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Preparation method for chitosamine hydrochloride and thin layer chromatography scanning detection method

A technology of glucosamine hydrochloride and thin-layer chromatography, applied in the field of preparation of glucosamine hydrochloride, to achieve the effects of increasing economic benefits, improving utilization rate, and enriching comprehensive utilization

Inactive Publication Date: 2015-05-27
SHANDONG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, if Antarctic krill is used as raw material to prepare glucosamine hydrochloride, it is an effective and resource-efficient method.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Example 1 Using Antarctic krill as raw material to prepare glucosamine hydrochloride and perform thin-layer chromatography scanning detection

[0031] The method is: take 5.01g of frozen Antarctic krill, put it into a beaker filled with 30ml of 95% ethanol, soak it for 5 hours, filter, then add the filter residue to a beaker filled with 30ml of 4% dilute hydrochloric acid, soak it for 10 hours, filter it, and wash the filter residue with water until neutral, put it into a conical flask filled with 30ml of 2% KOH solution, heat in a water bath at 80°C for 45 minutes, filter, wash the filter residue with water until neutral, put it into a beaker filled with 30ml of 4% dilute hydrochloric acid for 1.5h, filter, and filter the residue Wash with water until neutral, put it into a conical flask containing 30ml of 2% KOH solution again, heat and stir at a medium speed at 60°C on a constant temperature magnetic stirrer for 1h, obtain a white filter residue, put it into a 250ml c...

Embodiment 2

[0033] Example 2 Using Antarctic krill as raw material to prepare glucosamine hydrochloride and perform thin-layer chromatography scanning detection

[0034]Preparation and detection of glucosamine hydrochloride: Take 5.00g of frozen Antarctic krill, put it into a beaker with 40ml of 95% ethanol, soak for 4 hours, filter, put the filter residue into a triangular flask, add 40ml of distilled water, and use a constant temperature magnetic stirrer Stir at 40°C for 2 hours, filter, add the filter residue to 80ml of 5mol / L concentrated hydrochloric acid, connect the condensing reflux device, heat and acidify the filter residue at 105°C for 6.5 hours in a DHT type constant temperature heating and stirring device, and obtain the acid hydrolysis solution. Other subsequent operations are the same as in Example 1, but the developer is methanol-acetone-glacial acetic acid-water-isopropanol, and the volume ratio is 4:3.5:0.5:1:1.5. The migration value Rf of glucosamine hydrochloride is 0....

Embodiment 3

[0035] Example 3 Using Antarctic krill as raw material to prepare glucosamine hydrochloride and perform thin-layer chromatography scanning detection

[0036] Preparation and detection of glucosamine hydrochloride: Take 5.00g of frozen Antarctic krill, put it into a beaker filled with 40ml of 3% dilute hydrochloric acid, soak for 12h, filter, wash with water until neutral, and put the filter residue into a 40ml 1.5%KOH solution in a triangular flask medium, heated in a water bath at 85°C for 50 minutes, filtered, washed the filter residue with water until neutral, then soaked in a beaker filled with 40ml of 3% dilute hydrochloric acid for 2 hours, filtered, washed the filter residue with water until neutral, and put it into a triangle of 40ml of 1.5% KOH solution again. In the bottle, heat and stir at a medium speed at 70°C on a constant temperature magnetic stirrer for 1 hour to obtain a white filter residue; put the white filter residue into a 250ml Erlenmeyer flask, add 100ml...

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PUM

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Abstract

The invention discloses a thin layer chromatography scanning detection method for chitosamine hydrochloride. The method has the advantages of simplicity and convenience, quickness, accuracy, reliability and stability, and comprises the following steps: step (1), dripping sample liquid and standard liquid on a same efficient thin layer silica gel plate GF254, unfolding, and airing; step (2), spraying the acetone solution of aniline-diphenylamine-trichloroacetic acid on the efficient thin layer silica gel plate uniformly, or soaking the plate for 1 min, airing, and baking and dyeing; step (3), adopting a thin layer scanner to conduct thin layer chromatography scanning, so that the chitosamine hydrochloride RF and the peak area integral quantity are obtained; calculating the relationship between the standard liquid quality and the peak area integral quantity through thin layer chromatograph management software, and calculating the chitosamine hydrochloride content of the sample according to the peak area integral quantity of the sample liquid. The invention further discloses a method for preparing the chitosamine hydrochloride by adopting antarctic krill as a raw material through acidolysis, so that the comprehensive utilization of the antarctic krill is enriched, the utilization ratio is increased, and the economic benefit is increased.

Description

technical field [0001] The invention relates to a preparation method of glucosamine hydrochloride and a thin layer chromatography scanning detection method. Background technique [0002] Glucosamine hydrochloride, also known as glucosamine hydrochloride, molecular formula C 6 h 13 NO 5 HCl, it has important physiological functions to the human body, participates in liver and kidney detoxification, plays an anti-inflammatory and liver-protecting role, has a good curative effect on the treatment of rheumatoid arthritis and gastric ulcer, and is the main raw material for the synthesis of antibiotics and anticancer drugs. It can be used in chemical industry, food, cosmetics and feed additives. The main active ingredient of amino sugar capsule health products currently on the market is glucosamine hydrochloride or glucosamine sulfate, which can be obtained by high-temperature hydrolysis of chitin hydrochloride. Chitin is an important component of the shells of many lower anim...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/90C07H5/06C07H1/00
Inventor 蒋新英苏树朋刘代成
Owner SHANDONG NORMAL UNIV