乙醇-K_(2)HPO_(4)-H_(2)O双水相萃取体系结合GC-MS检测白酒中的邻苯二甲酸酯  

Determination of phthalates in white spirit through ethanol-K_(2)HPO_(4)-water aqueous two-phase extraction combined with GC-MS

作　　者：王湘敏[1] 李婧闻 邬旭然[1] 刘永明[1] WANG Xiang-min;LI Jing-wen;WU Xu-ran;LIU Yong-ming(School of Chemistry and Chemical Engineering,Yantai University,Yantai 264005,China)

机构地区：[1]烟台大学化学化工学院,山东烟台264005

出　　处：《化学研究与应用》2021年第2期352-357,共6页Chemical Research and Application

基　　金：国家自然科学基金项目(21575122)资助。

摘　　要：本文直接以白酒中的乙醇为萃取剂,通过双水相萃取技术结合气相色谱质谱联用法,建立了一种测定白酒中邻苯二甲酸酯类化合物的方法。实验对双水相体系的形成条件进行了研究,并探讨了双水相体系对邻苯二甲酸酯类的萃取效率。实验结果表明:乙醇-磷酸氢二钾-水双水相体系对邻苯二甲酸酯类物质有较高的萃取效率,在上相萃取液中加入无水MgSO_(4)去除水分后,可直接进行GC-MS检测。该方法操作简便,无需使用其他有机溶剂,有效避免了样品处理过程中邻苯二甲酸酯的污染。用于白酒中16种邻苯二甲酸酯类物质的测定,回收率为80.3%~98.0%,相对标准偏差为0.5%~8.5%,检出限为0.01~0.31 mg·kg^(-1)。A new method for the determination of phthalate esters in white spirit was established by using ethanol as extractant with ethanol-K_(2)HPO_(4)-water aqueous two-phase system.The formation conditions of aqueous two-phase system were studied,and the extraction efficiency of phthalates by aqueous two-phase system was discussed.The results showed that the phthalate esters were extracted with high efficiency in salting-out system which formed by ethanol-K_(2)HPO_(4)-water of two-phase system.After the anhydrous magnesium sulfate(MgSO_(4))was added to eliminate the moisture in upper phase of the two-phase system,the upper phase was directly used for analyzed with gas chromatography-mass spectrometry.This method is easy to operate and does not need to use other organic solvents.It can effectively avoid the pollution of phthalate in the process of sample treatment.The method was applied in the determination of phthalate esters in white spirit.The spiked recoveries and the relative standard deviation values were 80.3%~98.0%and 0.5%~8.5%,respectively.The detection limits were in the range of 0.01~0.31 mg·kg^(-1).

关 键 词：邻苯二甲酸酯 双水相 气相色谱质谱联用 白酒 

分 类 号：O657.7[理学—分析化学]