反乳化分散液液微萃取-HPLC测定水中二氯酚

Demulsified Dispersive Liquid-Liquid Microextraction Coupled with High Performance Liquid Chromatography for the Determination of 2,4-dichlorophenol and 2,6-dichlorophenol in Environmental Water Samples

建立了一种快速、简便、灵敏的反乳化分散液液微萃取新方法,并与高效液相色谱联用成功用于环境水样中2,4-二氯酚与2,6-二氯酚的测定。对萃取条件（如萃取剂、分散剂/反乳化剂的种类和体积、盐浓度、p H等）进行了优化,得到了最佳的反乳化分散液液微萃取条件。对2,4-二氯酚与2,6-二氯酚测定的线性范围分别为5~600μg/L（r=0.999 8）和5~600μg/L（r=0.999 7）,检出限（3σ）为2.06μg/L和2.88μg/L。对200μg/L的标准溶液测定得到的相对标准偏差（RSD）分别为1.71%和2.67%（n=6）。该方法已成功用于3种实际环境水样中痕量2,4-二氯酚与2,6-二氯酚的测定,加标回收率为83.2%~118.2%,RSD为0.56%~17.81%（n=3）。

A rapid, simple and sensitive method, the demulsified dispersive liquid-liquid microextraction was established, and coupled with high performance liquid chromatography, which was successfully used for the determination of 2,4- dichlorophenol（2,4-DCP） and 2,6-dichlorophenol （2,6-DCP） in environmental water samples. The extraction conditions such as the type and volume of extraction solvent and dispersive/demulsified solvent, salt concentration, pH and other factors were optimized, the best demulsified dispersive liquid-liquid microextraction conditions were found. Through the determination of 2,4-DCP and 2,6-DCP, the linear range of 2,4-DCP and 2,6-DCP were 5~600 μg/L（r=-0.999 8）and 5~600 μg/L（r=0.999 7） respectively. The limits of detection（LOD） （3δ） were 2.06 p.g/L and 2.88 μg/L. To determine the standard solution of 200μg/ L, the relative standard deviation （RSD） were 1.71% and 2.67%（n=6）respectively. The developed method was successfully applied to the determination of trace amount of 2,4-DCP and 2,6-DCP in three kinds of real environmental water samples, with the spiked recoveries in the range of 83.2%~118.2% and RSD of 0.56%~17.81% （n=3）.