超高效液相色谱串联质谱法快速测定地下水和含水层介质中16种全氟烷基酸

Quick analysis of sixteen PFAAs in groundwater and aquifer by ultra-performance liquid chromatography-triple quadrupole mass spectrometry

全氟烷基酸(PFAAs)是一种新型的持久有机污染物,在各种环境介质中被频繁检出。目前,PFAAs的检测方法主要包括液相色谱串联质谱法(HPLC-MS/MS)、超高效液相色谱串联质谱法(UPLC-MS/MS)、气相色谱法和光谱类方法。但是,上述方法多存在样品前处理过程复杂、周期长、成本高的问题,不适用于PFAAs的快速检测。为此,本文建立了一种快速测量地下水和含水层介质中16种PFAAs的UPLC-MS/MS方法。水样过0.22μm滤膜后直接测定浓度,土样经过超声离心后,取上清液过滤测量浓度。本方法分别为16种PFAAs建立了低浓度(5~50μg/L)和高浓度(100~500μg/L)两条校准曲线,相关系数R^2>0.99。地下水中16种PFAAs快速检测方法检出限为0.06~1.07μg/L,回收率为75%~120%,精密度(RSD)为2.61%~9.19%(除高浓度时全氟丁烷磺酸和全氟已烷磺酸分别为11.34%和14.70%外)。含水层介质中14种PFAAs(全氟十三酸和全氟十四酸除外)方法检出限为2.69~12.33ng/g,回收率为65%~103%,精密度(RSD)为1.96%~7.22%。

Perfluorinated alkyl acids(PFAAs)are a group of emerging persistent organic pollutant that have received increasing attention due to their global occurrence,accumulation and toxicity.At present,PFAA detection mainly uses high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS),ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS),gas chromatography(GC)and spectroscopy.However,these detection methods often involve complicated sample pretreatment,longer work cycle and higher cost,therefore,they are not suitable for quick PFAA detection.In this study,we developed a method for quick analysis of 16 PFAAs in groundwater and aquifer based on UPLC-MS/MS.In the experiment,the groundwater sample was filtered through 0.22μm membrane and injected directly into the detection instrument;the aquifer sample was prepared by liquid solvent extraction.A good linear calibration using 16 PFAAs standards was achieved(R^2>0.99)in the low and high concentration ranges of 5-50 and 100-500μg/L,respectively.The method’s detection limits(MDLs)of 16 PFAAs in groundwater were 0.06-1.07μg/L,and the recovery rates were 75%-120% with relative standard deviations(RSD)at2.61%-9.19%.In aquifer media,MDLs of 14 PFAAs were 2.69-12.33 ng/L,and the recovery rates were65%-103% with RSDs at 1.96%-7.22%.