建立了白酒中15种全氟化合物(PFCs)的分散固相萃取-高效液相色谱-串联质谱快速分析方法。1.0mL白酒样品用50mgPSA吸附剂进行富集净化,用50mmol/L三乙胺一甲醇液洗脱后,采用HPLC—ESI—MS—MS电喷雾负离子模式电离、多反应监测模式对样品进行检测,内标法进行定量分析。15种PFCs在0.1~20μg/L质量浓度范围内呈良好的线性关系,方法的检出限为0.03~0.15μg/L,定量限为0.10~0.45μg/L。在0.5、1.0、2.0、5.0μg/L4种添加水平下,15种PFCs的加标回收率为83.8%~119%。方法可用于多种白酒样品的分析。
A rapid method using dispersive solid phase extraction and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS-MS) was developed for the determination of 15 perfluorinated compounds (PFCs) in Chinese spirit. Totally 1.0 mL of samples were purified with 50 mg of PSA absorbents and eluted with 50 mmol/L triethylamine inmethanol. The extract was then detected by HPLC-MS-MS in a negative electrospray ionization (EI) mode with multiple reaction monitoring (MRM) using an internal standard method for quantitative determination. Good linearity was observed for 15 PFCs in the range from 0.1 to 20.0μg/L. The limits of detection were 0.03-0.15 μg/L while the limits of quantitation were 0.09-0.45 μg/L. The average recovery rate of 15 PFCs was 83.8%-119% at spiked levels of 0.500, 1.00, 2.00μg/L and 5.00 μg/L. The developed method is applicable to analyze several Chinese spirit samples.