全氟化合物的快速确认和准确定量。

A method was developed for the determination 16 perfluorinated compounds（ PFCs）in egg by high performance liquid chromatography-tandem mass spectrometry（ HPLC-MS/MS）combined with dispersive solid phase extraction. The samples were extracted with acetonitrile in an ultrasonic bath at 40 ℃. The extract was concentrated with N2 ,purified with graphitized carbon black（ GCB）, and analysed by HPLC-MS/MS. The calibration curves of 16 PFCs were linear in the concentration range of 0. 50 -10. 0 μg/L with correlation coefficients（r）of 0. 996 2-0. 999 9. The limits of de-tection for 16 PFCs were between 0. 001 μg/kg and 0. 093 μg/kg,and the limits of quantitation were between 0. 003 μg/kg and 0. 310 μg/kg. The mean recoveries of 16 PFCs at spiked levels of 0. 5, 1. 0,2. 0 μg/kg were in the range of 79% -125% with relative standard deviations（RSDs,n=6） of 0. 26% -14% . The method was suitable for the identification and quantification of 16 perfluorinat-ed compounds in egg due to its advantages of simplicity,accuracy and high sensitivity.