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

介绍了一种配备超声分子束进样系统（HPLC/SMB/MS）的新型高效液相色谱质谱系统（HPLC/MS）。以烷基胺化合物为测试样品，考察了其性能特性。HPLC检测有机分子的HSI （Hyperthermal Surface Ionization）特点：在反相HPLC中，经常使用高极性溶剂，如水、甲醇、乙腈等作为流动相。它们与探测器的固体表面相互作用，影响探测器的响应特性。我们使用HPLC/HSI检测器检测了这些影响，没有对形成的离子进行质量分析。流动相和固体表面的测试组合为：(i)水/铱（Ir）， （ii）水/铂（Pt）， （iii）正己烷/铂，（iv）甲醇/铂。所得结果总结如下。(1)测试了流动相流量作为(i)信号响应、（ii）噪声水平和（iii）背景水平的函数。在mL/min的顺序流速下，溶剂与固体表面的相互作用更大，而μL/min的顺序流速对溶剂的HPLC/HSI性能影响不大。(2)水/Ir体系对烷基胺的灵敏度约为1.0C/g。(3)正丙胺的最小检出量为10pg /Ir数量级。(4)在烷基胺的作用下，水/Ir的动态范围在104左右。(5)水/Ir对正丙胺的敏感性是水/Pt的10倍。(6)其他溶剂/表面体系的响应特性与(1)~(4)近似相同。结果表明，高极性溶剂可作为HSI操作的高效液相色谱流动相。乙腈还没有测试过。HPLC/HSI/MS操作：在各种操作条件下，已完成仪器设置，并开始进行光谱测量。它们是(i)喷嘴温度，这与分子动能有关；（ii）固体表面温度；（iii） HPLC流速；（iv）溶剂性质。使用Ir和Pt作为固体表面，(a)信号响应，(b)噪声电平，(c)背景电平，(d)动态范围，现在正在进行检查，并将在其他地方报道。少

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