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Application of molybdenum disulfide/nanosilver composite serving as matrix to matrix-assisted laser desorption/ionization time of flight mass spectrometry

A matrix-assisted laser and time-of-flight mass spectrometry technology, which is applied in the preparation of test samples, material analysis by electromagnetic means, and measurement devices, can solve the problems of poor dispersion of metal oxides and carbon-based materials, poor signal repetition, Limiting the application of nanomaterials and other issues, achieving strong anti-salt interference, high sensitivity, and improving the efficiency of laser desorption ionization

Active Publication Date: 2016-09-07
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Even so, these nanomaterials still have shortcomings. Most metal oxides and carbon-based materials are poorly dispersible in water, which makes the signal repetition effect not good in mass spectrometry detection.
In addition, the tedious assembly process of some nanomaterials takes a long time, which greatly limits the application of nanomaterials as substrates in mass spectrometry.

Method used

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  • Application of molybdenum disulfide/nanosilver composite serving as matrix to matrix-assisted laser desorption/ionization time of flight mass spectrometry
  • Application of molybdenum disulfide/nanosilver composite serving as matrix to matrix-assisted laser desorption/ionization time of flight mass spectrometry
  • Application of molybdenum disulfide/nanosilver composite serving as matrix to matrix-assisted laser desorption/ionization time of flight mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Example 1: Synthesis of molybdenum disulfide / nanometer silver composite.

[0041] (1) Under the protection of nitrogen, 0.019mol of molybdenum disulfide powder and 0.0475mol of n-butyllithium were quickly added to a 50mL polytetrafluoroethylene reactor, heated and reacted in an oven at 100°C for 4h, and naturally cooled to room temperature.

[0042] (2) The solution in step (1) was quickly transferred to a 250 mL three-necked bottle, and reacted at room temperature 25° C. for 48 h under nitrogen protection.

[0043] (3) Quickly filter the solution obtained in step (2) under reduced pressure, wash 3 times with 200 mL of n-hexane, then quickly transfer the product obtained by suction filtration to a certain amount of deionized water for ultrasonication for 4 hours, and centrifuge to remove the unstripped product Molybdenum disulfide, take the supernatant and save it, and finally measure its concentration.

[0044] (4) Take 16mL of the solution obtained in step (3) (conce...

Embodiment 2

[0046] Example 2: Synthesis of molybdenum disulfide / nanometer silver composite.

[0047] (1) Under the protection of nitrogen, quickly add 0.03mol molybdenum disulfide powder and 30mL n-butyllithium (1.6M) into a 50mL polytetrafluoroethylene reactor, heat and react in an oven at 150°C for 3h, and cool naturally to room temperature.

[0048] (2) The solution in step (1) was quickly transferred to a 250 mL three-neck flask, and reacted at 40° C. for 24 h under nitrogen protection.

[0049] (3) Quickly filter the solution obtained in step (2) under reduced pressure, wash with 200 mL of n-hexane for 3 times, then quickly transfer the product obtained by suction filtration to a certain amount of deionized water for ultrasonication for 2 hours, and centrifuge to remove the unstripped product Molybdenum disulfide, take the supernatant and save it, and finally measure its concentration.

[0050] (4) Get 30mL of step (3) gained solution (concentration is 0.05g / L), add 3mL trisodium c...

Embodiment 3

[0051] Embodiment 3: Synthesis of molybdenum disulfide / nano-silver composite.

[0052] (1) Under the protection of nitrogen, quickly add 0.06mol molybdenum disulfide powder and 40mL n-butyllithium (1.6M) into a 50mL polytetrafluoroethylene reactor, heat and react in an oven at 200°C for 6h, and cool naturally to room temperature.

[0053] (2) The solution in step (1) was quickly transferred to a 250 mL three-neck flask, and reacted at 50° C. for 48 h under nitrogen protection.

[0054] (3) Quickly filter the solution obtained in step (2) under reduced pressure, wash 3 times with 200 mL of n-hexane, then quickly transfer the product obtained by suction filtration to a certain amount of deionized water for ultrasonication for 8 hours, and centrifuge to remove the unstripped product Molybdenum disulfide, take the supernatant and save it, and finally measure its concentration.

[0055] (4) Get 4mL of step (3) gained solution (concentration is 0.5g / L), add 2mL trisodium citrate a...

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Abstract

The invention discloses application of a molybdenum disulfide / nanosilver composite serving as a matrix to MALDI (matrix-assisted laser desorption / ionization) time of flight mass spectrometry. Few-layer molybdenum disulfide is prepared according to an improved chemical lithium ion intercalation and exfoliation method, on the basis of which the molybdenum disulfide / nanosilver composite is prepared through in-situ reduction of silver nitrate. An analysis method taking molybdenum disulfide / nanosilver composite as an MALDI matrix is applicable to mass spectrometry of micromolecules with molecular weight smaller than 1000 and suitable for molecules of amino acids, oligopeptides, fatty acids, alkaloids, hormones, antibiotics, antibacterial drugs, anticancer drugs and the like. Matrix background interference is avoided when the method is adopted for detection of molecules with a mass-to-charge ratio (m / z) smaller than 1000. The method can be effectively applied to fields of organic and biomass spectrometry, imaging mass spectrometry, protein mass spectrometry, metabonomics, biomarker discovery, environmental analysis and the like.

Description

technical field [0001] The invention belongs to the field of advanced nanomaterials and nanotechnology, and specifically relates to the application of a molybdenum disulfide / nanometer silver compound as a MALDI matrix in the detection of small molecules. Background technique [0002] Matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS) technology has become a useful technique in the analysis of biomolecules such as peptides, proteins and oligosaccharides. However, although there are many kinds of organic small molecule matrices used in MALDI-TOF MS, it is difficult to use in the analysis of small molecular weight (below 1000 Da) compounds, mainly because the organic small molecular matrix will be fragmented and the association between molecules will occur. As a result, severe matrix background interference occurs. Secondly, the analyte and the matrix are miscible and there is an uneven co-crystallization phenomenon, which affects the r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/64G01N1/38
CPCG01N1/38G01N27/64
Inventor 许丹科赵亚菊刘晓辉李慧孙亮
Owner NANJING UNIV
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