基于低共熔溶剂的涡旋辅助悬浮固化-分散液液微萃取/高效液相色谱法测定水中三氯生与三氯卡班  

Determination of Triclosan and Triclocarban in Water Samples by High-performance Liquid Chromatography with Dispersive Liquid-Liquid Microextraction Based on Vortex-assisted Solidification of Floating Deep Eutectic Solvent

作　　者：陈梦轩 吴友谊[1,2] 周韫璐 许梦琪 CHEN Meng-xuan;WU You-yi;ZHOU Yun-lu;XU Meng-qi(School of Environmental Science and Engineering,Suzhou University of Science and Technology,Suzhou 215009,China;Jiangsu Key Laboratory of Environmental Science and Engineering,Suzhou 215009,China)

机构地区：[1]苏州科技大学环境科学与工程学院,江苏苏州215009 [2]江苏省环境科学与工程重点实验室,江苏苏州215009

出　　处：《分析测试学报》2020年第4期507-513,共7页Journal of Instrumental Analysis

基　　金：国家“十三五”水专项课题(2017ZX07205-02);江苏省环境科学与工程重点实验室项目(Zd1805)。

摘　　要：建立了基于低共熔溶剂的涡旋辅助悬浮固化-分散液液微萃取(VA-DLLME-SFDES)结合高效液相色谱测定水样中三氯生和三氯卡班的新方法。合成了6种疏水性低共熔溶剂(DES)并测定其密度、熔点和辛醇-水分配系数(KOW)。选取其中低密度、合适凝固点的DES作为萃取剂,样品经涡旋辅助萃取后冷冻,萃取剂固化附着于离心管内壁,弃去水相后,融化离心进样。最佳萃取条件为:选取由薄荷醇∶十二醇(摩尔比为1∶2)制备的DES作为萃取剂,萃取剂用量为70μL,水样pH值调至5.0,涡旋时间为1 min。在最优条件下,三氯生和三氯卡班分别在0.59~100μg/L和0.26~100μg/L质量浓度范围内线性关系良好(r2=0.9998),方法检出限(S/N=3)为0.08~0.18μg/L,富集倍数为141~148倍,回收率为86.0%~115%,日内精密度(n=6)和日间精密度(n=6)均不大于5.4%。该方法简便、快速,且萃取相易于收集,适用于水中三氯生和三氯卡班的测定。A novel high-performance liquid chromatography(HPLC)with dispersive liquid-liquid microextraction based on vortex-assisted solidification of floating deep eutectic solvent(VA-DLLME-SFDES)was established for the determination of triclosan and triclocarban in water samples.Six hydrophobic deep eutectic solvents(DESs)were newly synthesized,which physical and chemical constants such as density,melting point and octanol-water partition coefficient(KOW)were determined.One of the low-density DES with suitable freezing point was selected as the micro-extractant.After vortex-assisted extraction and freezing,the extractant was solidified and attached to the inner wall of the centrifuge tube.After removing the aqueous phase,the DES was melted and centrifuged in room temperature,and followed by HPLC analysis.The optimum extraction conditions were as follows:DES prepared with menthol-1-dodecanol(1∶2,molar ratio)as extraction solvent,volume of extraction solvent:70μL,pH of water sample:5.0,vortex time:1 min.Under the optimum conditions,there were good linearities for triclosan and triclocarban in the concentration ranges of 0.59-100μg/L and 0.26-100μg/L,respectively,with their correlation coefficients(r2)of 0.9998 and limits of detection(S/N=3)of 0.08-0.18μg/L.The enrichment factors for the analytes varied from 141 to 148.Meanwhile,the recoveries were in the range of 86.0%-115%with intra-precision(n=6)and inter-precision(n=6)not more than 5.4%.The method is simple,rapid and easy in collecting the extraction phase,and it is suitable for the determination of triclosan and triclocarban in water.

关 键 词：疏水性低共熔溶剂 悬浮固化 分散液液微萃取 湖水 三氯生 三氯卡班 

分 类 号：O657.7[理学—分析化学] X132[理学—化学]