69 results about "Cefamandole nafate" patented technology

The invention relates to a synthetic method of the antibiotic cefamandole nafate, which adopts the 7-amino-3-(1-methyl-1H-tetrazoline-5-base)-sulfomethyl-3-cef-4-carboxylic acid as raw material and gains the solid of the cefamandole nafate through such five steps as the silylation reaction, acylation reaction, hydrolysis reaction, decolorization and salifying. The silanizing agent used in the silylation reaction adopts the mixture of the silicon amine alkane and the alkylogen silane. Compared with the prior art, the invention is characterized by simple in process operation, low in cost, high in product yield, good in product quality and suitable for industrial production.

The invention relates to an aseptic powder injection of cefamandole nafate and a preparation method thereof; the aseptic powder injection of cefamandole nafate comprises cefamandole nafate and anhydrous sodium carbonate; after the improvement of the preparation technology, the dosages of auxiliary material are small, and therefore the aseptic powder injection of cefamandole nafate obtained is good in stability and low in cost. The synthetic process of the drug material of cefamandole nafate adopted by the invention has simple operation process, low material cost and moderate reaction conditions; the cefamandole nafate produced has high purity and high productive rate.

The invention relates to a cefamandole nafate hydrate. The molecular formula of the cefamandole nafate hydrate is C19H17N6NaO6S25H2O. The preparation method of the cefamandole nafate hydrate comprises the following steps of: dissolving cefamandole nafate crude drug in water and placing the dissolved cefamandole nafate crude drug in a crystallizer; adding 5-15 parts of elution agents, cooling the mixture to 2-8 DEG C, separating out solids and then filtering; and rinsing the solids in the elution agents, drying for 3-5 hours at the drying temperature of 10-50 DEG C under a ventilated or vacuumcondition to obtain the cefamandole nafate hydrate. The invention also provides a cefamandole nafate for injection, which is prepared by using the cefamandole nafate hydrate as the crude drug. The cefamandole nafate hydrate obtained in the method has the advantages of smooth surface, good stability and high dissolving sped in water. After the cefamandole nafate hydrate is dissolved in the water, the action mechanism and the clinical effect of the cefamandole nafate hydrate are the same as those of cefamandole nafate prepared in the traditional process.

The invention relates to a cefamandole nafate compound and a pharmaceutical composition of the cefamandole nafate compound. The cefamandole nafate compound is crystal, and is determined by X-ray powder diffraction, and the characteristic peak in an atlas is shown as 8.8 degrees, 9.5 degrees, 10.2 degrees, 11.3 degrees, 12.0 degrees, 14.4 degrees, 16.8 degrees, 17.3 degrees, 20.6 degrees, 25.0 degrees, 27.8 degrees, 28.1 degrees and 30.2 degrees in a range of 20+/0.2 degrees. The pharmaceutical composition of the cefamandole nafate compound is a preparation and a pharmaceutical composition preparation containing the above cefamandole nafate compound and the preparation is powder-injection. The cefamandole nafate crystalline compound is high in stability and few in insoluble particles; a cosolvent is not needed, so that the compound can be directly and aseptically sub-packaged to obtain cefamandole nafate powder injection for injection. The cefamandole nafate crystalline compound is also fully mixed with aseptic sodium carbonate powder to be aseptically sub-packaged. The number of insoluble particles added with the powder injection of sodium carbonate is few on the basis of reaching standard request.

The invention discloses a method for preparation of fine cefamandole nafate, comprising the steps of mixing crude cefamandole nafate with organic sodium salt, salt-free water and organic solvent (1); controlling pH value of the reaction system to 5.5-7.5 and reaction temperature to 5-15 DEG C; adding active carbon and then filtering to obtain filtrate; mixing the filtrate with organic solvent (2) and separating out crystal to obtain the cefamandole nafate. The method for preparation of the fine cefamandole nafate provided by the invention overcomes the disadvantages of prior preparation method, and has the advantages of simple operation, short preparation period, easy quality control, good product stability and important application value.

The invention provides a method for preparing a cefamandole nafate powder injection preparation. The method comprises the following steps: (a) performing a silanization reaction on 7-ACT and a silanization agent in a dichloromethane solvent under temperature control, and reducing the temperature after the reaction is completed so as to obtain a reaction liquid 1, wherein the solid-liquid ratio of7-ACT to dichloromethane is 1g:(3-6)ml; (b) dropwise adding (R)-(-)-O-formylmandeloyl chloride into the reaction liquid 1, controlling the temperature, performing an acylation reaction so as to obtaina reaction liquid 2; (c) performing treatment of extraction, decoloring and dehydration on the reaction liquid 2; (d) performing temperature control crystallization; and (e) washing a solid with acetone, drying, performing sterile sub-packaging, thereby obtaining the cefamandole nafate powder injection preparation. Due to adoption of a high-concentration dichloromethane reaction system, the method is rapid in silanization and acylation process, short in reaction time, low in reaction residue, high in product yield and small in impurity. After the reactions, organic solvents such as dichloromethane can be easily recycled and repeatedly used, so that the method is relatively environment-friendly, low in cost and applicable to large-scale industrial production.

The invention relates to a cefamandole nafate new crystal form and a crystallization 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 cefamandole nafate new crystal form is defined as VI. The preparing method comprises the following steps of adding the cefamandole nafate solid into the good solvent, and mixing at the temperature of 10-30 DEG C to enable the cefamandole nafate to dissolve completely, wherein the solution concentration is 0.05-0.4 g/ml; adding additives at different concentrations into the solution; adding a solventing-out agent into the solution, wherein the dosage of the solventing-out agent is 5-20 times the dosage of the good solvent; after cultivating the crystal, performing suction filtration on formed suspension liquid; drying to obtain a cefamandole nafate new crystal form product. The solubility of the new crystal form is improved by more than 5%; the new crystal form has higher solubility, so that the dissolution rate of a medicinal preparation can be improved. The traditional stable crystal form is of a needle shape, but the appearance of the new crystal form is of a prism shape, thus, the bulk density of products is improved by more than 8%, better mobility is realized, and accordingly convenience in package and transport of the products is improved.

The invention relates to suspension powder injection of cefamandole nafate and a preparation method thereof and further relates to new application of the injection in treating acute suppurative cholangitis. The frozen-dried suspension powder injection comprises the following components in parts by weight: 1 part of cefamandole nafate, 1.5-12 parts of surfactant and 2-15 parts of frozen-dried supporting agents.

The invention discloses a preparation method of a Cefamandole Nafate powder injection for injection. The method includes the steps of: (1) strain preparation; (2) preparation and culture of seed tank; (3) preparation and culture of a fermentation tank; (4) filtration; (5) decolorization and concentration; (6) preparation of a reaction tank and pipeline; (7) preparation of enzyme catalytic reaction; (8) enzyme catalytic reaction; (9) crystallization; (10) centrifugation and vacuum drying; (11) preparation of 7-ATCA; (12) preparation of cefamandole acid; (13) preparation of Cefamandole Nafate; and (14) aseptic subpackaging, thus obtaining the Cefamandole Nafate powder injection for injection. The invention provides the method of improving the 7-ACA preparation process so as to improve the product quality of cefamandole.

The invention relates to a cefamandole nafate medicine composition for treating bacterial infection and belongs to the technical field of medicines. The composition is composed of cefamandole nafate and sodium dihydrogen phosphate; cefamandole nafate is a crystal and an X-ray powder diffraction pattern obtained through measurement of Cu-K(alpha) ray is shown in the graph I. The novel crystal form of cefamandole provided by the invention is different from the crystal form structure in the prior art, through experimental verification, the fact that the novel crystal form compound is high in purity, good in mobility and stability, low in polymer content, low in hygroscopicity, and safe and reliable during clinical application is found, powder-injection prepared from the novel crystal form compound is good in stability, good in stability after being combined with a solvent, and extremely low in content of insoluble particles and is particularly suitable for being applied clinically.

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.

The invention provides a cefamandole nafate compound entity used for children. The structural formula is as shown in specifications. The cefamandole nafate compound entity is prepared through the following steps that step1, a cefamandole nafate crude product is dissolved in water, sodium hydrogen carbonate is added, pH is adjusted to 6.5-7.5, active carbon stirring and discoloring are performed, and then filtering is performed; step2, an extracting agent is added into filtrate, and then the filtrate is transferred into a pressure-resistant container in a filling mode and taken out after being defoamed and frozen in a temperature control mode; step3, an organic phase is removed, after a solid is melted, ethyl alcohol is dripped, and then slow stirring, crystal growing, filtration washing and vacuum drying are performed to obtain the cefamandole nafate finished product. The cefamandole nafate prepared through the method has the advantages of having few impurities, being high in purity and the like compared with a traditional technology.

The invention discloses a detection method of formic acid in cefamandole nafate. According to the method, a liquid chromatography is used for detecting; and a mobile phase used in a detection process is a phosphoric acid water solution with the volume concentration of 0.02%-0.1%. By taking the phosphoric acid water solution with the volume concentration of 0.02%-0.1% as the mobile phase for detecting the formic acid in the cefamandole nafate in a liquid chromatography, the dissociation of the formic acid can be effectively inhibited, and retention time and separation degree of the formic acid can be improved very well, so that the separation degrees of the formic acid and front and back adjacent impurity peaks are 3.68 and 1.78 respectively; and the blocking of a chromatographic column is not caused. Furthermore, the method has high accuracy and precision and good stability, and is easy to realize in industrialization.