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Alkylamine silica gel capillary monolithic column and preparation method and use thereof

A capillary monolithic column, alkylamine technology, applied in separation methods, chemical instruments and methods, other chemical processes, etc., can solve the problem of few silica-based monolithic columns, and achieve silica-based matrix network permeability and high mechanical strength, Increased hydrophilicity and solvent resistance

Inactive Publication Date: 2008-11-19
GUANGXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ding et al. (GuoshengDing, Zhenliang Da, Ruijuan Yuan, James J.Bao, Electrophoresis, 2006, 27, 3363-3372) prepared a reverse-phase-weak anion exchange mixed-mode silica-based monolithic column, but it is applied to polar and alkaline There are few reports on silica-based monolithic columns for active compounds (Sebastiaan Eeltink Wim Th.Kok Electrophoresis 2006, 27, 84-96)

Method used

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  • Alkylamine silica gel capillary monolithic column and preparation method and use thereof
  • Alkylamine silica gel capillary monolithic column and preparation method and use thereof
  • Alkylamine silica gel capillary monolithic column and preparation method and use thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0041] (1) Preparation of silica gel monolithic column: Take a quartz capillary with an inner diameter of 75 μm and an outer diameter of 365 μm, soak it with 1 mol / L NaOH solution overnight, rinse with secondary water, hydrochloric acid, secondary water, acetone, and anhydrous ether for 1 hour, Then pass N 2 Dry at 180°C for 3 hours, and seal both ends for later use. 0.22g of polyethylene glycol (Mr=10000), 0.225g of urea were dissolved in 2.5mL of 0.01mol / L acetic acid solution, wherein 1mL of tetramethoxysilane and methyltrimethoxysilane (9 / 1, v / v), stir vigorously in an ice bath until the solution becomes a transparent and uniform sol, inject it into the pretreated capillary, seal both ends with silicone rubber, put it in a constant temperature water bath at 40°C for 25h, take it out, and store it at 120°C Under heat treatment for 3h to obtain proper specific surface and pore structure. Cut off the seal, rinse out unreacted substances with water, rinse with water and abs...

Embodiment 2

[0047] Using 2.5 g of n-decylamine instead of n-tetradecylamine, the procedure in Example 1 was followed to obtain a n-decylamine capillary monolithic column.

Embodiment 3

[0049] Using the alkylamine silica gel capillary monolithic column prepared in Example 1, the cut-off total length is 30cm, and the effective length is 20cm. , v / v) buffer solution is the mobile phase, under the conditions of applied voltage -15kV and detection wavelength 214nm, the homologues of benzene are separated, and the corresponding peaks are 1. benzene, 2. toluene, 3. ethylbenzene, 4. propylene Benzene, 5. Butylbenzene, 6. Pentylbenzene, 7. Hexylbenzene. Its spectrum is as Figure 4 shown.

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Abstract

The invention provides a novel reversed phase electrochromatography silica-based monolithic column, that is, an alkylamine silica capillary monolithic column which can realize the separation and the analysis of most of organic compounds containing neutral, acidic and alkaline compounds on the premise of meeting the simple chromatographic conditions. The alkylamine silica capillary monolithic column can effectively improve the symmetry of chromatographic peaks in particular to the alkaline organic compounds. The alkylamine silica capillary monolithic column of the invention comprises a capillary and a fixed phase, in the structural formula of the fixed phase: Si represents the silica capillary monolithic column, R represents normal chain alkyl and R1 represents hydrogen or the normal chain alkyl. The invention further provides a preparation method of the alkylamine silica capillary monolithic column, and the specific synthesis steps are as follows: the silica capillary monolithic column is firstly prepared, then the silica capillary monolithic column containing epoxy is prepared and the alkylamine silica capillary monolithic column is finally obtained by connecting alkylamine. The invention further provides the application of the alkylamine silica capillary monolithic column in neutral, acidic and alkaline organic compounds.

Description

technical field [0001] The invention relates to a capillary electrochromatographic column, especially an alkylamine silica gel capillary monolithic column, a preparation method and application thereof. Background technique [0002] Capillary electrochromatography (CEC) is a new separation and analysis method that combines the two technical advantages of high performance liquid chromatography and high performance capillary electrophoresis. It has the characteristics of high efficiency, high selectivity, high resolution and rapid separation. CEC has opened up a new approach in the field of high-efficiency microanalysis and has become a new direction for the development of contemporary chromatography (Luo Guoan, Wang Yiming, Chen Lingxin, Liang Qionglin, Capillary Electrochromatography and Its Application in Life Sciences. Beijing, 2005, Science Press). [0003] The commonly used electrochromatographic columns are particle-packed columns. The filling of this type of column and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D15/22B01J20/291B01J20/283G01N30/60
Inventor 叶芳贵赵书林王顺
Owner GUANGXI NORMAL UNIV
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