Two-phase integral column as well as preparation and application thereof

A monolithic column and monolithic material technology, applied in other chemical processes, chemical instruments and methods, material separation, etc., to achieve the effects of easy fabrication, increased column length, and efficient separation

Inactive Publication Date: 2011-08-31
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, no one has reported the synthesis of two different monolithic materials before and after in the same capillary

Method used

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  • Two-phase integral column as well as preparation and application thereof
  • Two-phase integral column as well as preparation and application thereof
  • Two-phase integral column as well as preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1. Preparation of two-phase capillary monolithic column

[0024] Such as figure 2 As shown, a 10 cm long strong cation exchange material and a 65 cm long strong hydrophobic material were successively synthesized in a capillary with an inner diameter of 100 microns and a length of 75 cm.

[0025] 1. Capillary Pretreatment

[0026] First wash 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 until the pH of the effluent liquid is 7.0, then rinse the capillary column with methanol solution for 10 min, and dry it with nitrogen. A mixture of methanol and methacryloxypropyl-trimethoxysilane was injected into the capillary. React at a temperature of 20°C to 70°C for 5-24 hours. Then rinse with methanol and water. Finally, dry it with nitrogen gas.

[0027] 2. Synthesis...

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Abstract

The invention relates to a monolithic capillary column, in particular to a two-phase monolithic column which is characterized in that two fixed phases with different separation mechanisms exist in the same column pipe; the two phases exist in the form of a front section and a rear section. The two-phase monolithic column has the main advantages of basically eliminating dead volume which is generated when two monolithic columns with different separation mechanisms are connected in a micro-column liquid phase chromatographic separation system, carrying out automatic online multi-dimensional separation and having extremely strong capability of separating complex samples such as protein zymolyte; furthermore, the monolithic column has good permeability and low operation pressure, and is easy to be operated on a normal liquid chromatography and can obtain high-efficiency separation results.

Description

technical field [0001] The invention relates to a capillary monolithic column, in particular to a capillary monolithic column applied to micro-column liquid chromatography (μ-LC) on-line multi-dimensional separation and its preparation. Background technique [0002] Microcolumn 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 10 μm to 1 mm. Compared with conventional liquid chromatography, it has the advantages of high column efficiency, low mobile phase sample consumption, good column permeability, easy to achieve multi-stage chromatographic separation, and easy to combine with mass spectrometry to improve analytical sensitivity. It is widely used in biological samples. Separation analysis, especially suitable for proteomics analysis (Ivanov, A.R., ect, Anal. Chem., 2003, 75, 5306). [0003] In 1999, Yates et al. proposed ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/60B01J20/281
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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