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Method for preparing octyl group micro column liquid phase chromatograph integrate column

A technology of liquid chromatography and monolithic column, which is applied in the field of preparation of micro-column liquid chromatography monolithic column, which can solve the problem of low chromatographic capacity and achieve the effects of simple preparation, strong stability and high space utilization

Inactive Publication Date: 2004-12-15
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] So far, the monolithic column is mainly limited to conventional high-performance liquid chromatography (usually select a conventional stainless steel tube with an inner diameter of 3.2-4.6 mm) and capillary electrochromatography (usually choose a quartz capillary with an inner diameter of 100-25 μm), Pavel C. et al prepared a quartz capillary with an inner diameter of 320um using butyl methacrylate, but its chromatographic capacity is still low and requires high preparation technology, and corresponding modifications must be made to the liquid chromatographic instrument at the same time

Method used

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  • Method for preparing octyl group micro column liquid phase chromatograph integrate column
  • Method for preparing octyl group micro column liquid phase chromatograph integrate column
  • Method for preparing octyl group micro column liquid phase chromatograph integrate column

Examples

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Effect test

Embodiment 1

[0023] 1) Cleaning treatment of the inner wall of the capillary: take a quartz glass capillary with an inner diameter of 530 μm and a length of 5 m, wash it with 0.1 mol / L HCl solution at a flow rate of 1.0 mL / min for 0.5 h, and then use deionized water at a flow rate of 1.0 mL / min. Rinse at a flow rate until the washing solution is neutral, then rinse with 0.1moL / L NaOH solution at a flow rate of 1.0mL / min for 2.0h, rinse with deionized water at a flow rate of 1.0ml / min until the washing solution is neutral, and finally use methanol to After flushing at a flow rate of 1.0mL / min for 15min, purging with nitrogen for 2h.

[0024] 2) Pre-bonding of the inner wall of the capillary: Prepare 3.0 mL of a mixed solution of γ-methacrylateoxypropyltrimethoxysilane (γ-MAPS) and methanol (γ-MAPS:MeOH=1:0.5), and then add 3 μL of dry Pyridine, ultrasonically degassed for 10 minutes, injected into the pretreated capillary with a syringe, sealed with rubber stoppers at both ends of the capil...

Embodiment 2

[0027] The cleaning treatment of the inner wall of the capillary is the same as in Example 1. In the pre-bonding of the inner wall of the capillary, 3.0 mL of a mixed solution of γ-methacryloxypropyltrimethoxysilane (γ-MAPS) and methanol (γ-MAPS: MeOH=1 : 1), then add 6 μL of pyridine, inject it into the pretreated capillary, seal both ends of the capillary, place it at 45° C. for 12 h, purging with nitrogen for 2 h, and seal both ends for later use. Configure the reaction monomer mixture, wherein MAOE: EDMA: AIBN=59.5%: 39.5%: 1%; the ratio between the porogen mixture is: propanol 60%, 1,4-butanediol 30%, water 10% ; The ratio between the reaction monomer mixture and the porogen mixture is 35%: 65%; Use a syringe to draw the reaction solution into a pre-bonded empty capillary tube with a length of 23 cm and an inner diameter of 250 μm, seal both ends with rubber plugs, and react at 60 ° C for 12 hours. After the reaction, connect it to the liquid chromatography pump and use ...

Embodiment 3

[0029] Take a capillary with an inner diameter of 50 μm, and the cleaning treatment of the inner wall is the same as in Example 1. In the pre-bonding of the inner wall of the capillary, 3.0 mL of a mixed solution of γ-methacryloxypropyltrimethoxysilane (γ-MAPS) and methanol (γ-MAPS) was prepared. MAPS:MeOH=1:1.5), then add 9 μL of triethylamine, inject it into the pretreated capillary, seal both ends of the capillary, place it at 50°C for 24 hours, purging with nitrogen for 4 hours, and seal both ends for later use . Configure the reaction monomer mixture, wherein MAOE: EDMA: AIBN is 59.5%: 39.5%: 0.5%; the ratio between the porogen mixture is: propanol 70%, 1,4-butanediol 20%, water 10% ; The ratio between the reaction monomer mixture and the porogen mixture is 40%: 60%, and the mixture is injected into an empty capillary tube with an inner diameter of 50 μm and a length of 23 cm. Finally, connect to the liquid chromatography pump and rinse with methanol for 6 hours.

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Abstract

The process of preparing integral octyl group micro liquid phase chromatographic column includes the following steps: pre-bonding one layer of silane matter with olefin radical to the inner wall of capillary; preparing integral octyl methacrylate-glycol dimethyl methacrylate column; injecting the mixture of reactant monomer and pore creating agent into bonded capillary; reaction in water bath and flushing with methanol as flowing phase; and performing mu-HPLC separating operation. The present invention facilitates the reaction between gamma-MAPS and silicohydroxyl in the wall of the capillary and obtains integral column with excellent permeability, high space utilization, low column pressure, powerful stability, simple preparation and easy altering in performance and length.

Description

technical field [0001] The invention relates to a preparation method of a microcolumn liquid chromatography monolithic column, in particular to a preparation method of an octyl microcolumn liquid chromatography monolithic column. Background technique [0002] Micro-column high-performance liquid chromatography (μ-HPLC), also known as capillary liquid chromatography (c-HPLC), is a chromatographic micro-separation technology developed in recent years. It has the advantages of low pollution, high separation efficiency, and easy online combination with other detection methods, so it will play an important role in the fields of biochemistry, medicine, and environment. However, the preparation of μ-HPLC chromatographic columns often adopts the packing method, and there is a large column pressure under high flow conditions, which has a great impact on the service life of the chromatographic column and the maintenance of the instrument. If the flow rate is too small, the analysis t...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/60
Inventor 黄晓佳黄本立王秋泉
Owner XIAMEN UNIV
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