固相萃取-气相色谱/质谱联用法同时检测水体中9种环境雌激素  

Simultaneous Detection of Nine Kinds of Estrogens in Water by Solid Phase Extraction Coupled with Gas Chromatography-Mass Spectrometry

作　　者：廖涛[1] 吴晓翠[1,2] 王少华[1] 谢松光[3] 熊光权[1] 耿胜荣[1] 李新[1] 鉏晓艳[1] 胡筱波[2] 

机构地区：[1]湖北农业科技创新中心,湖北省农业科学院农产品加工与核农技术研究所/湖北省农产品辐照工程技术中心,武汉430064 [2]华中农业大学食品科学技术学院,武汉430070 [3]中国科学院水生生物研究所,武汉430072

出　　处：《分析化学》2013年第3期422-426,共5页Chinese Journal of Analytical Chemistry

基　　金：湖北省国际合作项目(No.2010BFA019);湖北省自然科学基金项目(No.2009CDB265);湖北省农科院青年科学基金项目(No.2012NKYJJ17)资助

摘　　要：建立了固相萃取-气质联用法(SPE-GC-MS)测定水体中9种环境雌激素:雌酮(E1)、17b-雌二醇(E2)、雌三醇(E3)、4-辛基酚(OP)、4-壬基酚(NP)、双酚A(BPA)、己烯雌酚(DES)、美雌醇(EE3ME)和17a-炔雌醇(EE2)的检测方法,优化了萃取和衍生化反应条件,实验结果表明:HLB柱回收率较高,衍生化反应的温度为75℃,衍生时间为90 min;本方法对9种环境雌激素的加标回收率为60.5%～126.7%,对应的相对标准偏差为0.8%～11.1%,方法检出限为1.08～8.60 ng/L,并将本方法应用于实际环境水样的检测。Nine target compounds including estrone （ E1 ）, 17/3-estradiol （ 17fl-E2 ）, estriol （ E3 ）, 4-oetylphenol （ 4-OP ）, 4-nonylphenol （ 4-NP ）, bisphenol A （ BPA ）, diethylstilbestrol （ DES ）, mestranol （EE3ME） and 17a-ethinyl estradiol （17a-EEl） were simultaneous detected by SPE-GC-MS. Extraction and derivatization conditions were optimized. The results showed that the average recoveries of the nine target estrogens extracted by Oasis HLB cartridges were higher than those by Satara cartridges, the optimal temperature of derivatization reaction was 75 ~C and the optimal time of derivatization reaction was 90 rain. The average recoveries of the nine target estrogens by Oasis HLB cartridges were 60.5% -126.7%, and the relative standard deviations （RSD） were 0.8% -11.1%, and the limits of detection （LOD） ranged from 1.08 ng/L to 8.60 ng/L. This method has been employed to detect the estrogens in environment samples from rivers.

关 键 词：环境雌激素 固相萃取 气相色谱 质谱联用法 

分 类 号：X832[环境科学与工程—环境工程] O657.63[理学—分析化学]