Chitosan bonded organic-silica gel hybridization monolithic column and preparation method thereof

A technology of silica gel hybridization and chitosan, applied in the chemical field, can solve the problems of cumbersome operation, difficult determination of the end point, and difficult control of titration conditions, etc., and achieve the effect of good biocompatibility and strong specific surface interaction

Inactive Publication Date: 2015-05-13
INSPECTION & QUARANTINE TECH CENT OF XIAMEN ENTRY EXIT INSPECTION & QUARANTINE BUREAU +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The chemical analysis method recommended in the current standards for sugar detection is the Rein-Enon method (GB 5413.5-2010). Because the titration conditions are not easy to control and the end point is not e

Method used

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  • Chitosan bonded organic-silica gel hybridization monolithic column and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Example 1: Preparation of chitosan-bonded organic-silica gel hybrid monolithic column

[0036]The mass ratio of acrylamide, methyl methacrylate-based cage polysilsesquioxane (Methacryl POSS? Cage Mixture), azobisisobutyronitrile initiator, toluene, and dodecanol mixed porogen is respectively according to The following data preparation: acrylamide 24.0%, methyl methacrylate cage polysilsesquioxane 6.0%, lauryl alcohol 44%, toluene 25%, azobisisobutyronitrile 1.0%. The mixture was ultrasonically treated at room temperature for 15 min in a nitrogen atmosphere, and the ultrasonically treated polymerization solution was evenly injected into a vinyl-derivatized quartz capillary, and both ends of the capillary were sealed, and immersed in a water bath at 60°C for 12 h; after the reaction was completed, , the resulting monolithic column was opened with methanol at a pressure of 20Mpa, and the resulting monolithic column was washed with methanol at a flow rate of 0.10 mL / min for...

Embodiment 2

[0037] Example 2: Application of chitosan-bonded organic-silica gel hybrid monolithic column

[0038] The chitosan-bonded organic-silica hybrid monolithic column prepared above (inner diameter 100 microns, total length 55.0 cm, effective length 30 cm) was used, pH 6.0, 30 mM phosphate buffer was used as the mobile phase, and the column pressure was 1000 psi. Auxiliary separation voltage +16kV, under capillary electrochromatography CEC cathodic electroosmotic flow mode, the protoopiate polar substances are separated. The elution peaks were: 1. berberine hydrochloride, 2. protoopiine, 3. tetrahydropalmatine, and the baseline separation was achieved under the above conditions.

Embodiment 3

[0039] Example 3: Application of chitosan-bonded organic-silica gel hybrid monolithic column

[0040] The chitosan-bonded organic-silica hybrid monolithic column prepared above was used, and acetonitrile-ammonium formate (pH 4.0, 10mM)=70:30 (volume ratio) solution was used as the mobile phase, the flow rate was 0.10 mL / min, and the column pressure was 1000 psi, auxiliary separation voltage +10 kV, column temperature 25°C, and micro-column chromatography-ultraviolet (detection wavelength 200 nm) detection mode, to separate carbohydrates, such as figure 1 As shown, glucose (1) and maltose (2) were well separated.

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Abstract

The invention discloses a chitosan bonded organic-silica gel hybridization monolithic column and a preparation method thereof. The chitosan bonded organic-silica gel hybridization monolithic column is prepared by combining the following components in percentage by mass with chitosan: 24% of a functional monomer with an amide group, 6% of a cage-like polysilsesquioxane cross-linking agent, 1.0% of an initiator and 69.0% of a pore-foaming agent. The invention further provides a preparation method of the chitosan bonded organic-silica gel hybridization monolithic column. The chitosan bonded organic-silica gel hybridization monolithic column disclosed by the invention has a nano cage-like siloxane structure, and is high in specific surface function and biocompatibility, and rich in hydroxyl and amino due to post-column bonded chitosan so as to provide abundant hydrogen bonds and perform hydrophilic interaction, thereby being applicable to analysis and separation of carbohydrates such as monosaccharide and disaccharide with high hydrophilcity.

Description

technical field [0001] The invention relates to the field of chemistry, in particular to a chitosan-bonded organic-silica gel hybrid integral column and a preparation method thereof. Background technique [0002] Sugar is the main carbohydrate in raw milk. Sugars such as monosaccharides and disaccharides play an important role in the formation of the nervous system, skin texture, and bones. For example, digested lactose can promote the formation of cerebrosides and mucopolysaccharides. Generation is crucial for the development of the infant brain. The quality control of carbohydrates in raw milk and dairy products is of great significance. [0003] At present, the determination methods of sugars such as monosaccharides and disaccharides mainly include enzymatic method, direct titration method, direct colorimetric method, near-infrared spectroscopy, optical rotation method, high performance liquid chromatography, capillary electrophoresis, etc. The chemical analysis method ...

Claims

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Application Information

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IPC IPC(8): B01D15/22B01J20/24B01J20/30B01J20/281G01N30/06
Inventor 郑向华龚吉军徐敦明周昱黄志强
Owner INSPECTION & QUARANTINE TECH CENT OF XIAMEN ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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