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Reversed phase/ion exchange mixed mode chromatography stationary phase, preparation method and application

A mixed-mode chromatography and chromatographic stationary phase technology, applied in the field of reversed-phase/ion-exchange mixed-mode chromatography stationary phase, preparation and application, can solve the problems of few varieties, single structure, inability to adapt to complex components, etc. Harm, good separation effect, simple and feasible process route

Active Publication Date: 2019-07-16
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, so far, there are not many varieties of mixed-mode chromatographic stationary phases with a single structure, which cannot meet the increasing analysis requirements of complex components in the field of pharmaceutical analysis, especially compound drugs.

Method used

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  • Reversed phase/ion exchange mixed mode chromatography stationary phase, preparation method and application
  • Reversed phase/ion exchange mixed mode chromatography stationary phase, preparation method and application
  • Reversed phase/ion exchange mixed mode chromatography stationary phase, preparation method and application

Examples

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preparation example Construction

[0047] Preparation of activated silica gel: add a certain amount of silica gel particles to 8-10 times the mass of 10%-15% HCl solution, stir, reflux at 105°C for 8 hours, wash with water until neutral, and vacuum dry at 80°C.

[0048] Preparation of epoxy-based silica gel: Put the above-mentioned acidified silica gel particles into an autoclave with a Teflon liner, and add 1.92mmol-3.6mmol of γ-(2,3-epoxypropoxy)propyl trimethyl per gram Oxysilane, seal the autoclave, and react at 150°C for 8h. The unreacted silylating reagent was washed away with absolute ethanol, the product was collected by filtration, and vacuum-dried at 80° C. to obtain epoxy-functionalized porous silica gel.

[0049] Preparation of sulfonic acid-based silica gel: Disperse the above-mentioned epoxy-bonded silica gel microspheres into ultrapure water with a mass number of 8-10 times, add 1.92mmol-3.6mmol sodium bisulfite per gram, and ultrasonically mix. Adjust the pH value to 7-8 with triethylamine, rea...

Embodiment 1

[0066] Activation of embodiment 1 silica gel microspheres

[0067] Take 10g of silica gel microspheres and add them to a 250mL three-neck flask, add 100mL of 10% HCl solution, stir mechanically, reflux at 105°C for 8h, wash with water until neutral, and dry in vacuum at 120°C overnight to obtain activated silica gel microspheres. The infrared characterization spectrum of silica gel microspheres is as follows: figure 2 shown at 3400cm -1 There are larger silanol absorption peaks.

Embodiment 2

[0068] Embodiment 2 Dry method preparation of epoxy-bonded silica gel microspheres

[0069] Take 10 g of activated silica gel microspheres prepared according to Example 1 and put them into an autoclave, add 5.31 mL of γ-(2,3-glycidoxy)propyltrimethoxysilane, and react at 150° C. for 8 h. Wash with absolute ethanol and dry under vacuum at 80°C to obtain epoxy-functionalized silica gel microspheres. The infrared characterization spectrum of the epoxy-functionalized silica gel is as follows: image 3 shown, after bond and epoxy at 2800cm -1 and 2890cm -1 The stretching vibration peak of C-H appears nearby, indicating that the epoxy group is bonded to the surface of the silica gel. The elemental analysis and characterization are shown in Table 1. The carbon content is 8.05%, and the calculated surface bond amount is 4.50mol / m 2 . The outstanding advantage of the method is that it does not use harmful organic solvents such as toluene, which is beneficial to the protection of he...

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Abstract

The invention relates to a reversed phase / ion exchange mixed mode chromatography stationary phase, a preparation method and an application. The reversed phase / ion exchange mixed mode chromatography stationary phase is called as an octadecyl / sulfonic acid group mixed chromatography stationary phase, and consists of the octadecyl and the sulfonic acid group bonded to the surface of porous silica gel. The preparation method is as follows: bonding gamma-(2,3-epoxypropoxy)propyltrimethoxysilane KH-560 to the surface of the porous silica gel particle by the chemical vapor deposition method, and respectively carrying out a reaction of KH-560 as a linker arm with sodium bisulfite and octadecyl chloride to prepare the octadecyl / sulfonic acid group mixed chromatography stationary phase.

Description

technical field [0001] The invention relates to a liquid chromatography stationary phase and a preparation method and application thereof. Background technique [0002] Drug analysis technology plays an important role in the quality control of drug R&D, production, storage and circulation. In order to improve the therapeutic effect of drugs on diseases, the combination of different single component drugs has become a widely used strategy, but the combination of drugs leads to a decrease in drug compliance and increases the risk of patients. Fixed-dose combination drugs developed in recent years are single dosage forms, such as capsules or pills, containing two or more active ingredients. It can not only use the synergistic effect of different drug ingredients to improve the therapeutic effect of the drug, but also reduce the number of tablets taken by patients. Therefore, it is welcomed by doctors and patients. The products include anti-AIDS drugs, anti-hypertensive drugs, ...

Claims

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Application Information

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IPC IPC(8): B01J20/286B01J20/28B01J20/30B01J39/17B01D15/36B01D15/32G01N30/02G01N30/06
CPCB01D15/327B01D15/362B01J20/28021B01J20/286B01J2220/4806B01J2220/4812B01J2220/52B01J2220/54B01J39/17G01N30/02G01N30/06
Inventor 万谦宏张双红陈磊张高乐焦亚磊丁超李宏亮
Owner TIANJIN UNIV
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