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High purity full porous silica gel-bonded chromatography immobile phase preparation method

A chromatographic stationary phase, fully porous technology, applied in the application of high performance liquid chromatography packing, the preparation of new high-purity fully porous silica gel bonded chromatographic stationary phase, can solve the problem of reducing surface activity, not too high coverage, not capping reaction Complete and other problems, to achieve the effect of improving chromatographic separation performance, expanding the separation range, and widening the separation range

Inactive Publication Date: 2013-07-24
BEIJING UNIV OF CHEM TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Kirkland et al. reported that the acid treatment of the surface can increase the surface silanol density and reduce the surface activity to a certain extent, but it still cannot solve the problem of alkaline compound tailing caused by surface heterogeneity; Ohstu et al. used three The end-capping treatment of the bonded phase by methyl chlorosilane can effectively reduce the unreacted silanol groups when the coverage of the C18 or C8 phase is not too high, and many new reagents and new methods have been used for end-capping technology. Such as the high-temperature silanization end-capping technology reported by Sudo, etc., but due to steric hindrance, the end-capping reaction is not complete, so this method cannot completely eliminate the silanol group; A new method developed to stabilize the performance of silica gel at the pH value. Ohstu et al. prepared a polymer-coated C18 silica gel coating phase. Engelhardt et al. used vinyl trichlorosilane and acrylic acid derivative polymerization methods. Chang Jianhua et al. Coat a layer of polyamine, and then react with epoxy to prepare cladding phase. The stationary phase prepared by coating and curing has stable silica gel in the center and inhibits the activity of residual silanol groups. However, the coated polymeric layer must be very Thin, otherwise it will affect the mass transfer, which is technically difficult

Method used

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  • High purity full porous silica gel-bonded chromatography immobile phase preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0033] A. Take a certain amount of self-made high-purity porous spherical silica gel in a conical flask, add nitric acid with a volume fraction of 10% according to the ratio of 30ml nitric acid: 1g silica gel, perform suction filtration after ultrasonication for 1 hour, wash with water until neutral, and bake at 100°C dry reserve;

[0034] B. Take a certain amount of acidified silica gel in step A and add it to a reaction vessel with a condensing device, add dry toluene solvent at the ratio of 40ml toluene: 1g silica gel under constant stirring, heat and reflux at 110°C for 2 hours, then press 0.8 Add p-toluenesulfonic acid catalyst at the ratio of 1g p-toluenesulfonic acid: 1g silica gel, stir for 10 minutes, then add silylating agent according to the ratio of 0.2g octadecyldimethylmethoxysilane: 1g silica gel, heat and reflux for 9 hours , stop heating, cool under stirring for 30 minutes, wash with toluene and methanol in turn, and vacuum dry at 120°C for 10 hours for later ...

Embodiment 2

[0041] A. Take a certain amount of self-made high-purity porous spherical silica gel in a conical flask, add nitric acid with a volume fraction of 20% according to the ratio of 20ml nitric acid: 1g silica gel, perform suction filtration after ultrasonication for 1.5 hours, wash with water until neutral, and bake at 90°C dry reserve;

[0042] B. Take a certain amount of acidified silica gel in step A and add it to a reaction vessel with a condensing device, add dry toluene solvent at the ratio of 30ml toluene: 1g silica gel under constant stirring, heat and reflux at 110°C for 3 hours, press Add p-toluenesulfonic acid catalyst at the ratio of 0.5g p-toluenesulfonic acid: 1g silica gel, stir for 12 minutes, then add silylating agent according to the ratio of 0.15g octadecyldimethylmethoxysilane: 1g silica gel, heat to reflux for 8 hour, stop heating, stir and cool for 30 minutes, wash with toluene and methanol successively, and vacuum dry at 100°C for 11 hours for later use;

...

Embodiment 3

[0047] A. Take a certain amount of self-made high-purity porous spherical silica gel in a conical flask, add nitric acid with a volume fraction of 30% according to the ratio of 10ml nitric acid: 1g silica gel, perform suction filtration after ultrasonication for 1 hour, wash with water until neutral, and bake at 80°C dry reserve;

[0048] B. Take a certain amount of acidified silica gel in step A and add it to a reaction vessel with a condensing device, add dry toluene solvent at the ratio of 20ml toluene: 1g silica gel under constant stirring, heat and reflux at 110°C for 4 hours, then press 0.3 Add p-toluenesulfonic acid catalyst at the ratio of 1g p-toluenesulfonic acid: 1g silica gel, stir for 15 minutes, then add silylating agent according to the ratio of 0.1g octadecyldimethylmethoxysilane: 1g silica gel, heat and reflux for 9 hours , stop heating, cool under stirring for 30 minutes, wash with toluene and methanol in turn, and vacuum dry at 80°C for 12 hours for later us...

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Abstract

The invention relates to a high purity full porous silica gel-bonded chromatography immobile phase preparation method, and belongs to the technical field of high-performance liquid chromatography packing preparation. According to the preparation method, a self-made high purity porous spherical silica gel is adopted as a raw material, and surface activation and other pre-treatments are performed on the silica gel, such that the surface of the porous silica gel microspheres presents low activity, low acidity and good uniformity; and octadecyldimethylmethoxysilane is bonded on the surface of the activated silica gel, then a linkage effect of a silane coupling agent gamma-aminopropyltriethoxysilane (KH550) is adopted to bond methyl iodide to the surface of the silica gel, and finally trimethylchlorosilane is adopted to carry out an end capping treatment to obtain the full porous silica gel-bonded chromatography immobile phase. With the method, a chromatography separation performance of the bonded silica gel packing can be improved, such that the immobile phase has advantages of rapid separation, good peak shape, wide separation range, and the like.

Description

technical field [0001] The invention belongs to the technical field of preparation of high-performance liquid chromatography packing, and relates to a preparation method of a novel high-purity fully porous silica gel bonded chromatography stationary phase and its application as a high-performance liquid chromatography packing. Background technique [0002] Commercial chromatographic fillers such as silica gel, bonded silica gel, alumina, organic polymer microspheres (including ion exchange resins), porous carbon, etc., the particle size is generally 3-10um, etc., and the theoretical column efficiency can reach 1-160,000 plates. / rice. Among them, the silica gel material is currently the most widely used chromatographic packing material due to its advantages such as good mechanical strength and easy surface modification as mentioned above. However, traditional silica gel reversed-phase column packings based on mineral raw materials contain a certain amount of metal impuritie...

Claims

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Application Information

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IPC IPC(8): B01J20/283B01J20/286B01J20/30B01J20/281
Inventor 杨俊佼刘丽娜
Owner BEIJING UNIV OF CHEM TECH
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