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Development of "One drop solvent concentration method"for Highly Sensitive Micro Analysis

开发用于高灵敏度微量分析的“一滴溶剂浓缩法”

基本信息

批准号：
05453113
负责人：
YOTSUYANAGI Takao
金额：
$ 4.22万
依托单位：
Tohoku University
依托单位国家：
日本
项目类别：
Grant-in-Aid for General Scientific Research (B)
财政年份：
1993
资助国家：
日本
起止时间：
1993 至 1994
项目状态：
已结题

来源：
https://kaken.nii.ac.jp/en/grant/KAKENHI-PROJECT-05453113/
关键词：
one drop concentration HPLC cobalt solvent extraction ion-pair HPLC 2,2'-ジヒドロキシアゾベンゼン

项目摘要

A simple and effective concentration method into micro volume of solvent has been developed. After solvent extraction, one drop of high boiling-point solvent is added to the separated organic phase, and the extracting solvent with low boiling-point is removed by evapolation. Thus, the analyte is concentrated into the residual micro volume of high boiling-point solvent.The proposed method has been successfully applied to the concentration of cobalt (II) ion with the enrichment factor of 1000 and introduced to ion-pair reversed-phase HPLC.Separtion of excess reagent from the analyte is required to obtain the large enrichment factor without precipi-tation in the final water-miscible solvent. The cobalt (III)-2,2'-dihydroxyazobenzene (DHAB,H_2L) complex, [CoL_2]^-, is extracted into chloroform as the ion-pair with tetrabutylammonium ion following removal of excess DHAB by extraction of its neutral species, H_2L.To the separated organic phasemicro volume of dimethylsulfoxide (DMSO,boiling point : 189 C) is added and the low boiling-point solvent, chloroform, is removed by evaporation to concentrate the analyte in the residual DMSO.The undesired depressiveeffect of the organic solvent on HPLC peak profiles was eliminated by using a suitable injection solution of 1 : 1 DMSO-water. When the startingaqueous sample volume of 100 cm^3 and 0.1 cm^3 of DMSO were used, the detection limit reached 3*10^<-11> mol dm^<-3> (1.8 ppt).

提出了一种简单有效的微量溶剂浓缩方法。在溶剂萃取后，向分离的有机相中加入一滴高沸点溶剂，并通过蒸馏除去低沸点的萃取溶剂。该方法已成功地应用于钴离子的富集，富集倍数为1000，并被引入到反相离子对高效液相色谱中，为了获得大的富集倍数，需要分离过量的试剂和分析物，而在最终的水溶性溶剂中不沉淀。钴（III）-2，2 '-二羟基偶氮苯（DHAB，H_2L）络合物[CoL_2]^-与四丁基铵离子形成离子对，用氯仿萃取，然后用其中性物H_2L萃取除去过量的DHAB（DMSO，沸点：189 ℃）并加入低沸点溶剂，氯仿，通过蒸发除去有机溶剂，使待测物浓缩在残留的DMSO中，消除了有机溶剂对HPLC峰形的不利影响通过使用1：1 DMSO-水的合适的注射溶液。当起始水溶液体积为100 cm ^3，DMSO为0.1 cm ^3时，检测限可达3 × 10 ~（-1）<-11>mol dm^<-3>（1.8 ppt）。