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建立了高效液相色谱-串联质谱法(HPLC-MS/MS)对水体中7种全氟烷基酸(C4~C10)和全氟辛烷磺酸的分析方法。水样抽滤除去颗粒物杂质,加入回收率指示物,再使用WAX固相萃取柱富集和净化,提取液浓缩后,使用HPLC/MS/MS分析检测。仪器分析过程中,由于液相系统无法避免含氟材料的使用,引入了较高的全氟辛酸(PFOA)污染。本研究使用杂质延迟法实现了液相系统中PFOA和样品中PFOA的分离。在系统干扰去除后,水体中PFOA的方法检出限降低为0.8 ng/L(取样量500 mL),低定量浓度为3.2 ng/L;其它目标物的方法检出限为0.2~1.2 ng/L,低定量浓度为0.8~4.8 ng/L。本方法具有良好的重现性,6次平行样品测定中各检出化合物的相对标准偏差(RSD)均小于16%,6次基体加标实验中各目标物的回收率为87%~129%,RSD<15%。杂质延迟法有效的去除了系统干扰,降低了方法检出限,提高了方法精密度。
A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) method was developed for the determination of seven perfluoroalkyl acids (C4-C10) and perfluorooctane sulfonate in water. The water sample was filtered to remove particulate impurities, the recovery indicator was added, and the sample was concentrated and purified using a WAX solid phase extraction column. The extract was concentrated and detected by HPLC / MS / MS analysis. During instrumental analysis, PFOA contamination was introduced due to the inability of the liquid-phase system to avoid the use of fluorinated materials. In this study, impurity separation method was used to achieve the separation of PFOA from PFOA in the liquid system. The detection limit of PFOA in water was reduced to 0.8 ng / L (sample volume 500 mL) and low concentration of 3.2 ng / L after system interference removal. The detection limits of other targets were 0.2 ~ 1.2 ng / L, low concentration of 0.8 ~ 4.8 ng / L. The method has good reproducibility. The relative standard deviations (RSDs) of all detected compounds in six parallel samples were all less than 16%. The recoveries of all target compounds in six matrix spiking experiments were 87% -129% , RSD <15%. Impurity delay method effectively remove the system interference, reducing the method detection limit, improve the precision of the method.