Department of Chemistry, Shahid Beheshti University, G.C., Evin, Tehran, Iran.
Talanta. 2010 Nov 15;83(1):36-41. doi: 10.1016/j.talanta.2010.08.035. Epub 2010 Sep 27.
Temperature-controlled ionic liquid dispersive liquid phase microextraction (TCIL-DLPME) combined with high performance liquid chromatography-diode array detection (HPLC-DAD) was applied for preconcentration and determination of chlorobenzenes in well water samples. The proposed method used 1-butyl-3-methylimidazolium hexafluorophosphate ([C(4)mim][PF(6)]) as the extraction solvent. The effect of different variables on extraction efficiency was studied simultaneously using an experimental design. The variables of interest in the TCIL-DLPME were extraction solvent volume, salt effect, solution temperature, extraction time, centrifugation time, and heating time. The Plackett-Burman design was employed for screening to determine the variables significantly affecting the extraction efficiency. Then, the significant factors were optimized by using a central composite design (CCD) and the response surface equations were developed. The optimal experimental conditions obtained from this statistical evaluation included: extraction solvent volume, 75 μL; extraction time, 20 min; centrifugation time, 25 min; heating time, 4 min; solution temperature, 50 °C; and no addition of salt. Under optimal conditions, the preconcentration factors were between 187 and 298. The limit of detections (LODs) ranged from 0.05 μg L(-1) (for 1,2-dichlorobenzene) to 0.1 μg L(-1) (for 1,2,3-trichlorobenzene). Linear dynamic ranges (LDRs) of 0.5-300 and 0.5-500 μg L(-1) were obtained for dichloro- and trichlorobenzenes, respectively. The performance of the method was evaluated for extraction and determination of chlorobenzenes in well water samples in micrograms per liter and satisfactory results were obtained (RSDs<9.2%).
温度控制离子液体分散液相微萃取（TCIL-DLPME）结合高效液相色谱-二极管阵列检测（HPLC-DAD）用于预浓缩和测定井水样品中的氯苯。该方法采用 1-丁基-3-甲基咪唑六氟磷酸盐([C(4)mim][PF(6)])作为萃取溶剂。同时采用实验设计研究不同变量对萃取效率的影响。TCIL-DLPME 中的感兴趣变量包括萃取溶剂体积、盐效应、溶液温度、萃取时间、离心时间和加热时间。采用 Plackett-Burman 设计进行筛选，以确定显著影响萃取效率的变量。然后，通过使用中心组合设计（CCD）和响应面方程对显著因素进行优化。从该统计评估中获得的最佳实验条件包括：萃取溶剂体积 75 μL；萃取时间 20 min；离心时间 25 min；加热时间 4 min；溶液温度 50°C；不添加盐。在最佳条件下，预浓缩因子在 187 到 298 之间。检测限（LODs）范围为 0.05 μg L(-1)（1,2-二氯苯）至 0.1 μg L(-1)（1,2,3-三氯苯）。二氯苯和三氯苯的线性动态范围（LDRs）分别为 0.5-300 和 0.5-500 μg L(-1)。该方法用于井水样品中氯苯的萃取和测定，结果令人满意（RSDs<9.2%）。
