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Capillary monolithic column spray needle and preparation method and application thereof

A capillary monolithic column and capillary technology, which is used in measuring devices, instruments, scientific instruments, etc., can solve problems such as complexity and deviation, and achieve the effects of improving repeatability, improving service life, and improving separation efficiency and repeatability.

Inactive Publication Date: 2009-11-04
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Claims
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Problems solved by technology

Therefore, if the separated chromatographic peaks are disturbed and mixed, their corresponding mass spectra will become more complicated and biased, so electrospray spray also has a great influence on the quantitative method of stable isotope labeling

Method used

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  • Capillary monolithic column spray needle and preparation method and application thereof
  • Capillary monolithic column spray needle and preparation method and application thereof
  • Capillary monolithic column spray needle and preparation method and application thereof

Examples

Experimental program
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Embodiment 1

[0027] 1. Preparation of hydrophobic polymer monolithic column

[0028] Synthesize a C12 alkyl polymer monolithic column with strong hydrophobic retention mechanism in a capillary with an inner diameter of 75 or 25 μm and a length of 150 cm:

[0029] 1. Capillary pretreatment

[0030] First rinse the capillary empty column with 0.1M NaOH solution for 1h, then rinse the capillary with deionized water until the pH of the effluent liquid is 7.0, then rinse the capillary with 0.1M HCl solution for 4h, and then rinse the capillary with deionized water to the pH of the effluent liquid 7.0, then flush the capillary column with methanol solution for 10 minutes, and blow dry with nitrogen. A mixture of methanol and methacryloxypropyl-trimethoxysilane is injected into the capillary. React for 5-24 hours at a temperature of 20 degrees to 70 degrees. Then rinse with methanol and water. Finally, blow dry with nitrogen for use.

[0031] 2. Polymerization of C12 alkyl strong hydrophobic monolith...

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Abstract

The invention relates to an interface for microcolumn liquid chromatogram and mass spectrum, in particular to a capillary monolithic column spray needle. The capillary monolithic column spray needle comprises a capillary pipe, the capillary pipe is filled with monolithic material, a needle head used for electron spray extend at one end of the capillary pipe to form a capillary monolithic column spray needle, then the capillary monolithic column spray needle is connected to the tail end of a capillary separating column through a two-way pipe and the voltage used for electron spray is applied to the two-way pipe. The invention has the main advantages that because the dead volume existing in an electron spray needle in the combined use of the microcolumn liquid chromatography and the mass spectrum and the electron spray needle is eliminated, the capillary monolithic column spray needle eliminates the disturbance and the mixing action of the dead volume to the microcolumn liquid chromatography is eliminated, greatly enhances the separating capacity and the repeatability of the microcolumn liquid chromatography and represents superior performance to the commercial capillary electron spray needle in the quantitative proteomics; and in addition, because the monolithic column material exists in the capillary monolithic column spray needle, the problem that the electron spray needle is easy to be blocked during the separation and the analysis process is solved and the service life of the electron spray needle is greatly prolonged.

Description

Technical field [0001] The invention relates to a liquid-mass spectrometry interface, in particular to a capillary monolithic column spray needle applied to a microcolumn liquid chromatography and mass spectrometry system, and its preparation and application. Background technique [0002] Micro-column liquid chromatography (μ-LC) is an important direction of chromatographic miniaturization, which refers to the liquid chromatography analysis method of chromatographic columns with an inner diameter of 10μm to 1mm. Compared with conventional liquid chromatography, it has the advantages of high column efficiency, low mobile phase reagent consumption, easy to realize multi-dimensional chromatographic separation, and easy to combine with mass spectrometry to improve analysis sensitivity. It is widely used in the separation and analysis of biological samples, especially for proteins. Omics analysis (Ivanov, AR, ect, Anal. Chem., 2003, 75, 5306). The combined technology of microcolumn li...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/16G01N30/06
Inventor 邹汉法王方军叶明亮董靖
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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