涡旋辅助分散液液微萃取-悬浮固化/高效液相色谱法测定水样中7种萘二酚

Rapid Determination of Seven Naphthalenediols with Vortex-assisted Dispersive Liquid-Liquid Microextraction Based on Solidification of Floating Organic Drop and High Performance Liquid Chromatography

建立了水样中7种萘二酚的涡旋辅助分散液液微萃取-悬浮固化/高效液相色谱（VA-DLLMESFO/HPLC）测定方法。以乙醚-十二醇为二元微萃取剂,通过涡旋分散方式协同萃取水样中的目标化合物,采用C18色谱柱分离,HPLC测定。优化了萃取剂及用量、萃取时间、氯化钠用量等条件。最佳萃取条件为：萃取剂为100μL乙醚和50μL十二醇,氯化钠用量为0.2 g/mL,涡旋萃取3 min。在优化条件下,7种萘二酚在一定质量浓度范围内线性关系良好,相关系数均大于0.997,方法检出限（S/N=3）为1.7-6.0μg/L;3个加标水平下的平均回收率为82.1%-106.0%,日内相对标准偏差（RSD,n=5）为1.2%-4.1%;中间添加水平的日间RSD（n=5）为2.5%-5.7%。该方法前处理简单,涡旋分散大大提高了物质传质速率,增大了萃取效率,缩短了萃取时间,是一种适用于水样中萘二酚类物质富集检测的绿色方法。

A simple and rapid method for the preconcentration and determination of seven naphtha- lenediols in water samples with vortex-assisted dispersive liquid - liquid microextraetion based on solidification of floating organic drop （ VA - DLLME - SFO） and high performance liquid chromatography （HPLC） was established. The target compounds in water samples were synergistically extracted in vortex dispersed mode, with ethyl ether - dodecanol as binary micro-extraction agent, then separated on a C18 chromatographic column and determined by HPLC. The kind and dosage of extraction agent, extraction time, dosage of sodium chloride and other conditions were optimized. The optimum extraction conditions were as follows： extraction agent： 100 μL ethyl ether- 50 μL dodecanol, amount of sodium chloride ： 0. 2 g/mL, vortex extraction time ： 3 min. Under the optimized conditions, the calibration curves of 7 naphthalenediols were linear in the certain concentration range with correlation coefficients greater than 0. 997. The detection limits of the method （ SIN = 3 ） were between 1.7 μg/L and 6. 0μg/L. The average recoveries of naphthalenediols at three spiked levels in water sample ranged from 82. 1% to 106. 0% with relative standard deviations（ RSD, n = 5 ） of 1.2% -4. 1%.The inter-RSDs（n =5） ranged from 2. 5% to 5.7% at the middle spiked level. The developed method was simple and environment-friendly, and the vortex-assisted dispersion could largely enhance the mass transfer rate and shorten the required extraction time. Therefore, the method was suitable for the detection of naphthalenediols in water samples.