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Method of preparing octadecyl type integral liquid chromatography micro-column

An octadecyl-type, liquid chromatography technology, which is applied in the field of preparation of octadecyl-type monolithic liquid chromatography microcolumns, can solve the problems of difficult preparation of filter sieve plates and low success rate, and achieve permeability Good, fast analysis speed, low column pressure effect

Inactive Publication Date: 2006-09-20
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention aims at the existing liquid chromatography micro-column preparation method which affects the service life of the chromatographic column and corresponding instruments, requires high column packing technology, and is especially difficult for the preparation of filter sieve plates at both ends of the capillary chromatographic column , low success rate and other problems, provide a simple and convenient operation, the resulting monolithic liquid chromatography microcolumn has good permeability, low column pressure, high mechanical strength, fast analysis speed, and does not need to bond other functional groups on the surface of the monolithic column Preparation method of octadecyl-type monolithic liquid chromatography micro-column that can directly perform μ-LC separation operation, and can conveniently control the length of the monolithic column according to needs
The obtained monolithic column can be directly used for separation under μ-LC without bonding other functional groups

Method used

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  • Method of preparing octadecyl type integral liquid chromatography micro-column
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  • Method of preparing octadecyl type integral liquid chromatography micro-column

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 1) Cleaning and activation treatment of the inner wall of the capillary: Take a fused silica capillary with an inner diameter of 530 μm and a length of 3 m, first wash it with acetone for 30 minutes, and then use 1mol L -1After washing with NaOH for 30min, rinse with secondary water to neutrality, and then use 0.1mol L -1 Rinse with HCl at a temperature of 70°C for 2 hours, rinse with water twice to neutrality, place in a gas chromatographic column thermostat, blow nitrogen slowly at 160°C overnight, and then seal both ends and store in a desiccator.

[0036] 2) Pre-polymerization of the inner wall of the capillary: take 2.0mL of γ-methacrylic acid oxypropyl trimethoxysilane (γ-MAPS) and add 10 μL of dry acetic acid, nitrogen and ultrasonic vibration for 10min, and then inject it into the pretreated capillary Inside, both ends were sealed, placed in an oven at 60°C for 20 hours, and the remaining reaction liquid was flushed out with acetone, and then nitrogen was blown ...

Embodiment 2

[0039] The cleaning and activation 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, take 2.0 mL of γ-methacryloxypropyltrimethoxysilane (γ-MAPS) and add 2 μL of dry formic acid, and the others are the same as in Example 1. OMA: EDMA: AIBN=49.5: 49.5: 1 configuration reaction monomer mixture; The porogen is made up of 70% n-propanol and 30% 1,4 butanediol, and the proportion of the reaction monomer mixture and the porogen is respectively 45:55; 50:50; 55:45; 70:30 After mixing, nitrogen blowing, ultrasonic vibration and degassing for 15 minutes were injected into the pre-bonded capillary, one end was sealed and the other end was sealed after ultrasonic vibration. After reacting in a water bath at 50°C for 20 hours, connect it to the liquid chromatography pump and wash it with acetonitrile for 8 hours. image 3 3a, 3b, 3c, and 3d in the figure are the scanning electron micrographs of the proportions ...

Embodiment 3

[0041] The cleaning and activation 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, take 2.0 mL of γ-methacryloxypropyltrimethoxysilane (γ-MAPS) and add 5 μL of dry acetic acid. Others are the same as in Example 1. Prepare OMA: EDMA is respectively 69.5: 29.5, 64.5: 34.5, 59.5: 39.5, 54.5: 44.5, and AIBN is a reaction monomer mixture of 1; porogen consists of 70% n-propanol and 30% 1,4-butanediol Composition, the reaction monomer mixture and the porogen are mixed in a ratio of 40:60, then blown with nitrogen and degassed by ultrasonic vibration for 15 minutes, inject it into a pre-bonded capillary, seal one end and seal the other end after ultrasonic vibration. After reacting in a water bath at 60°C for 20 hours, connect it to the liquid chromatography pump and wash it with acetonitrile for 5 hours. Figure 4 4a, 4b, 4c, and 4d in are the SEM images of OMA:EDMA=69.5:29.5; 64.5:34.5; 59.5:39.5; 54.5...

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Abstract

An octadecyl-type integral liquid-phase chromatographic microcolumn with high throughput, mechanical strength and analyzing speed and low column pressure for direct mu-LC separation is prepared through activating the inner surface of capillary tube, prepolymerizing, and preparing the integral octadecyl methylacrylate-glycol dimethylacrylate column from the octadecyl methylacrylate-glycol dimethylacrylate copolymer as skeleton, the n-propanol-1,4-butanediol mixture as pore forming agent, and azodiisobutanenitrile as trigger through reaction and flushing.

Description

technical field [0001] The invention relates to a liquid chromatography microcolumn, in particular to a preparation method of an octadecyl monolithic liquid chromatography microcolumn. Background technique [0002] Micro-column high-performance liquid chromatography (Micro-column HPLC), referred to as micro-column liquid chromatography (μ-LC), is a chromatographic micro-separation technology developed in recent years. Manufacturing technology greatly improves the separation ability of the chromatographic column, in addition, it has mobile phase, stationary phase, low sample consumption and is easy to combine with mass spectrometry (MS), nuclear magnetic resonance spectroscopy (NMR) or with other high performance liquid chromatography columns ( SEC, IC) form two-dimensional HPLC and other advantages, making it a major research hotspot in the modern chromatographic field. It will have broad application prospects in the fields of medicine, food, environment, biomacromolecule (...

Claims

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Application Information

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IPC IPC(8): B01J20/285B01D15/10G01N30/60
Inventor 徐振东王秋泉付强
Owner XIAMEN UNIV
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