Department of Analytical Chemistry, University of P. J. Šafárik, Košice, Slovakia.
J Sep Sci. 2013 Mar;36(5):932-8. doi: 10.1002/jssc.201200614. Epub 2013 Feb 4.
Three modes of liquid-liquid based microextraction techniques--namely auxiliary solvent-assisted dispersive liquid-liquid microextraction, auxiliary solvent-assisted dispersive liquid-liquid microextraction with low-solvent consumption, and ultrasound-assisted emulsification microextraction--were compared. Picric acid was used as the model analyte. The determination is based on the reaction of picric acid with Astra Phloxine reagent to produce an ion associate easily extractable by various organic solvents, followed by spectrophotometric detection at 558 nm. Each of the compared procedures has both advantages and disadvantages. The main benefit of ultrasound-assisted emulsification microextraction is that no hazardous chlorinated extraction solvents and no dispersive solvent are necessary. Therefore, this procedure was selected for validation. Under optimized experimental conditions (pH 3, 7 × 10(-5) mol/L of Astra Phloxine, and 100 μL of toluene), the calibration plot was linear in the range of 0.02-0.14 mg/L and the LOD was 7 μg/L of picric acid. The developed procedure was applied to the analysis of spiked water samples.
比较了三种基于液-液的微萃取技术模式——辅助溶剂辅助分散液-液微萃取、低溶剂消耗辅助溶剂辅助分散液-液微萃取和超声辅助乳化微萃取。苦味酸被用作模型分析物。测定基于苦味酸与 Astra Phloxine 试剂的反应，生成易于用各种有机溶剂萃取的离子缔合物，然后在 558nm 处进行分光光度检测。比较的每个程序都有优点和缺点。超声辅助乳化微萃取的主要优点是不需要危险的氯化萃取溶剂和分散溶剂。因此，选择该程序进行验证。在优化的实验条件下（pH 3、7×10(-5)mol/L Astra Phloxine 和 100μL 甲苯），校准曲线在 0.02-0.14mg/L 范围内呈线性，苦味酸的检出限为 7μg/L。所开发的程序被应用于加标水样的分析。
