School of Chemistry and Chemical Engineering, Henan University of Technology, Zhengzhou 450001, China.
J Chromatogr A. 2010 Jul 30;1217(31):5013-20. doi: 10.1016/j.chroma.2010.05.057. Epub 2010 Jun 2.
The paper described a new ionic liquid, 1,3-dibutylimidazolium hexafluorophosphate, as extraction solvent for extraction and preconcentration of organophosphorus pesticides (fenitrothion, parathion, fenthion and phoxim) from water and fruit samples by dispersive liquid-liquid microextraction combined with high-performance liquid chromatography. The effects of experimental parameters, such as extraction solvent volume, disperser solvent and its volume, extraction and centrifugal time, sample pH, extraction temperature and salt addition, on the extraction efficiency were investigated. An extraction recovery of over 75% and enrichment factor of over 300-fold were obtained under the optimum conditions. The linearity relationship was also observed in the range of 5-1000 microgL(-1) with the correlation coefficients (r(2)) ranging from 0.9988 to 0.9999. Limits of detection were 0.01-0.05 microgL(-1) for four analytes. The relative standard deviations at spiking three different concentration levels of 20, 100 and 500 microgL(-1) varied from 1.3-2.7, 1.4-1.9 and 1.1-1.7% (n=7), respectively. Three real samples including tap water, Yellow River water and pear spiked at three concentration levels were analyzed and yielded recoveries ranging from 92.7-109.1, 95.0-108.2 and 91.2-108.1%, respectively.
本文描述了一种新型离子液体 1,3-二丁基咪唑六氟磷酸盐，可作为萃取溶剂，通过分散液液微萃取与高效液相色谱联用，从水样和水果样品中萃取和预浓缩有机磷农药（fenitrothion、parathion、fenthion 和 phoxim）。考察了实验参数，如萃取溶剂体积、分散剂溶剂及其体积、萃取和离心时间、样品 pH 值、萃取温度和加盐量对萃取效率的影响。在最佳条件下，萃取回收率超过 75%，富集倍数超过 300 倍。在 5-1000 μg/L 范围内也观察到了线性关系，相关系数（r(2)）范围为 0.9988 至 0.9999。四种分析物的检出限为 0.01-0.05 μg/L。在 20、100 和 500 μg/L 三个不同浓度水平下，相对标准偏差为 1.3-2.7%、1.4-1.9%和 1.1-1.7%（n=7）。分析了包括自来水、黄河水和梨在内的三个实际水样，加标回收率在 92.7-109.1%、95.0-108.2%和 91.2-108.1%之间。
