近岸海水中全氟化合物的液相色谱-离子阱质谱法测定

建立了利用高效液相色谱-电喷雾离子阱质谱(HPLC-ESI-IT-MS/MS)测定近岸海水中多种常见全氟化合物(PFCs)的分析方法.采用固相萃取法(SPE)对海水中的PFCs净化富集,用HPLC-ESI-IT-MS/MS多反应离子监测(MRM)模式对各组分(全氟己烷磺酸、全氟辛烷磺酸、全氟辛烷磺酰胺、全氟己酸、全氟庚酸、全氟辛酸、全氟壬酸、全氟癸酸、全氟十一酸、全氟十二酸)进行测定.在最佳实验条件下,采用基质匹配标准曲线法定量,以消除海水基质的影响,8种目标化合物的检出限介于0.50—1.00 ng·L-1,9种PFCs的回收率在71.0%—130.2%之间,能满足近岸海水中多种PFCs检测的要求.青岛沿岸表层海水样品测定结果显示,全部采样站点的海水样品中均检测到≥4种PFCs,说明青岛沿岸海水中已有一定程度的PFCs污染.

Simultaneous determination of common perfluorinated compounds in coastal seawater by liquid chromatography-ion trap mass spectrometry

In this study,a new analytical method for the determination of 10 PFCs(PFHxS,PFOS,PFOSA,PFHxA,PFHpA,PFOA,PFNA,PFDA,PFuDA,PFDoA) in coastal seawater was developed.PFCs in seawater samples were concentrated and cleaned via solid-phase extraction(SPE),and then were simultaneously determined by high performance liquid chromatography coupled to electrospray ionization-ion trap mass spectrometry(HPLC-ESI-IT-MS/MS).Data acquisition was performed by applying multiple reaction monitoring(MRM) for the quantification of PFCs in coastal seawater.Under the optimal conditions,the matrix-matched calibration curves were constructed and the interference effect of seawater matrices on the ionization was effectively eliminated.The developed method was validated with satisfactory linearity,precision and stability.The limits of detection for eight PFCs were in the range of 0.50 to 1.00 ng·L-1.The recoveries of 9 PFCs in seawater samples ranged from 71.0% to 130.2%.The proposed method was efficient for the simultaneous determination of several common PFCs in coastal seawater.Analysis of all the seawater samples from Qingdao coast led to the detection of more than four different PFCs,which indicates that the coastal seawater of Qingdao has been contaminated by PFCs to a certain extent.