高效液相色谱-串联质谱联用技术测定环境水样中的全氟化合物  

Determination of Perfluorinated Compounds in Water Samples by High Performance Liquid Chromatography-Electrospray Tandem Mass Spectrometry

作　　者：张萍[1] 史亚利[1] 蔡亚岐[1] 牟世芬[1] 

机构地区：[1]中国科学院生态环境研究中心环境化学与生态毒理学国家重点实验室,北京100085

出　　处：《分析化学》2007年第7期969-972,共4页Chinese Journal of Analytical Chemistry

基　　金：国家重点基础研究计划(973项目)(No2003CB415001);中国科学院重要方向性项目(NoKZCX2-YW-420-1)

摘　　要：采用HPLC—ESI—MS／MS联用技术，以C18反相柱为分析柱，以甲醇、醋酸铵为淋洗液，10min即可分离全氟庚酸（PFHeA）、全氟辛酸（PFOA）、全氟辛烷磺酸（PFOS）、全氟壬酸（PFNA）和全氟癸酸（PFDeA）5种全氟化合物。样品溶液500mL经RP柱离线浓缩、2mL甲醇洗脱、水定容至5mL后，50μL进样分析。以363／319、412．9／368．9、498．9／80、462．9／419和512．8／469离子对分别对PFHeA，PFOA，PFOS，PFNA和PFDeA进行监控和定量检测。线性范围在0．5～20ng／L之间（r≥0．9944），5种物质的检出限依次为0．10、0．15、0．11、0．11和0．18ng／L。该方法已成功运用于4种环境水样的测定，4ng／L的加标回收结果在52．6％～117．5％之间。A rapid and simple method was proposed for separation and determination of five perfluorinated compounds, perfluoroheptanic acid （PFHeA）, perfluorooctanic acid （PFOA）, perfluorooctanic sucfonic acid （PFOS）, perfluorononanic acid （PFNA） and perfluorodecanoic acid （PFDeA） by using high performance liquid chromatography/electrospray tandem mass spectrometry （LC/ESI-MS/MS） with a C18 reversed-phase column and CH3OH/NH4Ac eluent in 10 min. 500 mL sample liquor was concentrated by off-line RP cartridge, then washed with 2 mL methanol. The extractant solution was finally added with water to 5 mL before 50 μL injection. Transitions of 363/319,412.9/368.9,498.9/80,462.9/419 and 512.8/469 were selected to qualification and quantification of PFHeA, PFOA, PFOS, PFNA and PFDeA. Linear calibrations were acquired in the range of 0.5 - 20 ng/L with correlation coefficients more than 0. 9944. The detection limits （S/N=3） for these five PFCs were 0.10, 0.15, 0. 11, 0.11 and 0. 18 ng/L respectively. This method was applied to detect PFCs in environmental water samples. The recoveries were in the range of 52.6% - 117. 5%.

关 键 词：全氟表面活性剂 高效液相色谱-串联质谱 

分 类 号：X832[环境科学与工程—环境工程]