离子液体微波辅助液相萃取-高效液相色谱法同时测定土壤中5种微量有机氧农药  

Ionic liquid-based microwave-assisted extraction followed high-performance liquid chromatography for the simultaneous determination of five organic oxygen pesticides in soil samples

作　　者：董社英[1] 胡清[1] 李靖[1] 付一乐[1] 邢远清[1] 黄廷林[2] 

机构地区：[1]西安建筑科技大学理学院,西安710055 [2]西安建筑科技大学环境与市政工程学院,西安710055

出　　处：《分析试验室》2013年第8期48-52,共5页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金重点项目(50830303);长江学者与创新团队发展计划(IRT0853);陕西省科学技术研究发展计划项目(2012k08-12);陕西省教育厅专项研究基金(11JK0570)资助

摘　　要：采用离子液体([BMIm]PF6)微波辅助液相萃取-高效液相色谱法建立同时测定土壤中5种有机氧农药(6-糠氨基嘌呤、咪唑乙烟酸、2,4-二氯苯氧乙酸、苄嘧磺隆、烯效唑)的残留分析方法。研究了离子液体的种类和浓度、微波功率、时间、温度对色谱峰面积的影响。并检测了西安近郊地区苹果园和葡萄园土壤样品,在2种浓度添加水平2.00和20.0μg/mL下,5种有机氧农药的平均回收率分别为76.4%～125.0%和86.2%～117.0%,相对标准偏差(RSD)为1.2%～13%和3.9%～17%(n=6),方法检出限为0.03～0.13μg/mL。研究表明离子液体微波辅助液相微萃取可有效地萃取土壤中有机氧农药的残留。Ionic liquid-based（[BMIM]PF6） microwave-assisted extraction（IL-MAE） was successfully developed for the pretreatment of five organic oxygen pesticides（6-KT,imazethapyr,2,4-D,bensulfuron,uniconazole） to the determination by high-performance liquid chromatography（HPLC）.Several experimental parameters influencing extraction and determination such as the type and concentration of ionic liquids,microwave power,microwave time,and microwave temperature were investigated.Under the optimal conditions,limits of detections for five analytes were in the range of 0.03 ～ 0.13 μg /mL.The relative standard deviations at spiked two different concentration levels of 2.000 μg /mL and 20.00 μg /mL varied between 1.2% and 17%（n =6）.Two real samples including vineyard soil and orchard soil at two concentration levels were analyzed,and recoveries ranged from 76.40% to 125.0% and 86.20% ～ 117.0%,respectively.The results showed that IL-MAE method using（[BMIM]PF6） could be used for concentrating five organic oxygen pesticides effectively in soils with the advantages of high extraction efficiency,good sensitivity,simplicity and environment-friendly.

关 键 词：离子液体([BMIm]PF6) 微波萃取 高效液相色谱 有机氧农药 土壤样品 

分 类 号：O657.7[理学—分析化学]