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High substitution degree carboxymethyl indianbread polysaccharide and its preparation method and uses

A Poria cocos polysaccharide technology with a high degree of substitution is applied to metabolic diseases, medical formulas, medical preparations of non-active ingredients, etc. It can solve the problems of limiting the clinical application range of CMP, difficult separation and removal of impurities, and difficult industrial production, etc. Environmental protection, shortening of reaction time, and improvement of solubility

Active Publication Date: 2007-05-30
HUNAN BUTIAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Hamuro et al. (1971) used isopropanol and water as the medium to synthesize CMP under liquid-solid phase oscillation conditions. Because of the need for large-scale oscillation equipment, it was difficult to carry out industrial production, and a large amount of organic solvents (such as ether, methyl alcohol) were required , acetone, acetic acid and ethanol) to carry out post-treatment and purification of CMP, not only the production cost is higher, but also cause environmental pollution
[0005] Shi Qingdong et al. (1996) used ethanol and water as the medium to replace and prepare CMP under liquid-solid phase stirring conditions. The carboxymethyl substitution degree (D S) of the obtained CMP was 0.92, showing that the solubility of the product was small , the impurity content is relatively high, in terms of NaCl, the chloride content is less than 3.0%; in terms of P b Calculated, heavy metal %<0.002%, and it is difficult to separate and remove contained impurities, which greatly limits the scope of clinical application of CMP, such as the CMP prepared by this method cannot be used to prepare injections

Method used

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  • High substitution degree carboxymethyl indianbread polysaccharide and its preparation method and uses
  • High substitution degree carboxymethyl indianbread polysaccharide and its preparation method and uses
  • High substitution degree carboxymethyl indianbread polysaccharide and its preparation method and uses

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0092] Example 1 Preparation of CMP with high degree of substitution

[0093] High degree of substitution CMP is prepared by the following method:

[0094] 1) 75 kg of dried poria cocos, crushed into fine powder, put into a soaking tank, pumped into 400L of water, stirred evenly, and soaked for 12 hours;

[0095] 2) Slowly pump 400L of sodium hydroxide solution with a concentration of 2.25mol / L into the soaking tank, stir and react for 1h, filter, and take the filtrate;

[0096]3) Add 300 L of chloroacetic acid solution with a concentration of 5.3 mol / L into the neutralization tank, then slowly add 300 L of sodium hydroxide solution with a concentration of 6.25 mol / L, stir until the reaction is sufficient, and cool to room temperature;

[0097] 4) Pump the reaction solution in step 3) into the filtrate obtained in step 2), mix well, then slowly raise the temperature to 75°C, and react at constant temperature for 2.5 hours;

[0098] 5) Use 6mol / L hydrochloric acid solutio...

Embodiment 2

[0111] Example 2 Determination of Molecular Weight of Carboxymethyl Pachyranan

[0112] Determination conditions: the instrument is LKB column chromatography system, SephadexG-200 column. The mobile phase is 0.2mol / L NaCl solution (pH 7.0) buffer solution, the flow rate is 0.5ml / min, the injection volume (W / V) is 1mg / ml, and the constant temperature is 10°C. Differential refraction is automatically detected, and the recorder records the peak position.

[0113] Standard curve: use standard polysaccharides Dexfran T2000 (Mw2000000), T500 (Mw500000), T40 (Mw40000), T20 (Mw20000), T10 (Mw10000), T5 (Mw5000) with known molecular weight to make a standard curve, according to Ka.v logarithm Log Mw plotted, the standard curve is shown in Figure 1.

[0114] The elution curve of the carboxymethylpachyran that the present invention makes on the SephadexG-200 chromatographic column is referring to Fig. 2, according to the Ka.v value that records, obtains its molecular weight (Mw) to...

Embodiment 3

[0116] Example 3 Determination of Carboxymethyl Substitution Degree (D·S) of Carboxymethylpachyan by Acidification Method

[0117] Precisely weigh 0.4041g of carboxymethylpachyran sample, put it in a 150ml beaker, heat in a water bath at 80°C, stir to dissolve, after cooling, adjust the pH to 4.0 with 2mol / L hydrochloric acid solution, add 100ml of absolute ethanol, stir Evenly, let it stand overnight, centrifuge to separate the alcoholate, and wash the alcoholate repeatedly with 95% ethanol until the washing liquid does not contain chloride ions. Wash the alcohol analyte and dissolve it with 40.00ml of 0.1000mol / L NaoH standard solution. After the solution becomes transparent, immediately use 0.1000mol / L standard hydrochloric acid solution for back titration until the red color of the phenolphthalein indicator just fades away, record the back titration The volume of the consumed 0.1000mol / L hydrochloric acid standard solution is 21.60ml.

[0118] Calculate the degree of ...

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Abstract

The invention discloses a carboxymethyl pachyman (CMP) with high-degree of substitution and making method and application, which is characterized by the following: adopting water or water alcohol solution as dielectric; proceeding substitution reaction for pachyman, chloroacetic acid and fitful excessive sodium hydroxide to obtain CMP without vibrating technique and equipment; improving CMP D / S and solubility to reach injection need.

Description

technical field [0001] The invention belongs to the field of anti-tumor macromolecule polysaccharides, and in particular relates to carboxymethylpachymaran (CMP) with a high degree of carboxymethyl substitution as a biological response regulator, a preparation method and an application thereof. Background technique [0002] Poria cocos is the dry sclerotia of Poria cocos (Schw.) Wolf, a plant of Polyporaceae. It has been one of the "four monarchs and eight treasures" of traditional Chinese medicine since ancient times. The component pachyan has a β(1→3)-bonded glucose linear structure and a β(1→6)-bonded glucosyl branched structure. Tests have shown that Poria cocos polysaccharide without chemical modification has no anti-tumor activity, and the decoction yield of Poria cocos in boiling water does not exceed 1%. The chemically modified carboxymethylpachypolysaccharide (CMP) obviously improves the water solubility of the polysaccharide, which is beneficial to the absorption ...

Claims

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Application Information

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IPC IPC(8): C08B37/00A61K31/715A61K47/36A61P37/04A61P35/00A61P3/06A61P3/10A61P39/06A61P1/16A61P31/12A61P31/04
Inventor 陈春霞
Owner HUNAN BUTIAN PHARMA
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