固相萃取-气相色谱质谱法测定水样中5种邻苯二甲酸酯研究

摘要

建立了采用固相萃取技术结合气相色谱质谱法对5种邻苯二甲酸酯(PAEs) 进行富集、检测的方法,并成功应用于实际水样分析.实验中采用加标回收率来评价萃取效率,考察并优化了影响萃取效率的主要因素,包括固相萃取小柱的种类、洗脱剂类型、洗脱次数和用量、样品环境影响等.结果表明:在最佳萃取条件下,该法对5种PAEs(邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二丁酯、邻苯二甲酸丁基苄基酯和邻苯二甲酸(2-乙基己基)酯)具有较高的萃取效率;在浓度范围为0.50~10.0 mg/L时,线性相关系数为0.992 6~0.999 8;检出限为0.05~0.37μg/L,定量限为0.20~1.48μg/L,空白水样加标回收率范围为95%~115%,相对标准偏差为2.4%~11.1%.该方法操作简单、稳定性好、回收率高,可以用于测定实际水样中的PAEs类增塑剂.%A method of the solid-phase extraction coupled with gas chromatography-mass spectrometry (SPE-GC-MS) was developed for the determination of five typical phthalate esters(PAEs).The analyzed PAEs included dimethyl phthalate(DMP),diethyl phthalate(DEP),dibutyl phthalate(DBP),benzyl butyl phthalate(BBP) and bis (2-n-butoxyethyl) phthalate(DBEP).Experiments investigated and optimized the main factors on the extraction efficiency,including the types of extraction column,eluant type,washing times and sample condition etc.The calibration curves of phthalate esters showed good linearity in the range of 0.50~10.0 mg/L with the correlation coefficients(r) between 0.992 6 and 0.999 8.The limits of detection of phthalate esters in water samples ranged from 0.05 to 0.37 ug/L and the limits of quantitative ranged from 0.20 to 1.48 ug/L.The average recoveries of 5 analytes spiked in water ranged from 95% to 115% with the relative standard deviations (RSDs,n =6) of 2.4%~11.1%.The method is suitable for the determination of 5 phthalate esters simultaneously in water samples with easy operation,high recovery and stability.