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Application of submicron carbon oxide balls as medium in MALDI-MS

A technology of micron carbon oxide and carbon oxide spheres, which is applied in measuring devices, material analysis through electromagnetic means, instruments, etc., can solve problems affecting the stability and repeatability of mass spectrometry detection, complicated preparation process, and limited applicability, etc. Achieve the effects of eliminating background interference, good water solubility, and improving repeatability

Active Publication Date: 2017-06-13
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

[0005] However, it is difficult to control the size of carbon materials such as carbon nanotubes or graphene, and the development of modified water-soluble carbon-based materials as a matrix preparation process is complex and costly, and it is difficult to provide dimensionally stable matrix materials for MALDI-MS, which affects the quality of mass spectrometry Stability and reproducibility, which limit the suitability of carbon-based nanomaterials as matrices for MALDI-MS applications

Method used

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Examples

Experimental program
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Embodiment 1

[0035] Embodiment 1: the preparation of the carbon oxide sphere that diameter is 180nm-250nm

[0036] (1) Disperse 0.029g CTAB and 0.96g F127 in ethanol / water (7mL / 14mL) solution, and magnetically stir at room temperature for 20min to form a colorless transparent solution.

[0037] (2) Add 0.093g (30mmoL) of resorcinol and 0.171mL of ammonia water (mass concentration: 25%) to step (1), and stir electromagnetically at 60°C.

[0038] (3) After half an hour, 0.126 μL of formaldehyde was added to step (2), and electromagnetic stirring was continued for 16 hours.

[0039] (4) Centrifuge the reaction solution obtained in step (3), wash with water three times, and wash with ethanol twice. Vacuum dried overnight to obtain a khaki carbon sphere precursor.

[0040](5) The khaki carbon sphere precursor obtained in step (4) was carbonized at 600° C. for 4 hours in a nitrogen atmosphere, and cooled naturally to obtain carbon spheres with an outer diameter of 180 nm-250 nm.

[0041] (6) ...

Embodiment 2

[0043] Embodiment 2: the preparation of the carbon oxide sphere that diameter is 600nm-800nm

[0044] The experimental operation steps are the same as those described in steps (1)-(6) in Example 1, except for the following special instructions.

[0045] The amount of CTAB used in step (1) is 0.232g.

[0046] In step (5), the temperature is naturally lowered to obtain carbon spheres with an outer diameter of 600nm-800nm.

[0047] Vacuum drying in step (6) to obtain carbon oxide spheres with an outer diameter of 600nm-800nm.

[0048] figure 2 It is the transmission electron micrograph of carbon oxide spheres with a diameter of 600nm-800nm ​​obtained in Example 2;

[0049] The preparation method of the submicron carbon oxide spheres involved in the present invention is simple, the raw materials used are cheap, and the prepared materials are spherical with regular appearance, and the particle diameter can be adjusted between 70nm and 1000nm. The obtained carbon oxide spheres ...

Embodiment 3

[0052] Example 3: 180nm-250nm carbon oxide spheres as a matrix MALDI-TOF MS detection of sugar compounds D-xylose (MW=150.13), a sugar compound that is not easily ionized, was used as the detection object.

[0053] 1. Prepare 10Mm of D-xylose mother solution (aqueous solution), and obtain a 1Mm dilution by gradient dilution. It can be stored in a refrigerator at 4°C.

[0054] 2, the carbon dioxide sphere matrix solution of 180nm-250nm in the preparation 2mg / Ml embodiment 1 (solvent used is ethanol water mixed solution, V 乙醇 :V 水 =1:1). Ultrasound for 5 minutes to disperse evenly. It can be stored in a refrigerator at 4°C.

[0055] 3. Take 0.5 μL of the 1 Mm diluent in step 1, drop it on the 384-well stainless steel MALDI sample target, and let it dry naturally to form a uniform sample layer.

[0056] 4. Take 0.5 μL of the matrix solution in step 2, apply it on the sample layer, and let it dry naturally.

[0057] 5. Send to MALDI-TOF MS for analysis. Mass spectrometry da...

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Abstract

The present invention relates to medium materials for MALDI, and in particular relates to application of submicron carbon oxide balls as a medium in MALDI-MS. In the present invention, the submicron carbon oxide balls are used as the MALDI-MS medium, a defect of medium interference when a conventional organic medium is used is solved, the accurate analysis of various compounds with molecular weight less than 1000 Dalton, such as amino acid amino acids, lipid compounds, polypeptides, oligosaccharides and drugs can be fast and efficiently achieved. The submicron carbon oxide ball medium related in the present invention can be prepared by using a simple and controllable method, is regular in morphology, uniform in size, low in cost, and good in water solubility, and overcomes a problem that the dimension is controlled difficultly so as to influence stability of mass spectrometric detection when carbon-based materials such as carbon nano tubes and graphene are used as the MALDI medium, thus being an optimized medium capable of assisting MALDI-MS to achieve high-sensitivity and high-throughput analysis on the compounds within a low molecular weight area.

Description

technical field [0001] The invention relates to an auxiliary matrix material for laser desorption ionization mass spectrometry detection, specifically the application of submicron carbon oxide spheres as a matrix in laser desorption ionization mass spectrometry (MALDI-MS). Background technique [0002] Since Tanaka and Hillenkamp proposed the matrix-assisted laser desorption ionization (MALDI) technology in 1988, this technology combined with time-of-flight mass spectrometry (MALDI-MS) has become an important tool in life science research such as genes and proteomics . (Rapid Commun Mass Sp 1988,2(8),151-153; Nature 2003,422(6928),198-207) [0003] In MALDI-MS technology, the matrix plays the role of absorbing and transmitting laser energy and ionizing the sample. The commonly used matrices in MALDI-MS technology are small molecular organic compounds, such as α-cyano-4-hydroxycinnamic acid (CHCA), 2,5-dihydroxybenzoic acid (DHB), sinapinic acid (SA), 3- Aminoquinoline (3-...

Claims

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Application Information

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IPC IPC(8): G01N27/64
CPCG01N27/64
Inventor 吴仁安李鑫徐桂菊
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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