功能化离子液体/离子液体分散液-液微萃取测定水中苯氧羧酸类除草剂  

Functionalized Ionic Liquid / Ionic Liquid Dispersive Liquid-Liquid Microextraction for Determination of Phenoxy Acid Herbicides in Water Samples

作　　者：杨素萍[1] 郭振福[1] 刘敏[1] 王素利[1] 

机构地区：[1]河北北方学院理学院和食品安全研究中心,张家口075000

出　　处：《分析化学》2015年第6期904-908,共5页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(No.21177155);河北省自然基金(No.B2011405007);河北北方学院创新人才项目(Nos.CXRC1301;CXTD1306)资助~~

摘　　要：建立了功能化离子液体/离子液体分散液-液微萃取（FIL/IL-DLLME）测定水中4种苯氧羧酸类除草剂的农药残留分析方法。离子液体[C4MIMBF4]有助于难溶于水的[C6Hy MIMTf2N]在水相中形成液滴。离子对[Li Tf2N]的引入有利于提高功能离子液体对分析物的提取效率,对影响萃取效率的重要因素进行选择和优化,最佳条件为：100μL[C6Hy MIMTf2N]）作为提取剂,100μL[C4MIMBF4]作为分散剂,在30℃下超声5 min,[Li Tf2N]浓度为5%和样品溶液的p H=2。在最佳优化条件下,5~500μg/L范围内线性良好,相关系数为0.9953~0.9996;对自来水、河水、田间水进行浓度为10和20μg/L添加回收实验,回收率为70.2%~107.5%,相对标准偏差RSD〈10%,检出限为0.05~0.2μg/L,得到满意的结果,说明本方法对于实际样本的检测具有可行性。Functionalized ionic liquid/ionic liquid ultrasound-assisted dispersive liquid-liquid microextraction （FIL/IL-DLLME） was developed for the determination of four phenoxy herbicides in water samples. The extraction procedure was induced by the formation of cloudy solution, which was composed of fine drops of [ C6HyMIMTf2N], dispersed entirely into sample solution with the help of hydrophilic [ C4MIMBF4 ]. The introduction of ion-pairing agent （ [ LiTfz N ] ） was beneficial to the improvement of the extraction efficiency. The main parameters relevant to this method were investigated and optimized as follows： 100 μL of [ C6HyMIMTf2N] and 100 p,L of [ CgMIMBF4 ~ were used as extraction solvent and dispersion, the ultrasonic time was fixed for 2 min at 30℃, 6% [LiTf2N] was added and the pH of sample solution was adjusted to 2. Under the optimum conditions, the linear correlation coefficient ranged from 0. 9953 to 0. 9996 for concentration levels of 5 -500 μg/L and the limits of detection （LODs） for the herbicides were between 0.05 μg/L and 0.2 μg/L. The recoveries （70.2%-107.5% ） of the target analytes were obtained in tap water, river water and field water at two spiked levels of 10 and 20 μg/L, the relative standard deviations （RSDs, n=6） were less than 10%, The results indicated that the proposed method was effective for the determination of phenoxy acid herbicides in water samples.

关 键 词：功能离子液体 分散液-液微萃取 高效液相色谱 苯氧羧酸类除草剂 水样 

分 类 号：O652.62[理学—分析化学] X832[理学—化学]