School of Chemistry and Chemical Engineering, Henan University of Technology, Zhengzhou 450001, China.
Anal Chim Acta. 2009 Nov 23;655(1-2):52-9. doi: 10.1016/j.aca.2009.09.044. Epub 2009 Oct 6.
Using 1-octyl-3-methylimidazolium hexafluorophosphate ([C(8)MIM][PF(6)]) ionic liquid as extraction solvent, organophosphorus pesticides (OPPs) (parathion, phoxim, phorate and chlorpyifos) in water were determined by dispersive liquid-liquid microextraction (DLLME) combined with high-performance liquid chromatography (HPLC). The extraction procedure was induced by the formation of cloudy solution, which was composed of fine drops of [C(8)MIM][PF(6)] dispersed entirely into sample solution with the help of disperser solvent (methanol). Parameters including extraction solvent and its volume, disperser solvent and its volume, extraction time, centrifugal time, salt addition, extraction temperature and sample pH were investigated and optimized. Under the optimized conditions, up to 200-fold enrichment factor of analytes and acceptable extraction recovery (>70%) were obtained. The calibration curves were linear in the concentration range of 10.5-1045.0 microg L(-1) for parathion, 10.2-1020.0 microg L(-1) for phoxim, 54.5-1089.0 microg L(-1) for phorate and 27.2-1089.0 microg L(-1) for chlorpyifos, respectively. The limits of detection calculated at a signal-to-noise ratio of 3 were in the range of 0.1-5.0 microg L(-1). The relative standard deviations for seven replicate experiments at 200 microg L(-1) concentration level were less than 4.7%. The proposed method was applied to the analysis of four different sources water samples (tap, well, rain and Yellow River water) and the relative recoveries of spiked water samples are 99.9-115.4%, 101.8-113.7% and 87.3-117.6% at three different concentration levels of 75, 200 and 1000 microg L(-1), respectively.
使用 1-辛基-3-甲基咪唑六氟磷酸盐([C(8)MIM][PF(6)])离子液体作为萃取溶剂,采用分散液-液微萃取(DLLME)结合高效液相色谱(HPLC)测定水中的有机磷农药(OPPs)(对硫磷、辛硫磷、甲拌磷和毒死蜱)。萃取过程是通过形成浑浊溶液诱导的,该溶液由[C(8)MIM][PF(6)]的细小液滴在分散溶剂(甲醇)的帮助下完全分散到样品溶液中形成。考察并优化了萃取溶剂及其体积、分散溶剂及其体积、萃取时间、离心时间、加盐量、萃取温度和样品 pH 等参数。在优化条件下,分析物的富集因子高达 200 倍,萃取回收率(>70%)可接受。对硫磷、辛硫磷、甲拌磷和毒死蜱的浓度范围分别为 10.5-1045.0μg L(-1)、10.2-1020.0μg L(-1)、54.5-1089.0μg L(-1)和 27.2-1089.0μg L(-1)时,校准曲线均呈线性。以信噪比 3 计算,检出限在 0.1-5.0μg L(-1)范围内。200μg L(-1)浓度水平 7 次重复实验的相对标准偏差均小于 4.7%。该方法应用于四种不同来源水样(自来水、井水、雨水和黄河水)的分析,加标水样在 75、200 和 1000μg L(-1)三个不同浓度水平的回收率分别为 99.9-115.4%、101.8-113.7%和 87.3-117.6%。