高效液相色谱-串联质谱法测定葡萄酒中14种全氟化合物

Determination of 14 Perfluorinated Compounds in Wine by High Performance Liquid Chromatography-Mass Spectrometry

建立了葡萄酒中14种全氟化合物的高效液相色谱-串联质谱分析方法。采用WAX固相萃取柱对3.0mL葡萄酒样品进行富集净化,然后用10mmol/L三乙胺-甲醇混合液进行洗脱,洗脱液经氮气浓缩,甲醇定容后,采用Poroshell 120 EC-C18色谱柱分离,电喷雾负离子多反应监测（MRM）模式检测,内标法进行定量分析。14种全氟化合物在0.1～20.0μg/L浓度范围内线性相关系数r〉0.998,检出限为0.02～0.19μg/L,定量限为0.16～0.63μg/L。在添加浓度为0.5,1.0和5.0μg/L水平下,14种全氟化合物的加标回收率为83.0%～117.0%,相对标准偏差均小于15.0%。

A LC-MS/MS method had been developed for the determination of 14 perfluorinated compounds （PFCs）in wine. About 3.0 mL wine sample was purified and enriched by WAX cartridge, and then it was eluted with 10 mmoL/L triethylamine-methanol solution. The eluent was evaporated under nitrogen and redissolved by methol. The preparation was separated with a Poroshell 120 EC-Cls colunm and detected by electrospray ionization in negative mode using multiple reaction monitoring （MRM）. Internal standard method was used for quantitative analysis. The linear correlation coefficients （r） of all 14 PFCs were more than 0.998 in the concentration range of 0. 1-20.0 μg/L. The limits of detection （LODs） of PFCs were between 0.02 and 0.19 μg/L, while the limits of quantitation （LOQs） were between 0.16 and 0.63 μg/L. The recoveries of all PFCs were at 83.0%-117.0%, and the relative standard deviations were less than 15.0% at the spiked levels of 0.5, 1.0 and 5.0 μg/L. The developed method had been applied to the analysis of several wine samples.