疏水性低共熔溶剂超声辅助联合高效液相色谱萃取测定环境水样中3种酚类污染物

Determination of three phenolic pollutants in environmental water samples by high performance liquid chromatography coupled with ultrasonic-assisted extraction based on hydrophobic deep eutectic solvent

建立了一种利用疏水性低共熔溶剂(DES)超声辅助萃取联合高效液相色谱(HPLC)分离检测实际水样中痕量苯酚、间苯二酚和双酚A的方法。对影响萃取效率的因素(萃取剂种类、超声时间、萃取温度、DES体积、离心时间以及水样pH等)和萃取机理进行了讨论,在最优条件下,利用甲基三辛基氯化铵(N_(8881)Cl)∶甘油(摩尔比1∶2)为萃取剂,8 min内可以有效萃取水样中的苯酚、间苯二酚和双酚A,在线性范围内(0.25~25 mg/L)具有良好的线性关系(R2≥0.9997),检出限(LOD)和定量限(LOQ)分别为8.3~7.8μg/L和38.2~27.6μg/L。样品加标回收率为87.2%~104%,相对标准偏差(RSD)为1.3%~8.6%。该方法应用于实际环境水样中痕量的苯酚、间苯二酚和双酚A的检测,结果满意。

A new method for the determination of trace phenol,resorcinol and bisphenol A in water samples was developed by high performance liquid chromatography(HPLC)coupled with ultrasonic-assisted extraction based on hydrophobic deep eutectic solvent(DES).The factors affecting the extraction efficiency(extractant type,ultrasonic time,extraction temperature,DES volume,centrifugal time and pH of water sample)and the extraction mechanism were discussed.Under the optimal conditions,DES composed of methyl trioctylammonium chloride(N_(8881)Cl)and glycerol at 1∶2 molar ratio was used to extract phenol,resorcinol and bisphenol A in water samples in 8 min.The calibration curves were linear for the concentrations ranging between 0.25 and 25 mg/L with good linearity(R2≥0.9997)for all analytes.The limits of detection(LODs)and limits of quantification(LOQs)were in the range of 8.3-7.8μg/L and 38.2-27.6μg/L,respectively.The recoveries were in the range of 87.2%-104%with the relative standard deviations(RSDs)between 1.3%and 8.6%.The proposed method has been applied to the determination of trace phenol,resorcinol and bisphenol A in actual environmental water samples with satisfactory results.