顶空衍生固相微萃取-气相色谱质谱法测定聚碳酸酯树脂中的环境雌激素  

Determination of enviromental estrogens in polycarbonate resins by solid phase microextracion with headspace derivatization and gas chromatography-mass spectrometry

作　　者：王楼明[1] 李英[1] 刘丽[1] 刘志红[1] 张琛[1] 叶锐均[1] 张昱[1] 庄绵雄[1] 

机构地区：[1]深圳出入境检验检疫局,深圳5118045

出　　处：《分析试验室》2006年第8期79-83,共5页Chinese Journal of Analysis Laboratory

基　　金：深圳出入境检验检疫局2001年科研项目(SZK15-2001)

摘　　要：建立了固相微萃取-气相色谱质谱联用测定聚碳酸酯树脂中环境雌激素4-枯基苯酚和双酚A的分析方法。优化了固相微萃取纤维、萃取温度和时间、解吸时间、搅拌速度、pH等萃取条件及衍生化温度和时间、衍生化方式等衍生化条件,并对样品浸泡时间、浸泡温度等进行了研究。方法的线性范围为0.05μg/L^1 mg/L,4-枯基苯酚和双酚A的检出限分别为50 ng/L和0.5 ng/L,相对标准偏差(RSD,n=5)分别为5.2%和1.6%,平均回收率(n=3)在90.50%~107.3%之间,该方法简单、快速、灵敏。A method for the determination of 4-cumylphenol and bisphenol A in polycarbonate resins by chromatography-mass spectrometry （GC-MS） using solid phase microextraction （SPME） was developed. Extraction and derivatization conditions, such as fibers for SPME, extraction temperature, extraction time, desorption time, stirring rate, pH, derivatization time, derivatization temperature, and derivatization manner were optimized. The dipping time and temperature were studied too. The linear ranges were from 0.05 μg/L to 1 mg/L, and the detection limits of 4-cumylphenol and Bisphenol A were 50 and 0.5 ng/L respectively. The relative standard deviations of the peak area were 5.2% and 1.6%. The recoveries range from 90.50% to 107.3% （ n = 3）, The method is simple, fast and sensitive.

关 键 词：固相微萃取 衍生化 气相色谱-质谱 聚碳酸酯树脂 环境雌激素 

分 类 号：O657.7[理学—分析化学]