Application of black phosphorus in matrix-assisted laser desorption ionization time-of-flight mass spectrometry

A matrix-assisted laser and time-of-flight mass spectrometry technology, applied in the field of mass spectrometry detection, can solve the problems of inaccurate quantitative analysis and poor sensitivity

Inactive Publication Date: 2018-01-23
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, SIL can also be used to solve the problems of poor sensi

Method used

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  • Application of black phosphorus in matrix-assisted laser desorption ionization time-of-flight mass spectrometry
  • Application of black phosphorus in matrix-assisted laser desorption ionization time-of-flight mass spectrometry
  • Application of black phosphorus in matrix-assisted laser desorption ionization time-of-flight mass spectrometry

Examples

Experimental program
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Effect test

Embodiment 1

[0039] [Example 1] Black phosphorus is used as a matrix to detect small molecule compounds

[0040] The black phosphorus used in the present invention was purchased from Xianfeng Nano Material Technology Co., Ltd. (Nanjing, China). Apply black phosphorus directly to the MALDI target to obtain a coating with a diameter of approximately 2 mm. As a comparison, 2 mg / mL CNTs, GO and C60 matrix dispersions were prepared respectively, and 0.5 μL of the dispersions were spotted on the plate as the matrix.

[0041] The analytes are more than 30 kinds of substances with a molecular weight range of 1-1000Da, including acidic substances (acid dyes, acidic surfactants and fatty acids), basic substances (basic dyes and cationic surfactants), amphoteric substances (amino acids and Polypeptides) and polycyclic aromatic hydrocarbons. Take 0.5 μL of the analyte solution and spot it on the matrix layer, and perform MALDI-TOF MS analysis after the solvent evaporates to dryness.

[0042] All mass...

Embodiment 2

[0044] [Example 2] Detection of 4-APC-labeled aldehydes by black phosphorus

[0045] In previous work, we developed the derivatization reagent 4-APC containing quaternary ammonium groups [1] , can be used to derive aldehydes, so in this invention we use black phosphorus to detect 4-APC and 4-APC-labeled five aldehydes: butyraldehyde, hexanal, heptanal, octanal and nonanal.

[0046] The steps for labeling aldehydes with 4-APC are as follows: Add 10 μL of NaBH to 10 μL of aldehyde mixture 3 CN methanol solution (1 mg / mL) and 20 μL of 4-APC methanol solution (1 mg / mL) were dilute to 100 μL with 50 mM ammonium acetate solution (pH 5.7). React for 1h in a constant temperature shaker at 25°C and 1500rpm, and take 0.5μL of the reaction product for MALDI-TOF MS analysis.

[0047] Test results such as image 3 Shown: the detection limit of black phosphorus to 4-APC is 51nM ( image 3 a), at the same time, it has a good detection effect on aldehydes labeled with 4-APC ( image 3 d)...

Embodiment 3

[0048] [Example 3] Black phosphorus detects BQB-labeled sulfhydryl compounds

[0049] In previous work, we developed the derivatization reagent BQB containing quaternary ammonium groups [2] , can be used to derivatize the sulfhydryl groups of thiol compounds, because in the present invention we use black phosphorus to detect four sulfhydryl compounds marked by BQB and BQB: N-acetylcysteine ​​(Nac), glutathione (GSH), Cysteine ​​(Cys) and Homocysteine ​​(HCys).

[0050] The steps for BQB labeling of thiol compounds are as follows: add 10 μL of BQB methanol solution (5 mM) to 10 μL of thiol compound standard mixture, and dilute to 100 μL with glycine hydrochloride buffer solution (5.0 mM, pH 3.5). React for 1h in a constant temperature shaker at 60°C and 1500rpm, and take 0.5μL of the reaction product for MALDI-TOF MS analysis.

[0051] Test results such as image 3 Shown: the detection limit of black phosphorus to BQB is 37nM ( image 3 b), at the same time, it has a good d...

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Abstract

The invention discloses application of black phosphorus to detection of a matrix-assisted laser desorption ionization time-of-flight mass spectrum (MALDI-TOF MS). The molecular weight of a substance to be detected in the application ranges from 0 Da to 1000 Da; black phosphorus serves as the matrix, and has a superior mass spectrum response to small molecules containing quaternary ammonium groups; black phosphorus is soft in texture, can be directly smeared to an MALDI target plate to be analyzed, and does not need to be dispersed in a solvent in advance, and the time-consuming solvent dispersing process is omitted; moreover, it is unnecessary to consider the problem of compatibility between the matrix and the sample solvent; under irradiation of laser, black phosphorus can generate multiple phosphorus clusters used for assisting analyte in the desorption and ionization process. Compared with a traditional organic matrix, interference of black phosphorus to the small-molecule area is small; in combination with a stable isotope labeling (SIL) strategy, black phosphorus is successfully used for fast qualitative and quantitative analysis of aldehydes materials, sulfhydryl compounds and acid plant hormone in saliva, urine samples and serum.

Description

technical field [0001] The invention belongs to the technical field of mass spectrometry detection, and in particular relates to the application of a phosphorus matrix in matrix-assisted laser desorption ionization time-of-flight mass spectrometry. Background technique [0002] Matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS) has been widely used in the structural analysis of proteins, sugars, nucleic acids, peptides and other biological macromolecules and polymers since it was developed in the late 1980s and molecular weight determination. Compared with other mass spectrometry techniques, MALDI has many advantages, such as easy operation, fast detection speed, high throughput, strong anti-interference ability, less organic solvent consumption (no mobile phase) and less sample consumption. However, since the traditional MALDI matrix is ​​mainly low-molecular-weight organic acids such as: α-cyano-4-hydroxycinnamic acid (α-cyano-4-hy...

Claims

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Application Information

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IPC IPC(8): G01N27/64
CPCG01N27/64
Inventor 冯钰锜何小梅
Owner WUHAN UNIV
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