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DIRECT COUPLING OF CAPILLARY ELECTROPHORESIS AND MASS SPECTROMETRY FOR HIGH SENSITIVITY DETECTION OF LOW MOLECULAR MASS COMPOUNDS

毛细管电泳和质谱直接耦合用于低分子质量化合物的高灵敏度检测

基本信息

批准号：
07554040
负责人：
TERABE Shigeru
金额：
$ 10.56万
依托单位：
HIMEJI INSTITUTE OF TECHNOLOGY
依托单位国家：
日本
项目类别：
Grant-in-Aid for Scientific Research (A)
财政年份：
1995
资助国家：
日本
起止时间：
1995 至 1996
项目状态：
已结题

项目摘要

A Hitachi M-1000 quadrupole mass spectrometer equipped with atmospheric pressure chemical ionization (APCI) interface and electrospray ionization (ESI) interface was employed to develop a direct coupling method of capillary electrophoresis (CE) and mass spectrometry (MS). The APCI interface consisted of an electrospray nebulizer nozzle, a vaporizer and a chemical ionization chamber having a corona discharge electrode.1. The ESI interface was employed for the detection of closely related peptides, which were separated by CE using a nonionicsurfactant in an ammonium formate buffer (pH 3.0). The partialfilling technique where a part of the capillary was filled with amicellar solution was employed to prevent the surfactant from entering the interface. A mixture of water/methanol/formic acid (50 : 50 : 1) was employed as a sheath liquid of the ESI interface. Three neurotensin analogues different in one amino acid residue were successfully separated and detected by CE-ESI-MS and MS spectra of the peptides were successfully recorded.2. The optimum operating conditions of APCI-MS were explored using caffeine as a test sample. Effects of the flow rate of the sheath liquid (methanol), drift voltage, and vaporizer temperature on sensitivity were examined for the molecular ion of caffeine. The drift voltage affected significantly on sensitivity. Other factors were not very important. Addition of ionic surfactants to the caffeine solution did not deteriorate sensitivity.

采用配备常压化学电离（APCI）界面和电喷雾电离（ESI）界面的日立M-1000四极杆质谱仪，建立了毛细管电泳（CE）和质谱（MS）的直接耦合方法。APCI接口由一个电喷雾雾化器喷嘴、一个汽化器和一个具有电晕放电电极的化学电离室组成。在pH 3.0的甲酸铵缓冲液中，使用非离子表面活性剂，用CE分离出密切相关的肽。采用部分填充技术，在毛细管的一部分填充胶束溶液，以防止表面活性剂进入界面。采用水/甲醇/甲酸（50:50:1）的混合物作为ESI界面的鞘液。用CE-ESI-MS对不同氨基酸残基的3种神经紧张素类似物进行了分离和检测，并成功地记录了肽段的质谱。以咖啡因为试品，探讨了APCI-MS的最佳操作条件。考察了鞘液（甲醇）流速、漂移电压和汽化器温度对咖啡因分子离子灵敏度的影响。漂移电压对灵敏度有显著影响。其他因素不是很重要。在咖啡因溶液中加入离子表面活性剂不会降低灵敏度。