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机构地区:[1]茂名学院化工与环境工程分院,茂名525000 [2]广东工业大学测试中心,广州510090 [3]农业部珠江流域渔业生态环境检测中心珠江水产研究所,广州510380
出 处:《分析试验室》2007年第5期68-71,共4页Chinese Journal of Analysis Laboratory
基 金:茂名学院重点课题基金(203251)项目资助
摘 要:利用固相萃取技术富集了水中5种邻苯二甲酸酯类(邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二(2-乙基己基)酯(DEHP)、邻苯二甲酸二辛酯(DOP)).借助均匀设计法及计算机回归建模优化技术对5种PAEs的固相萃取条件进行了设计与优化,得到最佳固相萃取条件为: 洗脱剂配比: V(正己烷)∶V(丙酮)=30∶1,洗脱体积2 mL,洗脱流速为4 mL/min,上样流速8 mL/min.富集后的样品用带电子捕获检测器的毛细管气相色谱检测,方法的线性范围为1~1000 μg/L (DMP,DEP,DOP),0.2~100 μg/L (DBP,DEHP);线性回归方程的相关系数为0.9970~1.000,检出限为0.02~0.4 μg/L,方法回收率为69%~117%,相对标准偏差为2.2%~9.5%.Solid phase extraction (SPE) technology coupled to GC-ECD was developed and validated for the trace analysis of phthalic acid esters (PAEs), namely Dimethyl phthalate (DMP), Diethyl phthalate (DEP), Di-n-butyl phthalate (DBP), Di-2-ethylhexyl phthalate (DEHP), Di-n-octyl phthalate (DOP). The C18 extraction conditions were optimized by homogeneous design and the related mathematical regressive model obtained by CRT Technology. The final C18 method employs hexane: acetone 30 : 1, elution volume 2 mL, elution flow rate 4 mL/min, sampling flow rate 8 mL/min. The linear response of the proposed method were in the range of 1 - 1000 μg/L ( DMP, DEP, DOP), and in the range of 0.2 - 100 μg/L ( DBP, DEHP) ; The correlation coefficients for the regression equations were 0.9970- 1.000. The limits of quantification of the method ranged from 0.02 to 0.4 μg/L. Recoveries were in the range of 69% - 117% and RSDs were in the range of 2.2% -9.5%.
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