析因设计DLLME-SFO同时萃取水中EDCs的应用

采用全析因设计对分散液液微萃取-上浮溶剂固化(DLLME-SFO)同时萃取水中五种环境内分泌干扰物包括雌酮(E1)、雌三醇(E3)、双酚A(BPA)、己烯雌酚(DES)和壬基酚(NP)的条件进行优化,建立了预测回归方程,并分析了因素对DLLME-SFO萃取回收率的影响。利用SAS软件分析得到的最优条件为盐浓度(m/v)15%、水样体积3 mL、分散剂(甲醇)体积0.5 mL以及萃取剂(十二醇)体积120μL。在优化萃取条件下,E1、E3、BPA、DES和NP萃取回收率的预测值分别为46.17%、74.38%、79.20%、69.62%和73.05%,实验验证值分别为44.15%、87.76%、77.83%、77.68%和70.01%,实验值与预测值的相对偏差小于10%。将建立的DLLME-SFO方法用于测定实际水样中的目标化合物,结果显示实际水样中E3、BPA、DES、E1和NP同时萃取回收率分别为64.81%~76.18%,88.09%~83.15%,68.38%~70.08%,66.37%~68.72%,68.35%~72.80%,相对标准偏差(n=3)在1.47%~8.09%之间。

Application of Factorial Design to Simultaneous Extraction of EDCs from Water Using DLLME-SFO

This paper refers to simultaneous extraction of endocrine disrupting chemicals including(EDCs),estriol(E3),bisphenol A(BPA),diethylstilbestrol(DES),estrone(E1) and nonylphnol(NP) from water sample using dispersive liquid-liquid micro-extraction based on solidification of floating organic drop(abbr.DLLME-SFO) and the factorial design which was used to optimize extraction process.Regression equations for predicting extraction recovery were established,the effects of factors on DLLME-SFO analyzed and then the optimum conditions obtained.Finally,DLLME-SFO was used to analyze EDCs in the tap water and it was concluded that the regression equations could predict the recovery of extraction of EDCs with a relative deviation range of 0.87%~8.28%.