凝固-漂浮分散液液微萃取-高效液相色谱法测定水样中氯酚

Dispersive Liquid-Liquid Microextraction Based on Solidification of Floating Organic Drop Combined with High Performance Liquid Chromatography for Determination of Chlorophenols in Aqueous Samples

采用凝固-漂浮分散液液微萃取(SFO-DLLME)-高效液相色谱法测定水样中3种氯酚。以密度小于水,且凝固点为24℃的1-十二醇为萃取剂,甲醇为分散剂,对水样进行分散液液微萃取。将混合液离心,再通过冷冻凝固操作使漂浮的萃取剂和水相分离,萃取剂复溶后进样测定。本实验确定的最佳实验条件为:萃取剂200μL、分散剂300μL、1.2gNaCl、1mol/LH3PO4200μL、样品体积8.0mL、萃取时间3min。3种氯酚测定的线性范围为0.05～6.0mg/L;检出限为20～38μg/L。应用本方法分析实际水样,加标回收率在90.11%～107.7%之间;日间相对标准偏差在3.5%～4.6%之间。本方法扩展了分散液液微萃取萃取剂的选择范围,具有简便、快速、准确、环境友好等特点。

Using the method of dispersive liquid liquid microextraction based on solidification of floating organic （DLLME-SFO） combined with HPLC,three kinds of chlorophenols in aqueous samples were determined.The DLLME method with 1-dodecanol whose density was less than water and freezing point was 24 ℃ utilized as extractant and methanol as dispersive solvent was applied to analyze water samples.After the mixture was centrifugaled,the floated extractant that was solidified in ice bath was easily removed from water phase.When the solidified extractant droplet was redissolved,it was injected into the HPLC for analysis.The optimal experiment conditions were as follows：extractant solvent 200 μL,dispersive solvent 300 μL,NaCl 1.2 g,1 mol/L H3PO4 200 μL,sample volume 8.0 mL,extraction time 3 min.The calibration curve was linear in the range of 0.05-6.0 mg/L of the three kinds of chlorophenols,and the detection limits were 20-38 μg/L.This method has been applied to the determination of real water samples,the recovery of standard additions were from 90.11% to 107.7% and the inter-day RSDs were between 3.5% and 4.6% .The method extended the range of choosing the extractant in DLLME,it was proven to be simple,rapid,accurate and environment friendly.