分散固相萃取-超高效液相色谱-质谱联用法测定食品中4种全氟化合物

Determination of Perfluorinated Compounds in Food by High Performance Liquid Chromatography-tandem Mass Spectrometry Combined with Dispersive Solid Phase Extraction

建立了肉、蛋和水果类样品中4种全氟化合物的高效液相色谱-串联质谱方法。样品经酸化乙腈提取,加入PSA、C18和GCB三种吸附剂后对样品进行净化。以HPLC-MS/MS检测萃取液中PFCs的含量,采用T3柱分离,负ESI电离和MRM定性分析。采用同位素内标物质进行定量分析。4种PFCs在0.05~20 ng/mL内线性良好,相关系数R>0.995,检出限为0.00062~0.00226μg/kg,定量限为0.00167~0.00615μg/kg。PFOS和PFHSX在添加水平分别为0.02、0.2、1μg/kg, PFOA和PFNA在添加水平分别为0.002、0.02、0.1μg/kg, PFCs的平均回收率在76.5%~106.0%之间,相对标准偏差为0.87%~12.0%。该方法快速、简单、准确,适用于肉、蛋和水果类样品中4种PFCs的检测。

A method was developed for the determination of 4 perfluorinated compounds in meats, eggs and fruits by high performance liquid chromatography-tandem mass spectrometry combined with dispersive solid phase extraction. The sample was extracted with acidified acetonitrile, and then cleaned-up by mixture of PSA,C18and GCB sorbents. Four PFCs were analyzed by HPLC-MS/MS with a T3 chromatographic column, adopting the MRM mode with negative ESI. For accurate quantitative analysis, the isotope internal standard method was used. The calibration curves were linear with the correlation coefficients over 0.995 in the range of 0.05~20 ng/mL for the 4 PFCs. The limits of detection were 0.00062~0.00226 μg/kg. The limits of quantification were 0.00167~0.00615 μg/kg. The mean recoveries of the PFOS and PFHSX at spiked levels of 0.02、0.2、1 μg/kg and of the PFOA and PFNA at spiked levels of 0.002、0.02、0.1 μg/kg were in the range from 76.5% to 106.0% with the relative standard deviations of 0.87%~12.0%. The developed method was rapid, simple, accurate. It was suitable for the determination of the four PFCs in large quantities of meats, eggs and fruits samples.