Cefamandole nafate new crystal form and crystallization preparing method thereof

A technology of cefamandole sodium and crystal form, which is applied in the field of new crystal form of cefamandole sodium and its preparation, can solve problems such as unsuitable for popularization and use, hidden safety hazards, poor stability, etc., and achieve easy commercial industrialization scale Implementation, good for long-term storage, good thermal stability

Inactive Publication Date: 2015-08-19
TIANJIN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Publication numbers CN201010257886.X and CN201010199235.X are both prepared hydrates, but substances containing crystal water often have the defect of unstable crystal water in the preparation process, and there is a problem of poor stabil...

Method used

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  • Cefamandole nafate new crystal form and crystallization preparing method thereof
  • Cefamandole nafate new crystal form and crystallization preparing method thereof
  • Cefamandole nafate new crystal form and crystallization preparing method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 2.50 g of dry cefamandole sodium solid into 5 mL of water and propionic acid mixed solution to form a suspension, wherein the volume ratio of water to propionic acid is 3:2, stir the suspension at 10°C to dissolve all the solids , constant temperature, dropwise add 25mL of acetone to the solution at a rate of 0.05ml / min, then cool down to 0°C at a rate of 0.05°C / min, let the crystal grow for 4h, filter and place the obtained wet product at 10°C at room temperature Dry under high pressure for 3 hours to obtain a new crystal product of cefamandole sodium. The X-ray powder diffraction pattern of the new crystal product is as follows: figure 1 As shown, it has characteristic peaks at diffraction angles 2θ=4.8, 8.5, 13.1, 14.5, 17.2, 18.2, 19.1, 19.6, 21.0, 21.6, 22.0, 23.4, 25.2, 31.1 degrees; the DSC of the new crystal form product is as follows figure 2 As shown, it has a characteristic endothermic peak at 169.25 °C. The melting point of the new crystalline product...

Embodiment 2

[0025] Add 2.00 g of dry cefamandole sodium solid into 3 ml of propionic acid to form a suspension, stir the suspension at 30°C to dissolve all the solids, and add 100 mL of ethanol dropwise to the solution at a rate of 20 ml / min at a constant temperature , then lower the temperature to 2°C at a rate of 1°C / min, let the crystal grow for 15 hours, filter and dry the obtained wet product at 10°C under normal pressure for 5 hours to obtain a new crystal form of cefamandole sodium. The X-ray powder diffraction pattern of the new crystalline product has characteristic peaks at diffraction angles 2θ=4.9, 8.3, 13.0, 14.5, 17.3, 18.1, 19.0, 19.7, 21.1, 21.7, 22.2, 23.4, 25.2, 31.0 degrees, DSC There is a characteristic endothermic peak at 169.20°C. The melting point of the new crystalline product obtained by this method is higher than that of the crystalline forms reported in all patents. It has high thermal stability, no degradation changes after long-term storage, and the appearance...

Embodiment 3

[0027] Add 2.00 g of dry cefamandole sodium solid into 2.5 ml dimethyl sulfoxide to form a suspension, stir the suspension at 30 ° C to dissolve all the solids, and add the solid to the solution at a constant temperature at a rate of 20 ml / min. Add 100mL of isopropanol dropwise, then cool down to 5°C at a rate of 1°C / min, let the crystal grow for 5h, filter and dry the obtained wet product at 10°C under normal pressure for 3h to obtain cefamandole sodium new Crystalline products. The X-ray powder diffraction pattern of the new crystalline product has characteristic peaks at diffraction angles 2θ=4.7, 8.2, 13.1, 14.4, 17.2, 18.2, 19.1, 19.6, 21.2, 21.7, 22.1, 23.3, 25.2, 31.0 degrees, DSC There is a characteristic endothermic peak at 168.05°C. The melting point of the new crystalline product obtained by this method is higher than that of the crystalline forms reported in all patents. It has high thermal stability, no degradation change after long-term storage, the appearance o...

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Abstract

The invention relates to a cefamandole nafate new crystal form and a preparing method thereof. The cefamandole nafate new crystal form is characterized by characterizing the characteristic peaks of a diffraction angle 2 theta degree and a DSC by using X-ray powder diffraction patterns, wherein the new crystal form of the cefamandole nafate compound as V. The preparing method includes the following steps of adding the cefamandole nafate solid into the good solvent at the temperature of 10-30 DEG C, mixing to let the cefamandole nafate dissolve completely, wherein the solution concentration is 0.5 to 1.0 g/ml,; adding the poor solvent, and then reducing the system temperature to 0 to 5 DEG C; standing for cultivating the crystal for 4 to 72 hours; filtering, washing, and drying to obtain a cefamandole nafate new crystal form product. The melting range of the new crystal form is 160 to 180 DEG C, and the peak value is 169+/-2 DEG C which is higher than the melting points of crystal forms which are reported by all the other patents, thus the product thermal stability is improved. The purity, color, and the form of the new crystal form product are not changed after being stored for 100 days under room temperature and dry conditions, so that long time storage is favorably realized.

Description

technical field [0001] The invention belongs to the technical field of medicine separation, and in particular relates to a new crystal form of cefamandole sodium and a preparation method thereof. Background technique [0002] The chemical name of Cefamandole Nafate is 7-D-(2-formyloxyphenylacetamide)-3-[(1-methyl-1H-tetrazol-5-yl)thiomethyl] -8-Oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid sodium salt, the molecular formula is C 19 h 18 N 6 NaO 6 S 2 , with a molecular weight of 512.50. The structural formula is as formula (I). [0003] [0004] Cefamandole sodium was developed by Lilly Company of the United States in 1972 and first listed in 1978. The trade name of injection is MANDOL. Cefamandole sodium is a second-generation semi-synthetic cephalosporin with strong bactericidal effect. It has some advantages of the first-generation and third-generation cephalosporins. It is relatively stable to β-lactamase and has low nephrotoxicity. , high blood co...

Claims

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Application Information

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IPC IPC(8): C07D501/36C07D501/12A61P31/04
CPCC07D501/36C07D501/12
Inventor 郝红勋陶灵刚何芳侯宝红吕军尹秋响王永莉龚俊波谢闯鲍颖
Owner TIANJIN UNIV
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