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).

已经开发了一种简单有效的浓度方法，用于微体积的溶剂。提取溶剂后，将一滴高沸点溶剂添加到分离的有机相中，并通过蒸发去除具有低沸点的溶剂。因此，分析物将集中在剩余的高沸点溶剂中。所提出的方法已成功地应用于钴离子（II）离子的浓度，富集因子为1000，并引入离子-PAIR反向相位的HPLC。在没有大量溶解的情况下，需要从分析中获得过量的试剂。 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）添加并通过蒸发将分析物浓缩在残留DMSO中的分析物中去除低的沸点溶剂，氯仿。当使用DMSO的100 cm^3和0.1 cm^3的起始样品体积时，检测极限达到3*10^<-11> mol dm^<-3>（1.8 ppt）。