吹扫捕集/气相色谱-质谱法测定水中痕量全氟碘烷类化合物

Determination on Trace of Polyfluorinated Iodine Alkanes in Water Using Purge and Trap/Gas Chromatography-Mass Spectrometry

利用吹扫捕集/气相色谱-质谱联用技术,建立了一种同时测定水中9种全氟碘烷类化合物的新方法,并对捕集管的型号、吹扫温度、吹扫时间、解吸时间及盐效应等样品吹扫条件进行了优化。在最佳实验条件下,9种全氟碘烷类化合物在0. 1～100μg·L-1范围内线性关系良好,相关系数(r2)不小于0. 996,方法检出限为5. 6～15 ng·L-1,定量下限为17～36 ng·L-1。在高、中、低3个加标水平下,9种全氟碘烷类化合物的回收率为75. 7%～118%,相对标准偏差为2. 2%～8. 3%。将建立的方法用于某典型污染区域环境水样的分析,检出9种全氟碘烷类化合物,质量浓度为21. 3～469 ng·L-1。

A novel gas chromatography-mass spectrometric(GC-MS)method coupled with purge and trap was developed for the simultaneous determination of nine neutral volatile polyfluorinated iodine alkanes(PFIs)in water samples.Several P&T parameters such as type of traps,purge time,purge temperature,desorbing time and ionic strength were optimized.Under the optimal conditons,the calibration curves for the nine PFIs showed good linear relationships(r 2≥0.996)in the concentration range of 0.1-100μg·L-1.The limits of detection(LOD)ranged from 5.6 ng·L-1 to 15 ng·L-1,and the limits of quantitation were from 17 ng·L-1 to 36 ng·L-1.The spiked recoveries for the analytes in water samples were in the range of 75.7%-118%with relative standard deviations(RSDs,n=7)of 2.2%-8.3%.The method was applied in the detection of volatile PFIs in water samples from the vicinity of a fluorochemical manufacturing plant,and nine PFIs were detected,with concentrations of 21.3-469 ng·L-1.