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Mass spectrum correction method for generating a series of standard metal cluster ions in site

A technology of metal clusters and correction methods, applied in the field of detection and analysis, can solve problems such as instability, lack of accurate correction methods, and small response of secondary fragment ion signals, and achieve high reproducibility

Inactive Publication Date: 2020-04-28
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The existing calibration technology lacks an accurate calibration method for the system. Although conventional laser dissociation substances such as peptides and proteins can generate abundant fragment ions, the overall dissociation efficiency is low, and the signal response of secondary fragment ions is small and insignificant. Stable and cannot be used for calibration of laser dissociation techniques

Method used

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  • Mass spectrum correction method for generating a series of standard metal cluster ions in site
  • Mass spectrum correction method for generating a series of standard metal cluster ions in site
  • Mass spectrum correction method for generating a series of standard metal cluster ions in site

Examples

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Effect test

Embodiment 1

[0034] Based on Au 25(SC 8 h 9 ) 5 (PC 18 h 15 ) 10 Cl 2 mass spectrometer calibration

[0035] The inventive method such as Figure 5 As shown, Au was prepared by liquid-phase synthesis method 25 (SC 8 h 9 ) 5 (PC 18 h 15 ) 10 Cl 2 , using electrospray ionization to introduce it into the mass spectrometer, based on its theoretical molecular weight, a single-point calibration of the mass spectrometer can be achieved ( figure 1 A). Based on its fragment ion composition distribution and signal intensity generated in the secondary dissociation mode, the correction of the secondary dissociation mode is realized ( figure 1 B). Under the irradiation of 100nm laser and 50μJ / pulse, a series of atomically continuous secondary fragment ions are generated, which can realize the mass calibration and resolution calibration of the mass spectrometer at multiple points ( figure 1 C), the calibration range is 190~5000m / z.

Embodiment 2

[0037] Based on Au 13 Ag 12 (PC 18 h 15 ) 10 Cl 7 UV laser-mass spectrometer calibration

[0038] Preparation of Au by Liquid Phase Synthesis 13 Ag 12 (PC 18 h 15 ) 10 Cl 7 , introduced into the mass spectrometer using electrospray ionization, based on its theoretical molecular weight a single-point calibration of the mass spectrometer can be tested ( figure 2 A). Based on its fragment ion composition distribution and signal intensity generated in the secondary dissociation mode, the correction of the secondary dissociation mode is realized ( figure 2 B). Under the irradiation of 214nm laser and 2mJ / pulse, a series of continuous secondary fragment ions are produced, which can realize the mass calibration and resolution calibration of the mass spectrometer at multiple points ( figure 2 C and D), the calibration range is 190~4000m / z.

[0039] Based on the difference of fragment ions of metal clusters under different laser energies, the photodissociation efficie...

Embodiment 3

[0041] Based on Au 144 (SC 8 h 9 ) 144 mass spectrometer calibration

[0042] Preparation of Au by Liquid Phase Synthesis 144 (SC 8 h 9 ) 144 , using electrospray ionization to introduce it into the mass spectrometer, based on the irradiation of 193nm laser and 10mJ / pulse, it can generate a series of continuous secondary fragment ions composed of atoms, which can realize the mass calibration and resolution of multiple sites of the mass spectrometer rate correction ( Figure 4 ), the correction range is 1000~15000m / z.

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Abstract

The invention provides a mass spectrum correction method for generating a series of standard metal cluster ions in situ, and belongs to the technical field of detection and analysis. According to themethod, ligand-protected metal cluster molecules are ionized through electrospray ionization and then introduced into a mass spectrometry system; laser is introduced into a mass spectrum dissociationtrap to carry out protective group stripping and core metal cluster dissociation on a metal cluster, a series of standard metal cluster ions are generated in situ, and the detection quality precision,resolution, sensitivity and laser dissociation efficiency of a laser-mass spectrum system are corrected based on the generated series of metal cluster ions with continuous mass distribution. The method has the characteristics of being rapid, simple, efficient, stable, high in repeatability, wide in quality correction range, high in correction standard coverage rate and the like, and an effectiveguarantee technology is provided for the comprehensive correction of laser-mass spectrometry system performance.

Description

technical field [0001] The invention belongs to the technical field of detection and analysis, and in particular relates to a mass spectrum correction method for generating a series of standard metal cluster ions in situ. Background technique [0002] Mass spectrometer is an important analytical instrument based on detecting ion charge-mass ratio to confirm molecular composition and structure. It is widely used in environmental testing, medical testing, drug testing and quality control. With the development of macromolecular mass spectrometry detection technology in recent years, mass spectrometers have played a vital role in the characterization and detection of macromolecules such as antibodies, protein complexes, and protein-small molecule complexes. However, due to the large molecular weight of such macromolecules, a mass spectrometer with a high detection range is usually required for detection and characterization. Taking a common antibody as an example, it consists o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/62
CPCG01N27/62G01N27/628
Inventor 王方军刘哲益
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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