分散液液微萃取-柱前衍生-高效液相色谱法测定水样中双酚A  

Combination of Dispersive Liquid-Liquid Microextraction and Pre-column Derivatization-High Performance Liquid Chromatography for Determination of Bisphenol A in Water Sample

作　　者：李鱼[1,2] 刘建林[1] 翦英红[2] 

机构地区：[1]华北电力大学能源与环境研究中心,北京102206 [2]吉林大学环境与资源学院,长春130012

出　　处：《分析化学》2009年第10期1484-1488,共5页Chinese Journal of Analytical Chemistry

基　　金：国家"973"计划项目(No.2004CB3418501)资助

摘　　要：建立了分散液液微萃取-柱前衍生-高效液相色谱法测定水样中双酚A的分析方法。通过交互正交试验和混合型优化实验设计对影响因素(萃取剂体积、分散剂类型及其体积、水样体积、pH值及离子强度)进行了优化。优化后的分散液液微萃取条件为:60μL萃取剂,0.4mL分散剂(甲醇),pH4.0;优化后的柱前衍生化条件:0.1mL2.0g/L衍生剂(对硝基苯甲酰氯)、衍生化时间30min;方法的线性范围:0.002～0.2mg/L(r=0.9997),检出限0.007μg/L(S/N=3);不同浓度双酚A的萃取率为59.0%～63.0%,相对标准偏差(RSD)2.5%～9.2%(n=5);水样中双酚A的加标率为86.5%～107.1%,RSD为4.0%～11.9%(n=5),其它雌激素(雌酮、雌二醇、雌三醇和17α-乙炔基雌二醇)对双酚A的测定无干扰。本方法可以对水环境中的痕量BPA进行检测,具有操作简便、快速等优点。An analytical method,dispersive liquid-liquid microextraction-pre-column derivatization-high performance liquid chromatography,was developed for the determination of bisphenol A（BPA） in water sample.Several factors,influencing the performance of dispersive liquid-liquid microextraction（DLLME） such as extractant volume,disperser type and volume,water volume,pH,and ionic strength,were studied and optimized using interactive orthogonal array and mixed level design experiments.The optimized dispersive liquid-liquid microextraction conditions were as follows：the volume of extractant was 60 μL,the volume of dispersive solvent（methanol） was 0.4 mL,and the value of pH was fixed at 4.0.The optimal pre-column derivatization conditions were as follows：the concentration of P-nitrophenyl chloride was 2.0 g/L and volume was 0.1 mL,the derivatization time was 30 min.The linear range of the proposed method was 0.002-0.2 mg/L with r=0.9997,and the limit of detection was 0.007 μg/L at S/N=3.The extraction recovery ranged from 59.0% to 63.0% with relative standard deviation（RSD） between 2.5%-9.2%（n=5）.The relative recovery（R） varied from 86.5% to 101.0%,and the RSD was in the range of 4.0%-11.9%（n=5）.Meanwhile,the determination of BPA was not interfered by other estrogens such as estrone,estradiol,estriol,and 17α-ethynylestradiol.The developed method was simple and fast for the trace level BPA determination in water sample.

关 键 词：分散液液微萃取 柱前衍生 高效液相色谱 双酚A 

分 类 号：X832[环境科学与工程—环境工程]