建立了羊肝样品中19种全氟烷基酸（ PFAs）的高效液相色谱-串联质谱检测方法。样品经酸化乙腈提取，加入乙二胺-N-丙基硅烷（ PSA）、C18、石墨化炭黑（ GCB）3种吸附剂后涡旋振荡对样品进行净化。以高效液相色谱-串联质谱（ HPLC-MS／MS）检测萃取液中 PFAs含量，采用 C18色谱柱分离，负离子模式电喷雾电离，配合多级反应离子扫描（ MRM）定性分析目标化合物。考察了盐酸和吸附剂的用量对加标回收率的影响，优化了主要影响因素和实验条件。在优化条件下采用同位素标记内标物进行定量分析。19种 PFAs 在0.05~20μg／kg 范围内线性关系良好，相关系数 R＞0.998，检出限（ LOD）为0.004~0.111μg／kg，定量限（ LOQ）为0.012~0.370μg／kg。在0.5、1.0、2.0μg／kg加标水平下，19种 PFAs的加标回收率为80％~128％，相对标准偏差（ RSD）范围为0.31％~11.1％。该方法快速、简单、准确，适用于羊肝样品中19种 PFAs的检测分析。
A method was developed for the determination of 19 perfluoroalkyl acids( PFAs)in lamb liver by high performance liquid chromatography-tandem mass spectrometry( HPLC-MS/MS)combined with dispersive solid phase extraction. The sample was extracted with acidified acetonitrile,and then cleaned-up by a mixture of N-propylethylenediamine( PSA ),C18 and graphitized carbon black( GCB)sorbents. The 19 PFAs were analyzed by HPLC-MS/MS with a C18 chromatographic column,adopting the multiple reaction monitoring( MRM ) mode with negative electrospray ionization. The effects of the dosages of hydrochloric acid and the sorbents on the recoveries of the 19 PFAs were studied. For accurate quantitative analysis,the isotope internal standard method was used. The calibration curves were linear with the correla-tion coefficients over 0. 998 in the range of 0. 05-20 μg/kg for the 19 PFAs. The limits of detec-tion were 0. 004-0. 111 μg/kg. The limits of quantification were 0. 012-0. 370 μg/kg. The mean recoveries of the 19 PFAs at spiked levels of 0. 5,1. 0,2. 0 μg/kg were in the range from 80%to 128% with the relative standard deviations of 0. 31%-11. 1%. The developed method is rapid, simple,accurate. It is suitable for the determination of the 19 PFAs in large quantities of lamb liver samples.
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