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Preparation method of cross-linking sodium carboxymethylcellulose pharmaceutical adjuvant

A technology of sodium carboxymethyl cellulose and cross-linked carboxymethyl, which is applied in the field of preparation of cross-linked sodium carboxymethyl cellulose pharmaceutical excipients, can solve the problem of lack of regulation and control of the degree of substitution of cross-linked sodium carboxymethyl cellulose. Conformity and other problems, to achieve the effect of mild reaction solvent, avoid hydrolysis, and controllable cross-linking degree

Active Publication Date: 2013-04-24
HUBEI GEDIAN HUMANWELL PHARMA EXCIPENTS
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the patent CN 101475696A and the patent CN 102093579A mentioned the degree of substitution of croscarmellose sodium, the degree of substitution of the target product croscarmellose sodium prepared by it was also specifically detected, but from its specific value It can be seen that the degree of substitution of some of its products has even reached above 0.90, which does not meet the requirements of Chinese medicinal excipients in the Pharmacopoeia, and there is no relevant report on the regulation of the degree of substitution of croscarmellose sodium in this patent

Method used

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  • Preparation method of cross-linking sodium carboxymethylcellulose pharmaceutical adjuvant

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Effect test

Embodiment 1

[0025] In a 250ml round bottom flask equipped with a condenser tube and a thermometer, add 67g of ethanol 75wt% as a dispersant, start stirring, then slowly add 10g of sodium carboxymethylcellulose with a degree of substitution of 0.80, after the addition is complete, to obtain The ethanol dispersion of sodium carboxymethyl cellulose is then heated to 40°C, and the pH value of the system is adjusted to 13 with 20wt% sodium hydroxide solution, and the stirring is continued for 30 minutes until the system is uniformly dispersed, and then the mass fraction is added dropwise while stirring It is 5 g of 20% epichlorohydrin ethanol solution, and the temperature is kept at 40 ° C, and the reaction is stirred for 5.5 h. After the reaction, neutralize to neutral with 36wt% acetic acid, and filter with suction. The suction-filtered product was washed twice with 75 wt% ethanol, suction-filtered, dried at 65°C, pulverized, and sieved to obtain croscarmellose sodium powder.

Embodiment 2

[0027] In a 250ml round bottom flask equipped with a condenser tube and a thermometer, add 67g of ethanol 75wt% as a dispersant, start stirring, then slowly add 10g of sodium carboxymethylcellulose with a degree of substitution of 0.80, after the addition is complete, to obtain Ethanol dispersion of sodium carboxymethyl cellulose, then warm up to 40°C, adjust the pH value of the system to 13 with sodium hydroxide solution, continue stirring for 30 minutes until the system is evenly dispersed, then add dropwise with a mass fraction of 20% while stirring The ethanol solution of epichlorohydrin was 6 g, the temperature was kept at 40° C., and the reaction was stirred for 5.5 h. After the reaction, neutralize to neutral with acetic acid, and filter with suction. The suction-filtered product was washed twice with ethanol aqueous solution, suction-filtered, dried at 90°C, pulverized, and sieved to obtain croscarmellose sodium powder.

Embodiment 3

[0028] Embodiment 3 is basically the same as Embodiment 1, but has the following changes:

[0029] Described dispersion agent is isopropanol aqueous solution, and wherein the massfraction of isopropanol is 55%, and the mass ratio of the quality of sodium carboxymethyl cellulose and isopropanol aqueous solution is 1:4;

[0030] Described basic catalyst is potassium hydroxide;

[0031] The massfraction that is added dropwise is the quality of the ethanol solution of 40% epichlorohydrin is 4g;

[0032] The mass fraction of the aqueous ethanol solution used for washing is 50%.

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Abstract

The invention relates to a preparation method of a cross-linking sodium carboxymethylcellulose pharmaceutical adjuvant. The method comprises the following steps: firstly, adjusting the pH value of a dispersion liquid of sodium carboxymethylcellulose with degree of substitution of 0.65-0.80 by a degree of substitution adjusting system to 10-14; continuously stirring till the system is uniformly dispersed; then, stirring and adding an ethanol liquid of epoxy chloropropane as a cross-linking agent, wherein epoxy chloropropane in the ethanol liquid of epoxy chloropropane accounts for 6-40wt% of ethanol liquid of epoxy chloropropane; stirring at 10-60 DEG C and reacting for 2-12 hours; after reaction, adding acid to neutralize; filtering, washing and drying; and smashing and sieving to obtain the cross-linking sodium carboxymethylcellulose, wherein the physicochemical properties of the cross-linking sodium carboxymethylcellulose meet the Chinese pharmacopoeia (2) (2010 Edition). The reaction condition is mild, the degree of crosslinking is controllable, the reaction solvent is mild, and no residual organic solvents are left after reaction. In cross-linking reaction under a cross-linking reaction, sodium carboxymethylcellulose is prevented from being hydrolyzed.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a preparation method of croscarmellose sodium pharmaceutical excipients. Background technique [0002] Sodium carboxymethyl cellulose was first produced in Germany in 1918, and it was patented in 1921 and came to the world. Compared with sodium carboxymethyl cellulose, croscarmellose sodium can swell rapidly when it meets water, has a good disintegration effect, and can make the drug disintegrate and dissolve quickly. Together with crospovidone, croscarmellose sodium starch and low-substituted hydroxypropyl cellulose, it is called the four super disintegrants. [0003] At present, there are generally two methods for preparing croscarmellose sodium: one is to carry out self-crosslinking of carboxymethyl cellulose sodium at high temperature or dissolved in a certain solvent; After sodium cellulose is dispersed in a solvent, it is cross-linked under the action of a cr...

Claims

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Application Information

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IPC IPC(8): C08J3/24C08L1/26C08K5/1515A61K47/38
Inventor 张阳洋李娟曾诚
Owner HUBEI GEDIAN HUMANWELL PHARMA EXCIPENTS
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