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Purification method of cefotiam hydrochloride and aseptic powder injection of cefotiam hydrochloride

A technology of cefotiam hydrochloride and sterile powder injection, which is applied in the field of cefotiam hydrochloride sterile powder injection and cefotiam hydrochloride purification, can solve the problems of acetone solvent exceeding the standard and cefotiam hydrochloride acetone exceeding the standard, and achieve low Organic residues, solution to excessive acetone, high yield

Active Publication Date: 2012-10-24
HAINAN JINXING PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] The purification method of cefotiam hydrochloride reported at present mainly utilizes the method for water-acetone recrystallization, but the cefotiam hydrochloride that utilizes this method to make easily causes the acetone solvent in the crude drug to exceed the standard
According to the technical guidelines for the research on residual solvents in chemical drugs issued by the State Food and Drug Administration, it is stipulated that the residual amount of acetone should not exceed the limit of 0.5% when the finished product is dried, and the crystals obtained by recrystallization with water-acetone are obtained by vacuum drying. All cefotiam hydrochloride has the problem of excessive acetone, and the content of acetone is generally in the range of 1.5-3.7%, seriously exceeding the limit stipulated in the Pharmacopoeia

Method used

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  • Purification method of cefotiam hydrochloride and aseptic powder injection of cefotiam hydrochloride
  • Purification method of cefotiam hydrochloride and aseptic powder injection of cefotiam hydrochloride
  • Purification method of cefotiam hydrochloride and aseptic powder injection of cefotiam hydrochloride

Examples

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Embodiment 1

[0051] Example 1 Purification of Cefotiam Hydrochloride Crude Product, Preparation of Cefotiam Hydrochloride Sterile Powder Injection

[0052] Weigh 500g of crude cefotiam hydrochloride with a purity of 92.1% (which contains impurities 7-ACA, DMMT, 7-ATA-HACA, and 7-DMT) and add it to the reaction kettle, add 1L of water to dissolve it, and then add 2.0g of activated carbon for injection , heated to 50°C, and filtered after 30 minutes; after filtration, take the obtained filtrate, add 3L of acetone, heat and stir to dissolve, and use a 0.22μm microporous membrane to filter under positive pressure at a temperature below 0.1Mpa; freeze the filtrate to 0°C, and Low-temperature crystallization for 2 hours, after the crystallization is completed, filter; put the obtained crystals into a crystallization tank, add 1.5L of methyl tert-butyl ether for beating and washing, and suction filter to obtain white crystals; then pour water into the white crystals Saturated with nitrogen, after...

Embodiment 2

[0060] Example 2 Purification of Cefotiam Hydrochloride Crude Product, Preparation of Cefotiam Hydrochloride Sterile Powder Injection

[0061] Weigh 500g of crude cefotiam hydrochloride with a purity of 92.1% (which contains impurities 7-ACA, DMMT, 7-ATA-HACA, and 7-DMT) and add it to the reaction kettle, add 0.5L of water to dissolve, add 3.0g for injection Activated carbon, heated to 60°C, and filtered after 30 minutes; take the obtained filtrate, add 2L acetone, heat and stir to dissolve, and use a 0.22μm microporous filter membrane to filter under positive pressure below 0.1Mpa; freeze the filtrate to 0°C, and cool Crystallize for 2 hours, after the crystallization is completed, filter; put the obtained crystals into a crystallization tank, add 2L of ether for beating and washing, and filter with suction to obtain white crystals; then pass water-saturated nitrogen into the white crystals, and filter with suction for 5 hours , vacuum-dried at 25° C. for 3 hours; the crystal...

Embodiment 3

[0067] Example 3 Purification of Cefotiam Hydrochloride Crude Product, Preparation of Cefotiam Hydrochloride Sterile Powder Injection

[0068] Weigh 500g of crude cefotiam hydrochloride with a purity of 92.1% (which contains impurities 7-ACA, DMMT, 7-ATA-HACA, and 7-DMT) and add it to the reaction kettle, add 0.5L of water to dissolve, add 5.0g for injection Activated carbon, heated to 55°C, and filtered after 30 minutes; take the obtained filtrate, add 2L acetone, heat and stir to dissolve, and use a 0.22μm microporous filter membrane to filter under positive pressure at a temperature below 0.1Mpa; freeze the filtrate to 0°C, and refrigerate Crystallize for 2 hours, after the crystallization is completed, filter; put the obtained crystals into a crystallization tank, add 1.5 L of methyl tert-butyl ether for beating and washing, and filter with suction to obtain white crystals; then pour water into the white crystals to saturate Nitrogen, after suction filtration for 4 hours, ...

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Abstract

The invention relates to the technical field of medicaments, and particularly relates to a purification method of cefotiam hydrochloride and an aseptic powder injection of cefotiam hydrochloride. The method comprises the steps of: dissolving cefotiam sodium hydrochloride crude product with water, adding activated carbon for injection to remove pyrogen, then adding acetone, recrystallizing, washing obtained crystal with ethyl ether or methyl tert-butyl ether, filtering, carrying out suction filtering water-saturated nitrogen gas, drying under reduced-pressure to obtain cefotiam aseptic powder which is low in organic residue, pyrogen-free and high in purity.

Description

technical field [0001] The invention relates to the technical field of medicines, in particular to a method for purifying cefotiam hydrochloride and cefotiam hydrochloride sterile powder injection. Background technique [0002] Cefotiam hydrochloride, the English name is Cefotiam Hydrochoride, and its chemical name is ((6R,7R)[2-(2-amino-1,3-thiazol-4-yl)acetamido]-3[[1-( 2-Dimethylaminoethyl)-1H-tetrazol-5-yl]thiomethyl]-8-oxo-5-thio-1-nitrobicyclo[4.2.0]oct-2-ene-2-carboxy acid dihydrochloride). The structural formula is as shown in formula I: [0003] [0004] Formula Ⅰ [0005] Cefotiam is a second-generation semi-synthetic cephalosporin developed by Takeda Corporation of Japan and first launched in Japan in 1981. The effect of this product on Gram-positive bacteria is close to that of cefazolin, and it has better effect on Gram-negative bacteria, such as Haemophilus, Escherichia coli, Klebsiella, and Proteus mirabilis. , Citrobacter, and indole-positive Proteus ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/36C07D501/12A61K31/546A61K9/14A61P31/04
Inventor 刘敏张丽杰刘全胜
Owner HAINAN JINXING PHARMA
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