摘要
研究了固相微萃取(SPME)/高效液相色谱(HPLC)联用测定环境中痕量邻苯二甲酸酯的分析方法.比较了5种不同类型涂层对5种邻苯二甲酸酯的萃取效果,采用3因素3水平正交实验设计对SPME的条件如萃取时间,离子强度,解吸时间等进行了优化.SPME优化的条件为:65 μm聚二甲基硅烷/乙烯苯(PDMS/DVB)涂层,室温,搅拌速率1 100r/min,萃取时间30 min,纯乙腈解吸,解吸时间2 min.HPLC的条件:C 18反相色谱柱,乙腈-水(体积比60:40)梯度淋洗,流速1 mL/min,紫外检测波长228 nm.方法的线性范围为0.50～80.00μg/L,检出限为0.11～2.20μg/L,相对标准偏差(n=6)为2.5%～9.6%.用于自来水、凉开水和雨水等实际水样的分析,回收率为82%～128%.
A solid-phase microextraction（SPME） mefhcd coupled with HPLC/UV was developed and validated for the determination of five phthalate esters （dimethyl-, diethyl-, di - n -butyl -, butylbenzyl-, di - 2- ethylhexyl- and di-n-octyl phthalate） in water samples. Five different types of SPME polymer coatings were investigated. On the basis of orthogonal experiments with three factors, three levels and nine groups, the SPME experimental conditions, such as extraction time, effects of ion strength, and thermal desorption time were optimized. The optimized parameters for the SPME method were as follows： 65μm PDMS/DVB fiber, room temperature, stirring rate of 1 100 r/min, extraction time of 30 rain. thermal desorption time of 5 min, and use of acetonitrile as desorption solution. Acetonitrilewater（60 ： 40 by volume） was used as the mobile phase with gradient elution on the C18 reversed phase chromatography column, and the flow rate was 1 mL/min. The detection wavelength was 228 nm with the UV - VIS detector. The linear range of the method was determined to be from 0.50 to 80.00μg/L, and the detection limit varied from 0.11 to 2.20μg/L. The relative standard deviation （n = 6） was 2.5 % - 9.6%. This method was used for determination of phthalate esters in water sample, such as tap, boiled and rain water, and the recoveries ranged from 82% to 128% . The method is fast, convenient, sensitive, solvent-free, and suitable for the determination of trace phthalate esters in environmental water samples.
出处
《分析测试学报》
CAS
CSCD
北大核心
2005年第5期35-38,共4页
Journal of Instrumental Analysis
基金
广东省自然科学基金资助项目(031586)
广东省高等学校"千百十工程"优秀人才培养基金资助项目(Q校02006)
贵州省科学技术基金资助项目
关键词
固相微萃取
高效液相色谱
邻苯二甲酸酯
水样
Solid-phase microextraction, High-performance liquid chromatography
Phthalate esters, Water sample
