环境水样中三氟乙酸的分析  

Determination of trifluoroacetic acid in water samples by gas chromatograph-mass spectrometry

作　　者：王巧云[1,2] 丁翔[1,2] 李德军[1] 王新明[1] 

机构地区：[1]中国科学院广州地球化学研究所有机地球化学国家重点实验室,广东广州510640 [2]中国科学院研究生院,北京100049

出　　处：《分析试验室》2009年第5期68-71,共4页Chinese Journal of Analysis Laboratory

基　　金：国家重点基础研究发展计划(973)(2002CB810403)项目资助

摘　　要：建立了环境水样中三氟乙酸（TFA）的分析方法。环境水样加入内标物五氟丙酸后经旋转蒸发浓缩至约50mL，以2，4-二氟苯胺作衍生化剂，N，N’-二环己基二酰亚胺作催化剂，乙酸乙酯为溶剂，进行衍生化反应。三氟乙酸的苯胺产物经过一系列萃取、洗涤净化、浓缩定容等步骤后，采用气相色谱-质谱进行分析。该方法在0.61-24.4μg／L范围内呈线性关系（R^2〉0.997），检出限1.8ng／L，加标回收率在79.3％-94.8％之间。方法适用于环境水中的痕量TFA的分析。A method was presented for the analysis of trifluoroacetic acid （TFA） in water samples. After spiked with internal standard pentafluoropropionic acid （PFPA）, water samples were reduced to about 50 mL in volume using a rotary evaporator at 50℃, and then the derivatization reaction occurred in an aqueous mixture using 2, 4-difluoroline （2, 4-DFAn） to produce the acid anilide, with ethyl acetate as solvent and N, N＇-dicyclobexylcarbodiimide as the catalyst. A series of extraction, purification and concentration were conducted before TFA anilide product was analyzed by gas chromatography with mass selective detector in the selected ion monitoring mode. Good linear correlation coefficient （R^2〉0.997） was observed between the concentrations and responses for TFA and PFPA mixed standard solutions in the range of 0.61-24.4μg/L in ethyl acetate. The method detection limit was 1.8ng/L for 500 mL water sample. Recoveries in fortified samples were in the range of 79.3%-94.8%. The method was highly sensitive for the determination of trifluomacetic acid in environmental water samples.

关 键 词：三氟乙酸 环境水 衍生化 GC-MS 

分 类 号：O657.63[理学—分析化学]