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Cefmetazole aseptic powder and its preparation method

A technology of cefmetazole sodium and sterile powder injection, which is applied in the direction of antifungal agents, pharmaceutical formulas, medical preparations containing active ingredients, etc., can solve the problems of low product purity, easy decomposition, fast evaporation speed, etc. The effect of high efficiency and high purity

Active Publication Date: 2012-08-08
HAINAN JINXING PHARMA
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Problems solved by technology

But the cefmetazole sodium purity that this method makes is not high, and the content of cefmetazole recorded by high performance liquid chromatography is 94.3%, can not meet the requirement of national drug standard
[0009] Chinese patent CN 101787039A discloses a preparation method of cefmetazole sodium compound. Through acid-base reaction, macroporous adsorption resin and activated carbon adsorption, high-purity cefmetazole sodium compound is obtained. The cefmetazole sodium compound prepared by this method is The HPLC purity is 99.7%, but the cefmetazole sodium prepared by this method has not been controlled by the polymer, and in this method, it needs to be dried in the range of 40-50 ° C, which is easy to produce polymer
However, cefmetazole sodium is extremely unstable in aqueous solution, and its aqueous solution degrades quickly at room temperature. After testing, it is found that the side chain 5-mercapto-1-methyltetrazole in the aqueous solution increases, and the content of cefmetazole sodium decreases.
And according to the Chinese patent report with the application number 200910305622.4, the aseptic freeze-dried powder prepared by ultra-low temperature freeze-forming technology has the following disadvantages: uneven freeze-dried powder, poor color, difference in pure loading, problems in clarity, prepared The purity of the product is low, the stability of the substance has not been completely resolved, and it is still not easy to store for a long time, etc., and the process of freeze-dried powder injection is relatively complicated and the cost is high
But the former utilizes ethanol and water solvent crystallization, under the condition that water exists, cefmetazole sodium is unstable, decomposes easily, and in the follow-up drying step, the temperature that needs is higher, easily causes cefmetazole sodium to decompose; Methanol and ether are recrystallized. Although it does not need to be in contact with water, ether has a low boiling point and a fast evaporation rate. During crystallization and filtration, water will be condensed on the crystal surface, making cefmetazole sodium unstable. Higher, it is easy to cause the increase of related substances such as polymers

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  • Cefmetazole aseptic powder and its preparation method
  • Cefmetazole aseptic powder and its preparation method
  • Cefmetazole aseptic powder and its preparation method

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preparation example Construction

[0048] A preparation method of cefmetazole sodium aseptic powder, comprising:

[0049] Step 1: Dissolve Cefmetazole Sodium with acetone, methanol or ethanol, heat to reflux, add the injection to absorb with activated carbon, and filter;

[0050] Step 2: Take the filtrate obtained in Step 1, add isopropyl ether, methyl tert-butyl ether, ethyl acetate or ethyl formate, heat and stir to dissolve, and filter under positive pressure;

[0051] Step 3: Freeze the filtrate obtained in step 2 to -5-5°C for crystallization, collect the obtained crystals, filter, dry under reduced pressure at 15-30°C, and pulverize.

Embodiment 1

[0055] Embodiment 1: Preparation of Cefmetazole Sodium Sterile Powder Injection

[0056] (1) Weigh 500g of cefmetazole sodium raw material, its HPLC purity is 94.0%, and its polymer content is 1.22%, put it into the reaction kettle, add 1L of acetone, and heat to dissolve;

[0057] (2) After the cefmetazole sodium raw material is dissolved, add 2.5 g of activated carbon for injection, and filter under reflux for 30 minutes;

[0058] (3) After filtering, add 2L of methyl tert-butyl ether to the filtrate, heat and stir to dissolve;

[0059] (4) After dissolving, below 0.1Mpa, use a 0.22μm microporous membrane to filter under positive pressure;

[0060] (5) After filtering, freeze the filtrate to 0°C, and crystallize at low temperature for 2 hours;

[0061] (6) After the crystallization is completed, filter, and vacuum-dry the obtained crystals at 15° C. for 4 hours;

[0062] (7) After drying, the crystals were pulverized to obtain 453.5 g of white cefmetazole sodium sterile p...

Embodiment 2

[0064] Embodiment 2: Preparation of Cefmetazole Sodium Sterile Powder Injection

[0065] (1) Take by weighing 500g cefmetazole sodium raw material, its HPLC purity is 94.0%, high molecular polymer content is 1.22%, add in the reactor, add the ethanol of 1.5L, heat reflux;

[0066] (2) After cefmetazole sodium is dissolved, add 7.5 g of activated carbon for injection, heat and reflux for 30 minutes and then filter;

[0067] (3) After filtering, add 1.5L ethyl acetate to the filtrate, heat and stir to dissolve;

[0068] (4) After dissolving, below 0.1Mpa, use a 0.22μm microporous membrane to filter under positive pressure;

[0069] (5) After filtering, freeze the filtrate to 5°C, and crystallize at low temperature for 2 hours;

[0070] (6) After the crystallization is completed, filter, and vacuum-dry the obtained crystals at 30° C. for 3 hours;

[0071] (7) After drying, the crystals were pulverized to obtain 456.5 g of white cefmetazole sodium sterile powder, with a yield o...

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Abstract

The invention relates to the field of pharmaceutics, specifically to cefmetazole aseptic powder and its preparation method. The preparation method comprises: employing a mixed solvent to recrystallize cefmetazole, using a good solvent to dissolve the cefmetazole raw material, adding activated carbon for injection to remove a pyrogen, then adding a poor solvent for recrystallization, and conducting drying at a low temperature, thus obtaining the cefmetazole aseptic powder with no pyrogen and high purity. Characterized by simple operation and high yield, the preparation method of the invention can prepare cefmetazole aseptic powder with high purity, safe and reliable quality, thus being suitable for preparing cefmetazole aseptic powder injections and widely applicable in large scale production of cefmetazole aseptic powder injections.

Description

technical field [0001] The invention belongs to the field of pharmaceutical preparations, and in particular relates to a cefmetazole sodium sterile powder and a preparation method thereof. Background technique [0002] Cefmetazole sodium, English name Cefmetazole, chemical name 6R, 7S-7-[2-[(cyanomethyl)thio]acetamido]-7-methoxy-3-[[(1-methyl -1H-tetrazol-5-yl)thio]methyl]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid sodium salt, Molecular formula is C 15 h 16 N 7 NaO 5 S 3 , the molecular weight is 493.52, and the structural formula is as follows: [0003] [0004] Cefmetazole sodium, also known as cyanazol-methoxycephalosporin, cefmetazol, and pioneer metabolite, is developed by Japan Sankyo (Sankyo Pharmaceutical Co., Ltd.) and is a broad-spectrum, high-efficiency, low-toxicity antibiotic. Its antibacterial The spectrum is similar to that of cefoxetine, and the performance is similar to that of the second-generation cephalosporins. Cefmetazole so...

Claims

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Application Information

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IPC IPC(8): C07D501/57C07D501/12A61K31/546A61P31/10
Inventor 刘敏张丽杰刘全胜
Owner HAINAN JINXING PHARMA
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