阿特拉津及其降解产物的磺酸化聚合物柱固相萃取及高效液相色谱-质谱法测定  

Determination of Trace Atrazine and Its Environmental Degradation Products by Solid Phase Extraction and Liquid Chromatography/Mass Spectrometry

作　　者：任晋[1] 蒋可[1] 徐晓白[1] 

机构地区：[1]中国科学院生态环境研究中心

出　　处：《分析化学》2004年第10期1273-1277,共5页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金资助项目 (No .2 99770 2 3 )

摘　　要：建立了环境水样中痕量除草剂阿特拉津 (ATR)及其环境中的主要降解产物Deethylatrazine (DEA) ,Deisopropylatrazine (DIA) ,Hydroxyatrazine (HA)的OasisMCX(磺酸化 (二乙烯基苯 N 乙烯基吡咯烷酮 )共聚物 )小柱离线萃取 ,HPLC MS选择离子检测的分析方法。对MCX(6 0mg ,3mL)小柱的萃取条件 (样品溶液的 pH ,上样速率 ,上样体积 ,洗脱液 pH)进行了优化 ,得出最佳的实验条件。ATR ,DEA ,DIA ,HA的穿透体积均大于 4 5 0mL。本实验利用HPLC APCI选择离子模式对被分析物进行检测 ,5 0 0mL水样的化合物检出限为 0 0 1～ 0 0 6 μg/L ;回收率均大于 75 % ,符合欧盟饮用水中单种农药浓度不应超出 0 .1μg/L的检测标准。该方法用于官厅水库坝后水样的分析 ,测出该处水样中ATR为 2 .0 4 μg/L ,DEA为 11.4 μg/L ,DIA为 0 .75μg/L。This paper describes a sensitive and specific method for trace determination of atrazine and its main degradation products (DPS); deethylatrazine (DEA), deisopropylatrazine (DIA hydroxyatrazine (HA), deethyldeisopropylatrazine (DEDIA) in environmental water. A chemically modified'polymeric resin (sulfonated divinylbenzene -N-vinylpyrrolidone copolymer) for solid phase extraction (SPE) was applied to extract the trace analytes in environmental water followed by liquid chromatography-atmospheric pressure chemical ionization (APCI)/massspectrometry (MS). This sulfonated modified copolymer has high selectivity for atrazine and its Us, and the breakthrough experiments show that the atrazine. and three, Us, ( DEA, DIA, HA) have high sorption capacity except DEDIA. On extracting from 500 mL water with concentration of 50 ng/L, recoveries of the analytes were better than 80% with relative standard deviations lower than 7%., The analyte was detected in selected ion monitoring (SIM) mode using APCI-MS. Time-scheduled SIM of the molecular ion (cone 14 V) could be performed down to 10 similar to 20 ng/L levels. Some environmental surface water, has been analyzed in practice.

关 键 词：除草剂 阿特拉津 降解产物 磺酸化聚合物 固相萃取柱 高效液相色谱 质谱 环境水样分析 

分 类 号：O657.7[理学—分析化学]