Surface desorption atmospheric chemical ionization source and method for analyzing surface desorption atmospheric chemical ionization mass spectrum

A chemical ionization source and chemical ionization technology, applied in the field of analytical chemistry, can solve problems such as low sensitivity, no atmospheric pressure chemical ionization source, heavy high-pressure cylinder nitrogen, etc., and achieve the effect of improving sensitivity

Active Publication Date: 2008-06-18
江西正谱奕和科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

With the deepening of research, people gradually realize that DESI also has some shortcomings, such as low sensitivity, and the need to use bulky high-pressure steel cylinders to provide a large flow rate of nitrogen, so powder samples cannot be directly analyzed, and there is no atmospheric pressure chemical ionization sour

Method used

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  • Surface desorption atmospheric chemical ionization source and method for analyzing surface desorption atmospheric chemical ionization mass spectrum
  • Surface desorption atmospheric chemical ionization source and method for analyzing surface desorption atmospheric chemical ionization mass spectrum
  • Surface desorption atmospheric chemical ionization source and method for analyzing surface desorption atmospheric chemical ionization mass spectrum

Examples

Experimental program
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Example Embodiment

[0081] Example 1: Determination of the active ingredient loratadine (Loratadine, FW 382) in Claritin(R) tablets in positive ion mode

[0082] The ion source of the present invention is connected to the LTQ mass spectrometer. During the experiment, the test sample Claritin(R) tablet is placed on the sample tray, and the angle between the ion source nozzle and the sample tray is adjusted to 45-80°, and the angle between the inlet capillary on the mass spectrometer and the sample tray is 5-10°. The distance between the nozzle and the inlet capillary of the mass spectrometer is 50mm. Adjust the parameters of the LTQ mass spectrometer. The chemical ionization reagent is water vapor (water content is 45-60%, nitrogen is used as carrier gas), the pressure is 20psi, and the discharge electrode is applied with a high pressure of 3-6KV. The sample is tested. The results are shown in Figure 5. Figure 5 shows that the active ingredient loratadine (FW382) in the tablet is very strong (1.16×10 ...

Example Embodiment

[0089] Example 2: Negative ion detection mode

[0090] SDAPCI can also work in negative ion mode, so that some components in the complex matrix can be converted into negative ions for mass spectrometry analysis. In the experiment, TNT (MW 227) was selected as the representative of the ionization source parameters in the table below, and the TNT (10pg / cm 2 ) Detection capability. Adjust the parameters during detection as follows:

[0091] Quality range

[0092] The results are shown in Figure 9, which shows that in the negative ion mode, the TNT MS spectrum clearly shows the negative ion peak m / z 226 after deprotonation, and a small amount of radical negative ions (m / z 227) are obtained. . The m / z 226 and 227 MS mass spectrometry results (see Figure 9A and Figure 9B) show that m / z 226 mainly loses NO to obtain fragments m / z 196, or directly loses NO2 to obtain fragments m / z 180. Among these fragment ions, the abundance of all ions is smaller than that of the parent ion (m...

Example Embodiment

[0093] Example 3: Analysis of free radical cations

[0094] In SDAPCI, since the operation is performed under normal pressure, operations such as replacement of reagents and addition of samples can be conveniently performed. Therefore, for different experimental purposes, reagents can be easily replaced to better detect the analytes in complex collective samples. The experiment shows that if the air is changed to argon, SDAPCI-MS detection can also be performed. When the argon does not contain active reagents such as water molecules, it can also obtain quite abundant free radical cations.

[0095]In the experiment, a sample of paracetamol was used to obtain the corresponding mass spectrum in an argon atmosphere (Figure 10). Acetylphenol is the main free radical cation (m / z 151). Since free radical cations have high energy, they are very active and can be quickly broken into smaller fragments. Therefore, in the MS spectrum, in addition to the base peak m / z 151, there are also many ...

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Abstract

The invention discloses a normal atmosphere chemical ionization source for surface desorption of a velocitron. A capillary and a spray point arranged in the capillary constitute a reagent ion generation system. When the reagent admitted through the capillary is sprayed out from one end of the capillary, the reagent is ionized to generate ions of the reagent due to the corona discharge of a discharge electrode; the reagent ions impact specimens inside a specimen disc to ionize the specimens, and the specimen ions are admitted into the velocitron inlet capillary to be used for detection. The ionization source disclosed by the invention is equipped with a moving interface, which can be connected with common velocitrons, such as LCQ, LTQ, TSQ and so on, so that the ionization source can be upgraded and become more powerful. The invention achieves quick and sensitive measurement of complicated basal body specimens by adopting the surface desorption atmospheric pressure chemical ionization mass-spectrometric technique under the condition that sample pretreatment is not required. In addition, the invention is applicable for real-time on-line non-destructive analysis in situ during industrial or environmental course. The ion source is joined with related velocitrons, and can achieve different detection modes, such as cation detection, anion detection, free radical ion detection and so on, according to the properties of specimens.

Description

technical field [0001] The invention relates to the field of analytical chemistry, in particular to an ion source of a mass spectrometer, specifically a surface desorption atmospheric pressure chemical ionization source and a technique for performing surface desorption atmospheric pressure chemical ionization mass spectrometry analysis using the ionization source. Background technique [0002] Mass spectrometry is a specialized science and technology widely used in various disciplines to identify compounds by preparing, separating, and detecting gas phase ions. Mass spectrometer is the basis of mass spectrometry research and application. A mass spectrometer generally includes a sample introduction system, an ion source, an ion optical system, a mass analyzer, a detector, a data acquisition and control system, a vacuum system, and the like. Internationally renowned mass spectrometry masters such as Professor R.Graham Cooks generally believe that the heart of a mass spectrome...

Claims

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Application Information

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IPC IPC(8): G01N27/64H01J49/10
Inventor 陈焕文张燮王志畅罗明标李建强
Owner 江西正谱奕和科技有限公司
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