JPH01140547A - Liquid chromatograph mass analysis device - Google Patents

Abstract

PURPOSE:To make it unnecessary to lead a sample solution mixing glycerin, and to extend the durable period of a chromatocolumn, by providing a mixer to mix a matrix into a leading pipe of developing solution from a liquid chromatograph, and an auxiliary column between the mixer and an ionization chamber of a mass analysis device. CONSTITUTION:A sample solution to analyze developed by a liquid chromatograph 5 is delivered to a mixer 10 through a pipe 6, a matrix responding to the flow of the sample solution is led from a feeding source 12 and mixed. The development condition of the sample solution disturbed in the mixing is corrected through an auxiliary column 11 to unify the mixing condition. The solution is led to an ionization chamber 2, oozed out to the surface through a porous target 7, given a shock by corpuscular beams B from a corpuscular beam generator 4 to ionize, and led to the mass analysis position through a slit electrode 3. In such a composition, the sample solution mixing glycerin is not necessary to use, the disturbance to the liquid chromatograph mass analysis is eliminated, the contamination of the chromatocolumn is prevented, and the durable period is extended.

Description

Detailed Description of the Invention [Industrial Application Field] The present invention relates to an apparatus for directly introducing a liquid sample separated by a liquid chromatograph into the ionization chamber of a mass spectrometer online, and particularly to The present invention relates to a sample introduction device suitable for use in an ionization device.

[Prior Art] As an ion source in which a sample liquid separated by a liquid chromatograph is directly introduced into a quality analyzer, one having a structure as shown in FIG. 2, for example, is known.

In FIG. 2, 1 is the ion source of the quality m analyzer, 2 is the ionization chamber, 3 is the slit electrode that accelerates and focuses the ions generated in the ionization chamber, 4 is the primary particle beam generator,
5 is a liquid chromatograph, 6 is an introduction tube for introducing the sample liquid separated by the liquid chromatograph 5 into the ionization chamber 2, 7 is a porous member target, and 8 is a connection between the introduction tube and the porous member target. The guide tube 9, which is placed over the tip of the introduction tube, is a heater.

In such a configuration, the sample liquid separated by the liquid chromatograph 5 is sequentially introduced into the ionization chamber 2 through the ionization tube 6 having the porous member 7 attached to the tip thereof, and It passes through the porous member target 7 and oozes out to the surface. Here, in the porous member target 7, the solvent component with a low boiling point is preferentially vaporized, and the sample component with a high boiling point is vaporized relatively slowly.

As a result, the concentration of sample components on the target surface increases relatively. Then, the sample liquid seeped onto the target surface is exposed to the impact of the primary particle beam B from the primary particle beam generator 4 (
ionized by high-velocity particle beam bombardment). The generated ions are introduced into a mass spectrometry field via the slit electrode 3 and subjected to mass spectrometry.

[Problem to be Solved by the Invention 7] In the so-called liquid chromatograph analysis device having the above-mentioned configuration, a non-volatile substance such as glycerin is mixed in advance as a matrix in the mobile phase used in the liquid chromatograph. has been done. Therefore, even if a sample solution mixed with glycerin is introduced into the ionization chamber with a high degree of vacuum, the glycerin, which is a highly viscous and low vapor pressure substance, surrounds the sample solution, and the sample solution that has oozed out onto the target surface becomes a high-speed particle. It is possible to prevent volatilization before receiving a radiation bombardment, and as a result, the produced ionology can be increased.

However, if a highly viscous matrix such as glycerin is mixed in advance, the matrix impairs the separation conditions of liquid chromatography, causing problems in chromatographic analysis. In addition, the contamination of the matrix makes the chromatocolumn more likely to become dirty, which poses a problem of shortening the service life of the chromatocolumn.

SUMMARY OF THE INVENTION An object of the present invention is to provide a sample testing device that overcomes the above-mentioned problems by mixing a matrix into the developing solution from a liquid chromatograph.

[Means for Solving the Problems] The present invention includes an ionization chamber, an introduction tube for introducing a sample liquid from a liquid chromatograph into the ionization chamber, and a primary particle beam directed toward the sample introduced into the ionization chamber. In an apparatus that is equipped with a primary particle beam generation source that irradiates the sample and ionizes the sample by the impact of the primary particle beam, a matrix is mixed into the introduction tube into which the developing solution from the liquid chromatograph is sent out. The present invention is characterized in that a mixer is provided and an auxiliary column is provided between the mixer and the ionization chamber of the pawnshop analyzer.

[Function] The liquid chromatograph mass spectrometer of the present invention is provided with a mixer for mixing a matrix into the introduction tube through which the developing solution from the liquid chromatograph is sent out, and the liquid chromatograph mass spectrometer
・In addition to mixing the matrix into the developing solution from the graph, an auxiliary column is installed between the mixer and the ionization chamber of the 11 analyzer δ, and the developed state of the sample solution mixed with the matrix is shaped in the auxiliary column. It is introduced into the ionization chamber.

[Example] Hereinafter, an example of the present invention will be described based on the drawings. 1st
The figure is a PJM4 diagram for explaining one embodiment of the present invention. In FIG. 1, the same components as in FIG. 2 are given the same numbers.

The embodiment shown in FIG. 1 is different from the conventional example in that a mixer 10 for mixing the matrix is provided in the introduction tube 6 through which the developing solution from the liquid chromatograph 5 is delivered.
A matrix is introduced from a matrix supply source 12 into the liquid chromatograph 5 to mix the matrix into the developing solution from the liquid chromatograph 5, and an auxiliary column 11 is inserted into the introduction pipe between the mixer 10 and the ionization chamber 2 of the interrogation analyzer. The point is that the sample liquid mixed with the matrix is introduced into the ionization column 2 through the auxiliary column 11.

The sample solution to be analyzed spread out in the liquid chromatograph 5 is sent to the mixer 10 through the introduction pipe 6. The mixer 10 is supplied with a matrix corresponding to the flow rate of the sample liquid from the matrix supply 112, and the sample liquid developed in the mixer and the matrix are mixed. Then, the sample liquid mixed with the matrix is introduced into the auxiliary column 11, and the spread state of the sample liquid that is disturbed when mixing the sample liquid with 71~ in the mixer 10 is adjusted, and the matrix and the sample liquid are to make the mixing state uniform. The sample liquid sent out from the auxiliary column 11 is sequentially introduced into the introduction tube ionization chamber, passes through the porous member target 7 attached to the tip of the introduction tube, and oozes out to the surface.

The sample liquid exuded onto the target surface is ionized by the impact (high-speed particle beam impact) of the primary particle beam B from the primary particle beam generator 4. The generated ions are introduced into the quality φ analysis field via the slit electrode 3 and subjected to total quality analysis.

Effects of the Invention] As is clear from the above description, the present invention provides a mixer for mixing a matrix into an introduction tube through which a developing solution from a liquid chromatograph is sent out, and a mixer for mixing a matrix in the mixer. In addition to mixing the matrix into the developing solution obtained from the graph, an auxiliary column is provided between the mixer and the ionization chamber of the mass spectrometer, and the auxiliary column corrects the state of development of the sample liquid that is disturbed by the mixing of the matrix. It is introduced into the ionization chamber.

Therefore, there is no need to introduce a sample solution mixed with a matrix such as glycerin into the liquid chromatograph in advance, and there is no need to introduce the sample solution into the liquid chromatograph and spread it. It disappears.

Furthermore, since the chromatographic column is not contaminated by the matrix, the service life of the chromatographic column is not shortened.

[Brief explanation of the drawing]

FIG. 1 is an apparatus configuration diagram for explaining one embodiment of the present invention, and FIG. 2 is a diagram for explaining a conventional example. 1: Ion source 2: Ionization chamber 3 Nislit electrode 4 Primary particle beam generator 5: Liquid chromatograph 6: Introducing tube 7: Porous member target 10: Mixer 11: Auxiliary column 12: Matrix supply source

Claims (1)

[Claims] An ionization chamber, an introduction tube for introducing a sample liquid from a liquid chromatograph into the ionization chamber, and a primary particle beam generation source for irradiating a primary particle beam toward the sample introduced into the ionization chamber, In an apparatus configured to ionize a sample by impact with a particle beam, a mixer for mixing a matrix is provided in an introduction tube through which a developing solution from the liquid chromatograph is sent, and the mixer and an ionization chamber of a mass spectrometer are connected. A liquid chromatograph mass spectrometer characterized in that an auxiliary column is provided between the two.