JPH11295289A - Liquid chromatograph three-dimensional quadruple mass spectrometry - Google Patents

Abstract

PROBLEM TO BE SOLVED: To display each constituent peak of adjacent samples separately by obtaining the outflow time of the samples from the rising edges and falling edges of total ion chromatograms(TIC) or mass chromatograms, integrating their outflow areas, and performing TIC display with any span of time. SOLUTION: In a liquid chromatograph three-dimensional quadrupole mass spectroscopy, the separate display of adjacent samples A and B is performed through processes using, for example, the mass spectrum of each sample. The mass spectrum Sa at the peak top tpa of the sample A is obtained, and its TIC is integrated between the rising edge tsa and failing edge tea to store the result as TICa. An integration result TICb on the sample B is similarly obtained. By displaying the stored integration results TICa and TICb, it becomes possible to display an adjacent mixed sample separately. In addition, a method using the outflow time of each sample obtained from any mass chromatogram of the mass spectrum is performed.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an LC / 3DQ mass spectrometry used for analyzing organic substances and the like.

[0002]

2. Description of the Related Art Conventionally, in a method of ionizing a component (hereinafter, abbreviated as a compound) of an organic substance sample which separates and flows out of an LC, the sample flowing out of the LC is ionized, a TIC is displayed, and a TIC is displayed. Can be displayed. In addition, a mass spectrum can be displayed from the TIC and the mass spectrometer.

[0003]

The above prior art is based on LC
If the components separated by ionization and mass spectrometry are inadequate in the mass spectrometry method, no consideration is given to the fact that each component overlaps and is not separated and looks like a single component. There was no problem.

An object of the present invention is to determine the outflow time of each sample from the TIC of the mass spectrum and the rise and fall of the mass spectrometer and integrate the mass spectra of the outflow areas of the adjacent components and calculate the TIC in an arbitrary time width. The purpose of the display is to separate and display each component peak of an adjacent mixed sample, and to provide a mass spectrometric method that facilitates structural analysis.

[0005]

In order to achieve the above object, the outflow time of a sample is determined from the rise and fall of the TIC of LC / 3DQ mass spectrum or mass flow, and the outflow areas thereof are integrated to obtain an arbitrary width. It is indicated by. In addition, the mass flow rate of the sample having the same mass number is added to the outflow time of the sample and displayed as a TIC. Thus, adjacent mixed samples are separately displayed.

[0006]

Embodiments of the present invention will be described with reference to the drawings. FIG. 1 shows an LC according to an example to which the present invention is applied.
FIG. 1 is an overall configuration diagram of a / 3DQ mass spectrometer.

In FIG. 1, a mixed sample 1 to be measured is introduced into an LC 3 together with a mobile phase 2, separated through a column 4 for each component, flows out, and ionized at an interface 5. The generated ions 6 are mass-separated by a mass spectrometer 7 and enter an ion detector 8. The ion detector 8 sends the mass spectrum 9 sampled at an arbitrary time to the data processing device 10 and stores it. Mass spectrum 9 stored
To make TIC11. The outflow time of the sample is determined from the rise and fall of the peak displayed on the TIC 11, the mass spectrum 9 of the determined outflow area is integrated, and the display is performed as the TIC 12 in an arbitrary time width. Component peaks can be separated and displayed.

FIG. 2 shows the T of two samples flowing out of the LC.
It is an example showing an IC. At this time, the rise of the TIC is ts, the fall of the TIC is te, the peak top of sample A is tpa, and the peak top of sample B is tpb. First, the mass spectrum of the sample A is defined as Sa from tpa. When the TIC of Sa is At, and the rising and falling of At are tsa and tea, respectively, t
The time between sa and tea is integrated and the result is stored as TICa. Further, the mass spectrum of sample B is represented by Sb from tpb. When the TIC of Sb is Bt, and the rise and fall of Bt are tsb and teb, respectively, t
The time between sb and teb is integrated and the result is stored as TICb. By displaying the stored TICa and TICb, the TIC of the adjacent mixed sample can be separately displayed.

FIG. 3 is an example showing the TIC when the separation of two samples flowing out of the LC is insufficient. In this case, the outflow time of the sample is obtained from an arbitrary mass spectrum of the mass spectrum, and the TIC of the mixed sample is separated and displayed. First, the mass spectrum from ts to te of the TIC is integrated to obtain a mass spectrum, and Sa and S are added to the spectrum.
If there is b, the respective masks are obtained as Ma and Mb and stored in the data processing device. As shown in FIGS. 3 and 5, the outflow times of the samples A and B are obtained from these masses, and the rising time of Ma is tsa, the falling time is tea, the peak top time is tpa, and the rising time of Mb is tsb. When the fall time is represented by teb and the peak top time is represented by tpb, the time from tsa to tea is obtained.
During the period, a mass spectrum of an arbitrary mass range is integrated and sample A
Is stored in the data processing device as the TICa of the data.

Similarly, during the period from tsb to teb, mass spectra in an arbitrary mass range are integrated and stored in the data processing device as TICb of the sample B. By displaying the TICa and TICb stored in these data processing devices, the TIC of the adjacent mixed sample can be separately displayed.

FIG. 4 shows an example in which the sample has one or more mass spectra. First, the mass spectrum between ts and te is confirmed, and each mass spectrogram is stored in the data processing device. The outflow time of the sample is determined from the rise and fall of the stored mass spectrometer, and the mass flow obtained by adding the mass flow having the same mass flow time is stored in the data processing device. Thereafter, the TIC is displayed separately in the same procedure as in the example of FIG.

[0012]

According to the present invention, in the method of ionizing and analyzing components (compounds) of an organic substance sample separated from and flowing out of LC, mass separation can be performed to separate and display TICs in which the separation of each component is insufficient and overlapped. Therefore, there is an effect that the compound can be recognized on the TIC. In addition, recognition of the compound has the effect of facilitating structural analysis.

[Brief description of the drawings]

FIG. 1 is a diagram showing a schematic configuration of an LC / 3DQ of the present invention.

FIG. 2 is a spectrum intensity characteristic diagram showing TIC of two samples in FIG.

FIG. 3 shows a TI obtained when the separation of two samples is insufficient in FIG.
FIG. 4 is a spectrum intensity characteristic diagram showing C.

FIG. 4 is a spectrum intensity characteristic diagram when the sample of the present invention has one or more mass spectra.

FIG. 5 is a flowchart showing the flow of a data processing device according to an embodiment of the present invention.

[Explanation of symbols]

1: mixed sample, 2: mobile phase, 3: LC, 4: column, 5
... Interface, 6 ... Ion, 7 ... Mass analyzer, 8
... Ion detector.

Claims (4)

[Claims] A liquid chromatograph (Liquid Chromatogra)
In the method of ionizing and mass spectrometrically analyzing the components of a sample that separates and flows out of pH (hereinafter abbreviated as LC), the rise of a total ion chromatogram (hereinafter abbreviated as TIC) of the mass spectrum of the sample flowing out of the LC. LC / three-dimensional four-dimensional four-dimensional analysis, in which the outflow time of the sample is determined from the falling edge and the mass spectrum of the outflow area is integrated, the TIC display is executed at an arbitrary time width, and adjacent mixed samples are separated and displayed. Heavy pole (LC / 3Di
mensional Quadropole (hereinafter abbreviated as LC / 3DQ) mass spectrometry. 2. The method according to claim 1, wherein the TIC is displayed by calculating an outflow time of the sample from a rise and fall of an arbitrary mass chromatogram, integrating the outflow area of the mass chromatogram, and displaying an arbitrary time width. L characterized by
C / 3DQ mass spectrometry. 3. The LC / 3DQ mass spectrometric method according to claim 2, wherein only mass chromatograms having a mass number equal to the sample outflow time are added and displayed as a TIC. 4. The mass spectrometer according to claim 1, wherein the mass spectrometer is a mass spectrometer.