固相微萃取新技术——固态吸附搅拌棒

Solid Phase Microextraction(SPME)Technology-Stir Bar Sorptive Extraction(SBSE)

用溶胶-凝胶方法制备了多孔结构的萃取固定相并应用于纤维针式固相微萃取(SPME)和固相萃取搅拌棒(SBSE)。所制备的萃取固定相能耐受300oC的热解吸温度,此温度下没有明显的流失。多孔结构有利于萃取和热解吸的传质动力学过程。用SBSE或SPME-GC-TSD方法萃取和分析了蔬菜、橙汁和红葡萄酒中的有机磷农药(OPs)残留,除杀扑磷外,其它Ops的检测下限在10ng/L以内,整个分析的标准偏差(RSD)在20%以内。还用SBSE-GC-FID方法萃取分析了海水中的多环芳烃类化合物(PAHs),检测下限为3￣14ng/L。

Extraction phase of porous structure was prepared by sol-gel technology and was applied in solid phase microextraction. The phase can withstand 300℃ of desorption temperature without noticeable bleeding. The porous structure of the membrane enhances mass transfer process and benefits the dynamics of extraction and desorption. Extraction and determination of organophosphorus pesticides （OPs） in vegetables, orange juice and red wine by the SBSE or SPME-GC-TSD were validated. Limits of detection for OPs were below 10 ng/L except methidathion. Relative standard deviations （R.S.D.s） were in the range of 1%-20% for pesticides being tested. Determination of PAHs in sea water by SBSE-GC-FID was also demonstrated. Limits of detection for PAHs were between 3-14 ng/L.