Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method of potassium clavulanate/microcrystalline cellulose composition

A technology of microcrystalline cellulose and potassium clavulanate, which is applied in the direction of drug combinations, medical preparations containing no active ingredients, medical preparations containing active ingredients, etc., can solve problems such as complex production process and dust explosion, and achieve The effect of short process route, avoiding dust explosion and improving safety

Active Publication Date: 2011-05-18
石药集团中诺药业(石家庄)有限公司
View PDF1 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the production process of this product is complex, with the characteristics of inflammability, explosion and continuity of the production process, dust explosion will occur during the mixing process, and there are serious safety hazards

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] ① Preparation of intermediate - tert-butylamine clavulanate powder

[0017] The pH of the clavulanic acid-ethyl acetate solution was adjusted to 5.0 with an aqueous solution of tert-butylamine, then the clavulanic acid was back-extracted from the ethyl acetate phase to the water phase, and then crystallized with acetone to prepare the clavulanic acid tert-butylamine powder.

[0018] Use HPLC (high performance liquid chromatography) to detect the content of tert-butylamine clavulanate in tert-butylamine clavulanate powder: Take 10-20 mg of tert-butylamine clavulanate powder, fully dissolve it in 80 mL of purified water, and dilute to 100 mL. Sampling was detected by HPLC, and the initial peak area of ​​potassium clavulanate was recorded.

[0019] HPLC detection conditions

[0020] Chromatographic column: C18 5μm, 250×4.6mm;

[0021] Mobile phase: 75mmol / L sodium dihydrogen phosphate buffer with pH 4.4: acetonitrile=950:50, flow rate 0.8ml / min;

[0022] Detection wavel...

Embodiment 2

[0041] The preparation method of clavulanic acid tert-butylamine powder is the same as embodiment one.

[0042] Potassium clavulanate / microcrystalline cellulose compositions were then prepared as follows.

[0043] ①Take 20g of clavulanic acid tert-butylamine powder and put it into 500mL reactor I, then add 70mL of isopropanol and 2.5mL of purified water to reactor I in sequence, mix well, slowly add glacial acetic acid with a weight content of 80%, adjust pH to 6.2, the temperature is controlled at 28-30°C to prepare clavulanic acid tert-butylamine-isopropanol solution;

[0044] ②Weigh 13g of potassium isooctanoate and dissolve it in 52mL of isopropanol to prepare potassium isooctanoate-isopropanol solution;

[0045] ③The potassium isooctanoate-isopropanol solution in step ② is slowly added dropwise to the clavulanic acid tert-butylamine-isopropanol solution in step ①, after the addition is completed, a large amount of crystals are precipitated, and the temperature is lowered...

Embodiment 3

[0049] ① Take 40 g of clavulanic acid tert-butylamine with a mass content of 78% in Example 1, put it into 1000 mL of reactor I, then add 140 mL of isopropanol and 5.0 mL of purified water to reactor I, mix well, and slowly add weight Glacial acetic acid with a content of 80%, adjust the pH to 6.0, and control the temperature at 28-30°C to prepare clavulanic acid tert-butylamine-isopropanol solution;

[0050] ② Dissolve 26g of potassium isooctanoate in 130mL of isopropanol to prepare a potassium isooctanoate-isopropanol solution;

[0051] ③The potassium isooctanoate-isopropanol solution in step ② is slowly added dropwise to the clavulanic acid tert-butylamine-isopropanol solution in step ①. After the addition is completed, a large number of crystals are complete, and the temperature is lowered to 2-5°C to obtain carat Potassium tretinoin-isopropanol solution;

[0052] ④ Before crystal growth, add 26 g of microcrystalline cellulose to the potassium clavulanate-isopropanol soluti...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a preparation method of a potassium clavulanate / microcrystalline cellulose composition, belonging to the preparation field of pharmaceutical raw materials. The preparation method of the invention comprises the following steps of: dissolving clavulanic tert-butylamine powder as a raw material in an isopropyl alcohol solution to prepare a clavulanic tert-butylamine-isopropyl alcohol solution; then, dipping a potassium ethylhexanoate-isopropyl alcohol solution to the clavulanic tert-butylamine-isopropyl alcohol solution until complete crystallization is finished; then, adding microcrystalline cellulose powder in 60-70 percent by weight of the clavulanic tert-butylamine powder; and finally, carrying out suction filtration, washing and drying to obtain the potassium clavulanate / microcrystalline cellulose composition. The adopted preparation method of the invention has low cost, high safety factor and short process flows and is suitable for mass production.

Description

technical field [0001] The invention relates to a preparation method of pharmaceutical raw materials, in particular to a preparation method of potassium clavulanate / microcrystalline cellulose composition. Background technique [0002] Clavulanic Acid (Clavulanic Acid), also known as clavulanic acid, is a β-lactamase inhibitor, which has a strong broad-spectrum inhibitory effect on β-lactamase produced by drug-resistant bacteria. After the combination of cillin, it can protect amoxicillin from being inactivated by β-lactamase and exert its bactericidal effect. Potassium clavulanate and microcrystalline cellulose are the main components of anti-inflammatory drugs for cardiovascular diseases. With the widespread use of antibiotics, bacterial drug resistance (MDR) is also generally enhanced, and drug-resistant bacteria are widely spread. Therefore, clavulanic acid The market demand for compound preparations continues to increase. [0003] At present, the method for preparing p...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): A61K31/424A61K47/38A61P31/04A61P9/00
Inventor 袁国强康辉陈雅洁李宁赵静
Owner 石药集团中诺药业(石家庄)有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com