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Method for preparing crystalline cefathiamidine and its usage

A cefathiamidine crystallization technology, which is applied in the field of crystalline cefathiamidine and its preparation, can solve the problems of inconvenient production operation, quality not conforming to cefathiamidine, high cost, etc., achieves reduction of production cost, simple and easy control of the production process, and clinical Apply a good effect

Inactive Publication Date: 2003-12-24
GUANGZHOU BAIYUNSHAN PHARMA HLDG CO LTD BAIYUNSHAN PHARMA GENERAL FACTORY +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Cefathiamidine, which is inconvenient in production and operation, high in cost, and whose quality does not meet pharmaceutical standards, is adopted by crystallization methods commonly used in pharmaceutical production, such as crystallization by changing temperature, crystallization by isoelectric point, crystallization by addition of salt, crystallization by azeotropic distillation, etc.

Method used

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  • Method for preparing crystalline cefathiamidine and its usage
  • Method for preparing crystalline cefathiamidine and its usage

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] At normal temperature, put 5 kg of cefathiamidine into the reactor, add 49 liters of water to dissolve, stir for 30 minutes, filter, adjust the pH of the filtrate to 4.5 with hydrochloric acid, add 200 liters of acetone until the filtrate is cloudy, and stir at 60 rpm , control the supersaturated concentration of the solution, continue to slowly add 200 liters of acetone / ethanol (weight ratio 10: 1), grow crystals, filter with suction, wash 2 times with 50 liters of acetone, drain, and dry under reduced pressure to obtain crystalline cefathiamidine 4.6 kilogram.

[0029]Use D / max-IIIA DIFFRATOMETER (RIGAKU CORPORATION, JANPAN) X-diffractometer, with Cu, K α 1, λ=1.54056A ray measurement, the X-ray powder diffraction pattern of crystalline cefathiamidine (see attached figure 1 ) is expressed in terms of 2θ, d-plane spacing and relative intensity greater than 5% as follows: 2θ d relative intensity I / I. (>5%)7.540 11.7146 58.340 ...

Embodiment 2

[0031] At 0° C., 50 liters of a 14% (w / w) cefathiamidine aqueous solution having a pH of 5.5 was put into the reactor, and sterile filtered. Under the aseptic production environment conditions that meet the requirements of GMP, with stirring at 70 rpm, add 300 liters of acetone to the sterile filtrate until the filtrate is cloudy, control the supersaturated concentration of the solution, continue to slowly add 350 liters of acetone, grow crystals, pump filtered, washed twice with 50 liters of acetone, drained, and dried under reduced pressure to obtain 7.3 kg of crystalline cefathiamidine sterile powder.

[0032] The X-ray and infrared spectra of the obtained crystals are consistent with those in Example 1. Stability test: according to the "Pharmacopoeia of the People's Republic of China" appendix drug stability test guidelines, select the amorphous cefathiamidine sample (batch number 8801) and the crystalline cefathiamidine sample (batch number 010210020) prepared by this emb...

Embodiment 4

[0040] Under normal temperature, put 5 kilograms of cefathiamidine crude products into the reactor, add 49 liters of water to dissolve, add 0.1 kilogram of activated carbon, stir for 30 minutes, press filter, adjust the pH of the filtrate to 5.5 with triethylamine, stir at 70 rpm Next, add 300 liters of ethanol until the solution is turbid, control the supersaturated concentration of the solution, continue to add 330 liters of isopropanol, grow crystals, filter with suction, wash twice with 60 liters of acetone, drain, and dry under reduced pressure to obtain crystalline cefathiamidine 4.4 kg.

[0041] The obtained crystalline infrared spectrum is consistent with that of Example 1.

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Abstract

A crystallized cefathiamidine is prepared from the cefathiamidine solution through controlling pH to 3.5-6.5, adding proper solvent until the solution becomes cloudy, controlling saturation procedureand crystal growth speed while adding said solvent, separating and drying. Its advantage is uniform granularity. It can be used to prepare the medicines for treating the infection of staphylococcus aureus, pneumoccus, enterococcus, streptococcus, etc.

Description

technical field [0001] The invention relates to the field of chemical pharmacy, in particular, the invention relates to crystalline cefathiamidine and its preparation method and application. Background technique [0002] The chemical name of cefathiamidine is (6R,7R)-3[(acetyl)methyl]-7-[α-(N,N'-diisopropylamidinothio)-acetylamino]-8-oxo Dai-5-thia-1-azabicyclo[4,2,0]-oct-2-ene-2-carboxylate betaine, the molecular formula is C 19 h 28 N 4 o 6 S 2 , the structural formula is: [0003] Cefathiamidine is a β-lactam antibiotic with a similar antibacterial spectrum to cefalotin. It has a strong effect on Staphylococcus aureus, Streptococcus viridans, and Pneumococcus, and has unique antibacterial activity against Enterococcus. , Haemophilus influenzae, streptococcus viridans, pneumococcus, diphtheria bacillus, tetanus bacillus, Escherichia coli, Proteus mirabilis, etc. also have certain effects, and are not absorbed when taken orally. The serum protein binding rate is lo...

Claims

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Application Information

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IPC IPC(8): A61K31/545A61P31/04C07D501/28
Inventor 王文梅谢彬黄伟东刘学斌周可祥许淑文
Owner GUANGZHOU BAIYUNSHAN PHARMA HLDG CO LTD BAIYUNSHAN PHARMA GENERAL FACTORY
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