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A New HPLC/MS System Equipped with a Supersonic Molecular Beam Sample Introduction System

配备超音速分子束进样系统的新型 HPLC/MS 系统

基本信息

批准号：
13640612
负责人：
KISHI Hiroshi
金额：
$ 2.24万
依托单位：
Oyama National College of Technology
依托单位国家：
日本
项目类别：
Grant-in-Aid for Scientific Research (C)
财政年份：
2001
资助国家：
日本
起止时间：
2001 至 2003
项目状态：
已结题

来源：
https://kaken.nii.ac.jp/grant/KAKENHI-PROJECT-13640612/
关键词：
High Performance Liquid Chromatography Mass Spectrometry Supersonic Molecular Beam Surface Ionization Reversed Phase HPLC Iridium Platinum Alkyl Amine 超音速分子加速電子衝撃

项目摘要

A new high performance liquid chromatography mass spectrometer system (HPLC/MS), equipped with a supersonic molecular beam sample introduction system (HPLC/SMB/MS) is described. Its performance characteristics are examined for alkyl amine compound as a test sample.1. Characteristics of HSI (Hyperthermal Surface Ionization) detection of organic molecules for HPLC :High polar solvents, such as water, methanol, and acetonitrile, are frequently used as mobile phase in reversed phase HPLC. They interact with solid surface of HSI detector, and affect its response characteristics. We examined these effects, using HPLC/HSI detector without mass analysis of formed ions. The tested combinations of mobile phase and solid surface are, (i) water/Iridium (Ir), (ii) water/Platinum (Pt), (iii) n-hexane/Pt, and (iv) methanol/Pt. The results obtained are summarized as below. (1) The mobile phase flow rate was tested as a function of, (i) signal response, (ii) noise level, and (iii) background level. A l … More arge interaction between solvent and solid surface was observed at mL/min order flow rate, whereas μL/min range had little effect to HPLC/HSI performance, for all of the solvents tested. (2) Sensitivity of around 1.0C/g was obtained for alkyl amine, using water/Ir system. (3) The minimum detectable amount of n-propylamine was the order of 10pg with water/Ir. (4) The dynamic range for water/Ir was around 104, with alkylamine. (5) The sensitivity for n-propylamine with water/Ir was 10 times greater than that with water/Pt. (6) Approximately the same response characteristics, as described in (1)〜(4), were obtained for the other solvent/surface system. It was concluded that high polar solvent can effectively be used as HPLC mobile phase for HSI operation. Acetonitrile has not been tested yet.2.HPLC/HSI/MS operation :The apparatus set up has been completed, and spectrum measurement has begun, under various operational conditions. They are (i) nozzle temperature, that is relevant to the molecular kinetic energy, (ii) solid surface temperature, (iii) HPLC flow rate, and (iv) the nature of the solvent. Using Ir and Pt as solid surface, (a) signal response, (b) noise level, and (c) background level, (d) dynamic range, are under examination now, and will be reported elsewhere. Less

介绍了一种新型高效液相色质联用系统，该系统配备了超声分子束进样系统(HPLC/SMB/MS)。以烷基胺类化合物为测试样品，考察了其性能特征。高效液相色谱中有机分子的高热表面电离检测特性：在反相高效液相色谱法中，经常使用水、甲醇和乙腈等高极性溶剂作为流动相。它们与HSI探测器的固体表面相互作用，影响其响应特性。我们在没有对形成的离子进行质量分析的情况下，使用高效液相色谱/高速离子检测器检测了这些影响。被测试的流动相和固体表面的组合是：(I)水/Ir(Ir)，(Ii)水/铂(Pt)，(Iii)正己烷/铂，和(Iv)甲醇/铂。所获得的结果总结如下。(1)流动相流速作为(I)信号响应、(Ii)噪声水平和(Iii)背景水平的函数进行测试。A L…在有序流量下，溶剂与固体表面有较强的相互作用，而μL/分钟对所考察的所有溶剂的性能影响不大。(2)在水/红外体系中，烷基胺的灵敏度约为1.0C/g。(3)正丙胺的最小检出量为10pg(水/红外)。(4)在烷基胺作用下，水/红外光谱的动态范围为104左右。(5)正丙胺对水/Ir的灵敏度比对水/铂的灵敏度大10倍。(6)对于另一种溶剂/表面体系，获得了与(1)~(4)中所描述的大致相同的响应特性。结论：高极性溶剂可以有效地作为HSI操作的高效液相色谱流动相。乙腈还没有进行测试。2.高效液相色谱/高分辨质谱联用操作：在各种操作条件下，仪器搭建完成，开始进行光谱测量。它们是：(I)喷嘴温度，与分子动能有关；(Ii)固体表面温度；(Iii)高效液相流速；(Iv)溶剂性质。使用Ir和Pt作为固体表面，(A)信号响应，(B)噪声水平，和(C)背景水平，(D)动态范围，目前正在研究中，并将在其他地方报告。较少