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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: 2014-05-28
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 Preparation of glucosamine hydrochloride with Antarctic krill as raw material and thin-layer chromatography scanning detection

[0031] The method is: take 5.01g of frozen Antarctic krill, put it in a beaker with 30ml of 95% ethanol, soak for 5h, filter, then add the filter residue to a beaker containing 30ml of 4% dilute hydrochloric acid, soak for 10h, filter, and wash the filter residue with water To neutrality, put it into an Erlenmeyer flask containing 30ml 2% KOH solution, heat in a water bath at 80°C for 45 min, filter, wash the filter residue to neutrality, and then put it in a beaker containing 30ml 4% dilute hydrochloric acid for 1.5 hours, filter, filter residue Wash with water until it is neutral, put it again in a triangular flask containing 30ml of 2% KOH solution, heat it on a thermostatic magnetic stirrer at 60℃ and stir at medium speed for 1 hour to obtain a white filter residue, put it into a 250ml triangular flask, and add 100ml of 6mol / L Conce...

Embodiment 2

[0033] Example 2 Preparation of glucosamine hydrochloride using Antarctic krill as raw material and scanning detection by thin layer chromatography

[0034] Preparation and detection of glucosamine hydrochloride: Take 5.00g of frozen Antarctic krill, put it in a beaker containing 40ml of 95% ethanol, soak for 4h, filter, put the filter residue into a triangular flask, add 40ml of distilled water, and use a thermostatic magnetic stirrer Stir at 40°C for 2h, filter, add the filter residue to 80ml of 5mol / L concentrated hydrochloric acid, connect the reflux device, and heat the filter residue at 105°C for 6.5h to obtain the acid hydrolyzed solution. The other subsequent operations are the same as in Example 1, but the developing agent 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 0.66. After detection and calculation, the mass of glucosamine hydrochloride obtained from acid h...

Embodiment 3

[0035] Example 3 Preparation of glucosamine hydrochloride with Antarctic krill as raw material and thin-layer chromatography scanning detection

[0036] Preparation and detection of glucosamine hydrochloride: Take 5.00g of frozen Antarctic krill, put it in a beaker containing 40ml of 3% dilute hydrochloric acid, soak for 12h, filter, wash with water until neutral, and put the filter residue into a 40ml flask of 1.5% KOH Heat in a water bath at 85°C for 50 minutes, filter, and wash the filter residue with water until it is neutral, then put it in a beaker containing 40ml 3% dilute hydrochloric acid and soak for 2h, filter, wash the filter residue with water until it is neutral, and put it in a triangle with 40ml 1.5% KOH solution again. In the bottle, heat at 70°C with 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 6mol / L concentrated hydrochloric acid, connect to the condens...

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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, which has important physiological functions to the human body, participates in liver and kidney detoxification, plays an anti-inflammatory and liver protection effect, has a good curative effect on the treatment of rheumatoid joint inflammation and gastric ulcer, and is the main raw material for the synthesis of antibiotics and anticancer drugs. It can be used in chemicals, food, cosmetics and feed additives. The main active ingredient of the amino sugar capsule health care products currently on the market is glucosamine hydrochloride or glucosamine sulfate, which can be prepared by high-temperature hydrolysis of chitin with hydrochloric acid. Chitin is an important component of the shells o...

Claims

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Application Information

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