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Application of naphthylhydrazine inorganic acid salt or Naphthylhydrazine organic acid salt as matrix in MALDI MS (matrix-assisted laser desorption/ionization mass spectrometry)

A technology of matrix-assisted laser and inorganic acid salts, which is applied in the field of mass spectrometry detection, can solve the problems of long time consumption, reduced analysis effect, and poor reusable effect, and achieve the effect of good sample compatibility and reduced requirements

Active Publication Date: 2013-04-24
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When desorption / ionization occurs on the porous silicon surface, the surface of the silicon crystal must first be etched to produce a nanostructured surface. Although peptides and antiviral drugs can be directly analyzed on such a surface, the repeated use of this surface is not effective. OK, so repeated treatments on the same nanostructured surface are required to get a reusable surface
In addition, it takes a long time to chemically modify the surface of porous silicon, and the analysis effect will be greatly reduced when the modified porous silicon is reused.

Method used

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  • Application of naphthylhydrazine inorganic acid salt or Naphthylhydrazine organic acid salt as matrix in MALDI MS (matrix-assisted laser desorption/ionization mass spectrometry)
  • Application of naphthylhydrazine inorganic acid salt or Naphthylhydrazine organic acid salt as matrix in MALDI MS (matrix-assisted laser desorption/ionization mass spectrometry)
  • Application of naphthylhydrazine inorganic acid salt or Naphthylhydrazine organic acid salt as matrix in MALDI MS (matrix-assisted laser desorption/ionization mass spectrometry)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Embodiment 1, the analysis of oligosaccharides

[0034] Take various prepared sample solutions and matrix solutions and mix them uniformly at a volume ratio of 1:1 (the molar ratios of 1-naphthylhydrazine hydrochloride to glucose, sucrose, maltose, and maltoheptaose are 5:1, 5:1, and 1.5: 1 and 1.5:1), then add 1 μL of the mixed sample on the MALDI target plate, dry in the air and enter the mass spectrometry analysis.

[0035] Among them, glucose, sucrose, maltose and maltoheptaose were all dissolved in pure water, the concentrations were 3mmol / L, 3mmol / L, 10mmol / L and 10mmol / L in turn, and the matrix 1-naphthylhydrazine hydrochloride was dissolved in the volume ratio of 1:1 Prepare a 3 mg / mL solution in acetonitrile / water solution.

[0036]The mass spectrometry conditions are: voltage: accelerating voltage: 19.000kV; delayed extraction voltage: 14.920kV; reflector voltage: 20.000kV; lens voltage: 7.000kV; frequency: 1.000Hz; laser energy: 75~80%; accumulation times: 8...

Embodiment 2

[0038] Embodiment 2, analysis of glucose content in serum

[0039] Mix 10 μL human serum with 30 μL acetonitrile, mix well, centrifuge, take 10 μL supernatant and mix with 10 μL matrix 1-naphthylhydrazine hydrochloride solution, and finally take 1 μL of the mixed solution and add it to the MALDI target plate, dry it in the air and enter the mass spectrometry analysis .

[0040] When using the standard addition method to quantitatively detect the glucose concentration, prepare isotope-labeled D-glucose-1,2- 13 C 2 aqueous solution, and glucose aqueous solutions with molar concentrations of 0, 1, 2, 3, 5 and 9 mmol / L respectively. Take the prepared deproteinized serum supernatant and mix it with 3 mg / mL matrix aqueous solution, isotope-labeled glucose aqueous solution and glucose solutions of different concentrations at a volume ratio of 1:1:1:1, and take 1 μL of the mixed solution for MALDI-TOF mass spectrometry analyze.

[0041] The mass spectrometry conditions are: voltag...

Embodiment 3

[0044] Example 3, Analysis of Homogentisic Acid Content in Urine

[0045] Take fresh urine to prepare 5 mg / mL homogentisic acid solution, take out 1 μL of the mixed solution and add it to the MALDI target plate, dry it in the air, and then enter the mass spectrometry analysis.

[0046] When drawing a standard curve to quantitatively detect homogentisic acid in urine of known concentration, prepare isotope-labeled homogentisic acid with a molar concentration of 3 mg / mL- 13 C 6 The urine sample solution was mixed with the urine sample solution of 0, 1, 2, 3, 4 and 5 mg / mL of molar concentration respectively and 3 mg / mL matrix aqueous solution in equal volumes (wherein 1-naphthylhydrazine hydrochloride The molar ratio to homogentisic acid is about 3:5), take 1 μL of the mixed solution for MALDI-TOF mass spectrometry analysis.

[0047] The mass spectrometry conditions are: voltage: accelerating voltage: 19.000kV; delayed extraction voltage: 14.920kV; reflector voltage: 20.000kV;...

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Abstract

The invention discloses application of naphthylhydrazine inorganic acid salt or naphthylhydrazine organic acid salt as a matrix in MALDI MS (matrix-assisted laser desorption / ionization mass spectrometry). The MALDI MS is MALDI-TOF MS (matrix-assisted laser desorption / ionization - time-of-flight mass spectrometry); the naphthylhydrazine inorganic acid salt is naphthylhydrazine hydrochloride, naphthylhydrazine nitrate, naphthylhydrazine phosphate or naphthylhydrazine sulfate; and the naphthylhydrazine organic acid salt is naphthylhydrazine trifluoroacetate, naphthylhydrazine acetate, naphthylhydrazine formate, naphthylhydrazine citrate or naphthylhydrazine oxalate; and hydrazine radicals on the naphthylhydrazine inorganic acid salt or naphthylhydrazine organic acid salt are all 1-substituted or 2-substituted. The application technically overcomes the defect that small-molecule samples cannot be effectively analyzed because serious matrix background interference is apt to be caused in a low molecular weight zone when organic small-molecule matrices are commonly used. The matrix used by the invention is not required to be added with ionizing reagent and the requirements on sample treatment are reduced; and since background interference hardly exists when m / z is smaller than 500, various complex mixed systems can also be analyzed by using the matrix.

Description

technical field [0001] The invention relates to the application of a naphthalene hydrazine inorganic acid salt or a naphthalene hydrazine organic acid salt as a matrix in matrix-assisted laser desorption ionization mass spectrometry, and belongs to the technical field of mass spectrometry detection. Background technique [0002] Since Karas et al. and Tanaka et al. reported in 1988 that matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS) technology can be used for effective mass spectrometry analysis of biological macromolecules, MALDI-TOF MS technology has been researched by many countries. favored by those. However, since the commonly used matrices of MALDI-TOF MS technology are small molecular organic compounds, such as α-cyano-4-hydroxycinnamic acid (CCA), 2,5-dihydroxybenzoic acid (DHB), sinapinic acid (SA), 3-Hydroxy-2-pyridinecarboxylic acid (3-HPA), anthracenol (DI) and 3-aminoquinoline (3-AQ), etc. During the analysis proces...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/62
Inventor 聂宗秀何清陈素明王佳宁侯剑
Owner INST OF CHEM CHINESE ACAD OF SCI
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