微波辅助萃取-固相微萃取联用气相色谱-质谱法测定土壤中的扑草净  

Determination of Prometryne in Soil by Gas Chromatography-Mass Spectrometry Using Microwave-assisted Extraction Associated with Solid Phase Microextraction

作　　者：杨云[1] 栾伟[1] 罗学军[1] 李攻科[1] 

机构地区：[1]中山大学化学与化学工程学院,广州510275

出　　处：《分析化学》2004年第6期775-778,共4页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金 (No .2 0 3 75 0 5 0 );广东省自然科学基金 (No .990 2 92 );广东省高等学校"千百十工程"人才培养基金资助项目(No .Q校 0 2 0 0 6)

摘　　要：研究了微波辅助萃取 固相微萃取联用、气相色谱 质谱联用测定土壤中除草剂扑草净的分析方法。采用正交设计实验优化了萃取溶剂种类和体积、微波辐射时间和微波功率等微波辅助萃取条件 ;研究了SPME萃取涂层、搅拌速度、萃取时间和解吸时间等对萃取效率的影响。方法的检出限为 0 .0 1ng/g ;线性范围为 0 .2～ 2 0 0 μg/L。在优化的条件下测定了 5和 5 0ng/g的合成土壤样品 ,回收率分别为 90 .1 %和 91 .6 % ;相对标准偏差分别为 9.4 %和 8.8% (n =6 )。本法综合了微波辅助萃取和固相微萃取的优点 ,操作简便 ,灵敏度高 。A method of microwave-assisted extraction (MAE) associated with solid phase microextraction (SPME) followed by gas chromatography-mass spectrometry (GC-MS) for the determination of prometryne in soil was developed. The MAE conditions, such as the extraction solvent type and volume, microwave heating time and magnetron power output, were optimized by a three-level orthogonal array design. The SPME conditions such as extraction time, stir speed, desorption temperature and desorption time were studied in detail. The linear range of the method was from 0.2 to 200 mug/L, and the detection limit was 0.01 ng/g. Spiked soil samples were analyzed under the optimum conditions. The recoveries of 5 ng/g and 50 ng/g spiked samples were 90.1% and 91.6%, the RSD were 9.4% and 8.8% (n=6) respectively. The method combines the advantages of MAE and SPME. It is sensitive, simple, and effective for the extraction of trace organic compounds in solid samples.

关 键 词：土壤 扑草净 微波辅助萃取 固相微萃取 气相色谱-质谱法 环境分析化学 

分 类 号：O657.63[理学—分析化学]