杂质延迟法去除液相系统中全氟辛酸的干扰  

Elimination of Perfluorooctanoic Acid Interference from Liquid Chromatography System by Impurity Delay

作　　者：张秀蓝[1] 郭婧[1] 李玲玲[1] 董亮[1] 史双昕[1] 张利飞[1] 周丽[1] 杨文龙[1] 黄业茹[1] 

机构地区：[1]国家环境保护二噁英污染控制重点实验室,国家环境分析测试中心,北京100029

出　　处：《分析化学》2014年第3期452-456,共5页Chinese Journal of Analytical Chemistry

基　　金：环保公益重大项目资助项目(Nos.20100902601,2010IM031000)

摘　　要：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）,最低定量浓度为3.2 ng/L;其它目标物的方法检出限为0.2～1.2 ng/L,最低定量浓度为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 spectrometric （HPLC-MS/MS） method was developed for the determination of seven perfluorinated alkyl acidin （ C4 -C10 ） and perfluorooctane sulfonate in water. After the particulate was removed by leaching, surrogate standard was added, then the sample was loading to a pre-conditioned WAX cartridge for purification, and then the eluent was concentrated and analyzed by HPLC-MS/MS. Due to the situation that the fluoride polymer was unavoidable to be used in the LC system, a delay column was employed and the perfluorooctanoic acid （PFOA） of interference was departed from the PFOA in sample. The method detection limit （MDL） of PFOA was O. 8 rig/L, and the lowest quantitative concentration （LQC） was 3.2 ng/L. For other compounds, the MDL was ranged from 0.2 to 1.2 ng/L, and the LQC was 0.8-4.8 ng/L. This method also had good reproducibility, for six duplicated samples, the relative standard deviations （RSD） of all target compounds were less than 16%. And the recoveries of target compounds at six spiked matrix samples ranged from 87% to 129% , and the RSD were less than 15%. Because of the connection of delay column, the background was well controlled, and a relatively lower MDL were obtained.

关 键 词：水 全氟辛酸 全氟化合物 杂质延迟法 干扰去除 

分 类 号：O652[理学—分析化学]