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Method for correcting mass spectrometer and/or molecular weight

A molecular mass, mass spectrometry technology, applied in the fields of instruments, scientific instruments, measuring devices, etc., can solve the problems of unsuccessful, difficult preparation and use of gold clusters, and achieve peak accuracy, avoid drift, and improve accuracy.

Active Publication Date: 2014-03-19
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are few chemical substances that can meet this requirement. Gold clusters are just such a class of substances, and some people have tried them. However, due to the limitations of existing technologies, there are difficulties in preparing and using gold clusters, so they have not been successful.

Method used

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  • Method for correcting mass spectrometer and/or molecular weight
  • Method for correcting mass spectrometer and/or molecular weight
  • Method for correcting mass spectrometer and/or molecular weight

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0027] (1) Preparation of silica particles

[0028] It is prepared by the hydrolysis of ethyl orthosilicate catalyzed by ammonia water. The specific method is as follows: put the round bottom flask in a constant temperature water bath, stir it magnetically, and add a certain amount of absolute ethanol, a certain amount of ammonia water, and a certain amount of ultrapure water to it in sequence. , A certain amount of tetraethyl orthosilicate, and continue to react for more than ten hours at constant temperature and constant speed. After the reaction is completed, they are successively centrifuged and washed with triple distilled water and absolute ethanol, and finally the silica particles are stored in absolute ethanol for later use.

[0029] (2) Preparation of silica photonic crystal

[0030] Pour the ethanol dispersion of silicon dioxide particles with a certain volume fraction of 20% into a weighing bottle, insert a glass slide vertically into the dispersion, and prepare it...

Embodiment 1

[0031] Example 1. Utilizing bare gold film to generate positive gold cluster ions and performing external standard calibration on mass spectrometer

[0032] (1) Preparation of gold film

[0033] Take by weighing the gold of 87mg and the chromium of 3mg, by the method for vacuum evaporation, at first one layer of chromium is plated on the surface of silicon dioxide photonic crystal as bonding layer, then evaporate a layer of gold film (JEE-4X vacuum coating instrument), The thickness is 50nm.

[0034] (2) Generation of positive gold cluster ions and external standardization of mass spectrometer

[0035] Place the glass slide prepared with the gold film in the MALDI-TOF mass spectrometer, and bombard it with a pulsed laser at a frequency of 10 Hz, and the power of the bombardment is 90% of the maximum power; use the reflected positive ion mode to obtain the positive ion peak of the gold cluster mass spectrum, such as figure 1 shown.

[0036] Apply the gold cluster peaks gene...

Embodiment 2

[0037] Example 2, using the bare gold film to generate gold cluster positive ions to perform internal standard calibration on the sample

[0038] (1) Preparation of gold film

[0039] The preparation method is the same as step (1) in the examples.

[0040] (2) Using gold cluster positive ions to perform internal standard calibration on mass spectrograms

[0041] Drop 1 μL of the Gly-Gly-Gly-Gly solution on the gold film, and after drying, place the above-mentioned glass slide prepared with the gold film in a MALDI-TOF mass spectrometer, and bombard it with a pulsed laser at a frequency of 30 Hz. Bombarded at 80% of maximum power; analyzed in reflected positive ion mode; using Au 1 + (196.9660), Au 2 + (393.9326) as an internal standard for Gly-Gly-Gly-Gly([M+Na] + Accurate correction of the molecular weight of the exact molecular weight is 269.0856), the result is as image 3 As shown, the deviation of the average molecular weight reaches 3.3ppm after internal standard ...

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Abstract

The invention discloses a method for correcting a mass spectrometer and / or molecular weight, comprising the following steps: evaporating and plating gold films on a substrate, and bombarding the gold films by laser in the mass spectrometer; or after coating a matrix, a sample under test or the mixture of the matrix and the sample under test on the gold films, bombarding the gold film coated by the sample under test, the gold film coated by the matrix or the gold film coated by the mixture of the matrix and the sample under test by laser in the mass spectrometer, analyzing obtained ions by using the mass spectrometer to obtain a mass spectrogram, and correcting the mass spectrometer and / or the molecular weight of the sample under test according to the theoretical mass of the gold clusters. The method provided by the invention can be used for correcting positive and negative charges. Because the gold clusters without isotopes are used, a series of ion peaks with the mass-charge ratio difference of 197 can be recorded. Because the accurate theoretical mass of the gold is used, the signal of the mass spectrometer and the molecular weight of a sample can be correctly calibrated with deviation reduced to be below 5ppm.

Description

technical field [0001] The invention relates to a method of calibrating a mass spectrometer and / or molecular mass. Background technique [0002] Whenever mass spectrometry is used to determine the mass of a substance, the instrument needs to be calibrated. In order to obtain the accurate mass of the substance, after the instrument is calibrated, it is necessary to use the internal standard technology to compare the mass of the substance at any time to reduce the impact of the nonlinear response to the mass of the substance and the change of the ambient temperature in the mass spectrometry. It is known that small changes in the temperature of the mass spectrometer can lead to mass measurement deviations at the ppm level. So mass calibration is the core step in mass spectrometry. So far, standard chemical substances have been used for mass spectrometry calibration, and commonly used standard substances include polyvinyl alcohol (PEG), standard peptides, and CsI. Currently, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/64G01N1/28
Inventor 陈义李晋成马力坡
Owner INST OF CHEM CHINESE ACAD OF SCI
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