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Pure water-resistant chromatographic stationary phase as well as preparation method and application thereof

A chromatographic stationary phase and a stationary phase technology, applied in the field of pure water-resistant reversed-phase chromatography stationary phase and its preparation, can solve problems such as hydrophobic collapse, and achieve the effects of improved state, simple and feasible steps, and mild reaction conditions

Inactive Publication Date: 2021-11-26
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

[0004] In order to solve the problem of "hydrophobic collapse" existing in ordinary reversed-phase chromatography stationary phases, the present invention discloses a pure water-resistant stationary phase and a preparation method thereof. "collapse" problem, to achieve the purpose of stationary phase resistant to pure water phase

Method used

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  • Pure water-resistant chromatographic stationary phase as well as preparation method and application thereof
  • Pure water-resistant chromatographic stationary phase as well as preparation method and application thereof
  • Pure water-resistant chromatographic stationary phase as well as preparation method and application thereof

Examples

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Effect test

Embodiment 1

[0020] In the three-necked reaction flask, add toluene 100mL, silica gel 20g (average particle size is 2.5μm, average pore diameter is 10nm, specific surface area is 300m 2 / g), pyridine 4g, stirring to fully disperse and infiltrate the silica gel, add 6g of octadecyldimethylchlorosilane, react at 110°C, react for 12hr, and cool down; Wash with 50% methanol / water (v / v) and methanol; take out the solid and dry it in vacuum at 80°C for 12 hours to obtain 24g of the product. The carbon mass content of the product element analysis is 11%, and the calculated stationary phase bonding density is 1.77μmol / m 2 . The product is filled with a 4.6*50mm (diameter and height) column for detection. The detection method is: use 10mM ammonium formate aqueous solution as the mobile phase (without organic solvent), flow rate 1mL / min, and the sample is a mixture of cytosine, uracil and thymine , record the retention time t of thymine after injection 1 ; After the analysis, set the flow rate to...

Embodiment 2

[0022] According to Example 1, the difference is that the silica gel particle size used is 5 μm, the pore diameter is 10 nm, and the specific surface area is 300 m 2 / g; the silane is octyldimethylchlorosilane, and the silane dosage is 5g. Finally, 23g of the product is obtained, the carbon content of the product is 5.5%, and the calculated bonding density is 1.86 μmol / m 2 , and the percent change in thymine retention time was 1.5%.

Embodiment 3

[0024] According to Example 1, the difference is that the silica gel particle size used is 10 μm, the pore diameter is 10 nm, and the specific surface area is 300 m 2 / g; the silane is hexadecyltrimethoxysilane, the silane feed rate is 18g, the product is 24g, the product carbon content is 11%, and the calculated bonding density is 2.0μmol / m 2 , and the percent change in thymine retention time was 0.82%.

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Abstract

The invention discloses a pure water-resistant chromatographic stationary phase as well as a preparation method thereof. According to the stationary phase, silica gel is taken as a matrix and is bonded with alkyl C1-C30, and the bonding density is 1.0-2.5 micromole / m < 2 >. The preparation method of the stationary phase comprises the following steps of: dispersing silica gel in an organic solvent; adding an inorganic weak base or an organic base as a catalyst; adding silane according to the feeding amount of 0.2-1.0 g per gram of silica gel; performing a reaction at 50-150 DEG C for 3-24 hours; filtering reaction liquid; cleaning a filter cake with a reaction solvent, methanol, 30-70% methanol / water (v / v) and methanol in sequence; and drying an obtained solid at 50-80 DEG C under a vacuum condition for 6-24 hours to obtain the stationary phase product. By optimizing the surface bonding density of the stationary phase, the state of the surface bonding phase of the stationary phase is improved, and the pure water-resistant chromatographic stationary phase is obtained. According to the stationary phase and the preparation method thereof, the reaction conditions are mild, the steps are simple and feasible, and repeated and large-scale preparation is easy.

Description

technical field [0001] The invention relates to a chromatographic stationary phase and a preparation method thereof, in particular to a pure water-resistant reversed-phase chromatographic stationary phase and a preparation method thereof. Collapse". Background technique [0002] Reversed-phase chromatography is currently the most widely used chromatographic mode. For the separation of some compounds with strong polarity, it is often necessary to use high-proportion water phase or even pure water phase (only water as the solvent) chromatographic conditions. For ordinary reversed-phase chromatography stationary phases, the hydrophobic groups on the surface of the stationary phase will curl up under the condition of pure water phase, resulting in the rapid weakening of the sample retention of the stationary phase, that is, the problem of "hydrophobic collapse" of the stationary phase. At present, the methods to solve the hydrophobic collapse of the reversed-phase stationary ph...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/28B01J20/30B01D15/32G01N30/02
CPCB01J20/286B01J20/28083B01J20/28059B01J20/28061B01D15/325G01N30/02B01J2220/80B01J2220/52B01J2220/54B01J2220/4806B01J2220/4812
Inventor 梁鑫淼郭志谋金高娃丁俊杰
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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