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Method of recovering effective components from potassium clavulanate mixed powder

A technology described from potassium clavulanate and potassium clavulanate, which is applied in the field of recycling active ingredients, can solve problems such as unqualified products and economic losses, and achieve the effects of low cost, simple process and high yield

Inactive Publication Date: 2014-06-04
SHANDONG NEWTIME PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the extreme instability of potassium clavulanate, during the production and storage of mixed powder, unqualified products may appear due to operational errors, improper storage, etc., resulting in serious economic losses
At present, there is no research report on the recovery of active ingredients from potassium clavulanate mixed powder

Method used

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  • Method of recovering effective components from potassium clavulanate mixed powder
  • Method of recovering effective components from potassium clavulanate mixed powder
  • Method of recovering effective components from potassium clavulanate mixed powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Take unqualified potassium clavulanate: silicon dioxide (1:1) mixed powder 200g, add 100mL purified water at 5°C, adjust pH to 5.0 with 15% acetic acid, stir to dissolve, filter to obtain clavulanate Aqueous solution of potassium phosphate and undissolved silica solid. The aqueous solution of potassium clavulanate is decolorized with 8g of activated carbon at 20°C, wherein the activated carbon is mixed with 767 type and 302 type according to the weight ratio of 2:1. In the decolorized potassium clavulanate aqueous solution, slowly add 20 times isopropanol for crystallization, the temperature is controlled at 0° C., and the crystal is grown with slow stirring for 2 hours. The crystallization solution was filtered, the crystals were washed three times with acetone, and vacuum-dried at 20°C to obtain 68.01 g of potassium clavulanate with a yield of 71.08%. Undissolved silica solids are not recovered due to their low economic value.

Embodiment 2

[0028] Take unqualified potassium clavulanate: microcrystalline cellulose (1:1) mixed powder 200g, add 50mL purified water at 20°C, adjust pH to 4.5 with 18% sulfuric acid, stir to dissolve, filter to obtain clavulanate Aqueous solution of potassium phosphate and undissolved microcrystalline cellulose solids. The aqueous solution of potassium clavulanate was decolorized with 12 g of 767 activated carbon at a temperature of 0°C. In the decolorized potassium clavulanate aqueous solution, slowly add 40 times of isopropanol for crystallization, the temperature is controlled at 5° C., and the crystal is grown with slow stirring for 2 hours. The crystallization solution was filtered, the crystals were washed three times with acetone, and vacuum-dried at 30°C to obtain 72.25 g of potassium clavulanate, with a yield of 76.00%. Undissolved microcrystalline cellulose solids are not recovered due to their low economic value.

Embodiment 3

[0030] Take unqualified amoxicillin: potassium clavulanate (2:1) mixed powder 200g, add 32mL purified water at 10°C, adjust pH 6.0 with 5% hydrochloric acid, stir to dissolve, filter to obtain clavulanic acid Aqueous solution of potassium and undissolved amoxicillin solid. The aqueous solution of potassium clavulanate is decolorized with 4g of activated carbon at 2°C, and the activated carbon is mixed with 772 type and 732 type according to the weight ratio of 1:1. In the decolorized potassium clavulanate aqueous solution, 45 times of acetone was slowly added for crystallization, the temperature was controlled at 3° C., and the crystal was grown with slow stirring for 2 hours. The crystallization solution was filtered, the crystals were washed three times with acetone, and vacuum-dried at 35°C to obtain 53.16 g of potassium clavulanate, with a yield of 78.02%. The undissolved amoxicillin solid was washed three times with 9.6 L of purified water, and then vacuum-dried at 50°C ...

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Abstract

The invention relates to a method of recovering effective components from potassium clavulanate mixed powder. The method comprises the following steps: dissolving potassium clavulanate in the mixed powder by purified water according to different solubilities of various effective components in the mixed powder; initially separating as other components are insoluble; and further purifying to obtain the effective components such as potassium clavulanate which satisfies the requirements of pharmacopeia. The invention creatively develops the novel method of recovering effective components from potassium clavulanate mixed powder and can be used for recovering effective components such as potassium clavulanate from unqualified potassium clavulanate mixed powder so as to turn waste into wealth, thereby satisfying the requirements on green production and circulating economy. Meanwhile, the method is simple in process, high in yield and low in cost, and has high practical and economic values.

Description

technical field [0001] The invention belongs to the field of pharmaceutical industry and relates to a method for recovering active ingredients from potassium clavulanate mixed powder. Background technique [0002] The chemical name of clavulanic acid is (2R,5R,Z)-3-(2-Hydroxyethylidene)-7-oxo-4-oxa-1-azabicyclo[3.2.0]heptane- 2-Carboxylic acid, the structure is as follows: [0003] [0004] Potassium salt of clavulanic acid is currently the most widely used β-lactamase inhibitor, which can increase the antibacterial effect several times or even dozens of times. With the increasing clinical bacterial resistance, its application is becoming more and more extensive. [0005] In the production of potassium clavulanate, it is usually produced, stored and sold in the form of mixed powder, such as potassium clavulanate: silicon dioxide (1:1), potassium clavulanate: microcrystalline cellulose (1:1 ), Amoxicillin: Potassium Clavulanate (2:1), Amoxicillin: Potassium Clavulanate ...

Claims

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Application Information

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IPC IPC(8): C07D503/18C07D503/02
CPCC07D503/18C07D499/18C07D499/68C07D503/02
Inventor 靳孝庆隋华芹
Owner SHANDONG NEWTIME PHARMA
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