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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

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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 source It has selectivity, and like ESI and APCI, it needs to use harmful reagents (such as methanol) to generate reagent ions to spray onto the sample surface, which will contaminate the tested product during real-time detection, making it difficult to use in related fields such as medicine and food. get practical application

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
Comparison scheme
Effect test

example 1

[0081] Example 1: Determination of active ingredient Loratadine (Loratadine, FW 382) in Claritin® tablet under positive ion mode

[0082] The ion source of the present invention was coupled to the LTQ mass spectrometer. During the experiment, the detection sample Claritin(R) tablet is placed on the sample disk, the angle between the ion source nozzle and the sample disk is adjusted to be 45-80°, and the angle between the inlet capillary on the mass spectrometer and the sample disk is 5-10°. The distance from the nozzle to the inlet capillary of the mass spectrometer is 50 mm, and the parameters of the LTQ mass spectrometer are adjusted well. 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 added with a high voltage of 3-6KV to detect the sample. The results are shown in Figure 5. Figure 5 shows that the active ingredient loratadine (FW382) in the tablet is very stro...

example 2

[0089] Example 2. Negative ion detection mode

[0090] SDAPCI can also work in the negative ion mode, so that some components in the complex matrix can be transformed into negative ions for mass spectrometry analysis. During 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: in the negative ion mode, the spectrum of TNT primary mass spectrometry clearly shows the negative ion peak m / z 226 after deprotonation, and a small amount of free radical negative ion (m / z 227) is obtained at the same time . The MS / MS results of m / z226 and 227 (see Figure 9A and Figure 9B) show that m / z 226 mainly loses NO to obtain fragment m / z 196, and can also directly lose NO2 to obtain fragment m / z 180. Among these fragment ions, all ions are l...

example 3

[0093] Example 3. Analysis of free radical cations

[0094] In SDAPCI, operations such as replacement of reagents and addition of samples can be easily performed due to the operation under normal pressure. Therefore, for different experimental purposes, the reagents can be easily replaced, so as to better detect the analyte in complex collective samples. Experiments show that if the air is replaced by argon, SDAPCI-MS detection can also be performed. When argon does not contain active reagents such as water molecules, a considerable abundance of free radical cations can also be obtained.

[0095]In the experiment, a paracetamol sample was used to obtain a corresponding mass spectrum in an argon atmosphere (as shown in FIG. 10 ). Paracetamol is the predominant free radical cation (m / z 151). Due to their high energy, free radical cations are very active and can be rapidly broken down into smaller fragments. Therefore, in the MS spectrum, in addition to the base peak m / z 151,...

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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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