Patents Assigned to HAINAN LINGKANG PHARMACEUTICAL CO., LTD.
  • Publication number: 20180111949
    Abstract: It discloses a new industrial crystallization method of Cefuroxime Sodium, wherein supercritical fluid extraction technology and traditional crystalline technology are combined to realize the recrystallization of Cefuroxime Sodium. Processes such as extraction, adsorption, crystallization and drying are carried out with a supercritical fluid, a solvent, an extraction cell and a crystallization tank to realize the recrystallization of Cefuroxime Sodium under a specific pressure at a specific temperature.
    Type: Application
    Filed: August 25, 2017
    Publication date: April 26, 2018
    Applicants: HAINAN LINGKANG PHARMACEUTICAL CO., LTD, TIANJIN UNIVERSITY
    Inventors: Linggang TAO, Hongxun HAO, Jingkang WANG
  • Publication number: 20170349609
    Abstract: A novel crystalline form is defined by diffraction angle 2?° of X-ray powder diffraction pattern and characteristic peak of differential scanning calorimetry (DSC). The novel crystalline form of Cefamandole Nafate is prepared as follows: adding Cefamandole Nafate in solid state to an organic solvent to form a suspension with a concentration of 0.04˜0.3 g/ml, stirring the suspension at 40˜50° C. for a period of time, and then cooling to 5˜15° C. at certain cooling rate, continuing to stir for a period of time, then suction filtrating the obtained suspension, the resulting filer cake is Cefamandole Nafate as wet product, which is dried to constant weight to provide the novel crystalline form of Cefamandole Nafate as final product.
    Type: Application
    Filed: August 25, 2017
    Publication date: December 7, 2017
    Applicants: TIANJIN UNIVERSITY, HAINAN LINGKANG PHARMACEUTICAL CO., LTD
    Inventors: Hongxun Hao, Linggang Tao, Fang He, Baohong Hou, Jingkang Wang, Jun Lv, Qiuxiang Yin, Yongli Wang, Junbo Gong, Chuang Xie, Ying Bao
  • Patent number: 9834567
    Abstract: A novel crystalline form is defined by diffraction angle 2?° of X-ray powder diffraction pattern and characteristic peak of differential scanning calorimetry (DSC). The novel crystalline form of Cefamandole Nafate is prepared as follows: adding Cefamandole Nafate in solid state to an organic solvent to form a suspension with a concentration of 0.04˜0.3 g/ml, stirring the suspension at 40˜50° C. for a period of time, and then cooling to 5˜15° C. at certain cooling rate, continuing to stir for a period of time, then suction filtrating the obtained suspension, the resulting filer cake is Cefamandole Nafate as wet product, which is dried to constant weight to provide the novel crystalline form of Cefamandole Nafate as final product.
    Type: Grant
    Filed: August 25, 2017
    Date of Patent: December 5, 2017
    Assignees: TIANJIN UNIVERSITY, HAINAN LINGKANG PHARMACEUTICAL CO., LTD
    Inventors: Hongxun Hao, Linggang Tao, Fang He, Baohong Hou, Jingkang Wang, Jun Lv, Qiuxiang Yin, Yongli Wang, Junbo Gong, Chuang Xie, Ying Bao
  • Patent number: 9834540
    Abstract: It discloses Omeprazole Sodium semihydrate and preparation method thereof, wherein every mole of Omeprazole Sodium semihydrate contains 0.5 mole of water, and it has an X-ray diffraction pattern comprising characteristic peaks at diffraction angles 2? of 6.26°±0.1°, 11.10°±0.1°, 12.20°±0.1°, 15.58°±0.1°, 16.02°±0.1°, 17.12°±0.1°, 19.08°±0.1°, 21.00°±0.1°, 22.68°±0.1°, 23.48°±0.1°, 24.08°±0.1°, 26.52°±0.1° and 28.08°±0.1°. A raw material of Omeprazole Sodium hydrate is added into an organic solvent, stirring for 2˜9 hours at constant temperature of 25˜60° C., thereafter Omeprazole Sodium semihydrate is provided after filtrating and drying.
    Type: Grant
    Filed: November 20, 2015
    Date of Patent: December 5, 2017
    Assignees: TIANJIN UNIVERSITY, HAINAN LINGKANG PHARMACEUTICAL CO., LTD
    Inventors: Ying Bao, Linggang Tao, Long Li, Hongxun Hao, Jun Lv, Baohong Hou
  • Publication number: 20170197937
    Abstract: A novel crystalline form is defined by using diffraction angle 2?° of X-ray powder diffraction pattern and characteristic peaks of differential scanning calorimetry (DSC). Pantoprazole Sodium solid is added to an alcohol solvent to form a suspension with a concentration of 0.05˜0.2 g/mL, and then an antioxidant is added to the suspension, completely dissolving the solid at a temperature of 15˜35° C., and a solventing-out agent is dropwise added to the solution under the application of ultrasonic wave, wherein the amount of the solventing-out agent is 3˜10 times (in volume) of the alcohol solvent; followed by cooling the solution down to 0˜5° C., continuing to stir for 1˜3 h, and suction filtrating obtained solid-liquid suspension to provide a novel crystalline form of Pantoprazole Sodium crystal after drying the product to constant weight.
    Type: Application
    Filed: November 20, 2015
    Publication date: July 13, 2017
    Applicants: TIANJIN UNIVERSITY, HAINAN LINGKANG PHARMACEUTICAL CO., LTD
    Inventors: Hongxun HAO, Linggang TAO, Shen JIANG, Yongli WANG, Jingkang WANG, Jun LV, Qiuxiang YIN, Baohong HOU, Zhao XU, Chuang XIE, Zhao WANG
  • Publication number: 20170158711
    Abstract: It discloses a new industrial crystallization method of Cefuroxime Sodium, wherein supercritical fluid extraction technology and traditional crystalline technology are combined to realize the recrystallization of Cefuroxime Sodium. Processes such as extraction, adsorption, crystallization and drying are carried out with a supercritical fluid, a solvent, an extraction cell and a crystallization tank to realize the recrystallization of Cefuroxime Sodium under a specific pressure at a specific temperature.
    Type: Application
    Filed: November 27, 2015
    Publication date: June 8, 2017
    Applicants: HAINAN LINGKANG PHARMACEUTICAL CO., LTD., TIANJIN UNIVERSITY
    Inventors: Linggang TAO, Hongxun HAO, Jingkang WANG
  • Patent number: 9637502
    Abstract: A novel crystalline form of Cefathiamidine compound and its preparation method, characterizing in its X-ray powder diffraction pattern and differential scanning calorimetry thermogram. Dissolving Cefathiamidine compound with a purity of 98% or higher in a solvent at a temperature of 30˜45° C. to form a solution, whose concentration is controlled within 0.05˜0.2 g/mL, and then adding a solventing-out agent to the solution, wherein the amount of the solventing-out agent is 3˜5 times (in volume) of that of the solvent; followed by cooling the solution down to 0˜10° C. at a rate of 0.2˜1° C./min; continuing to stir for 1˜3 hours, and separating the obtained solid-liquid suspension to provide a novel crystalline form of Cefathiamidine compound after drying.
    Type: Grant
    Filed: November 20, 2015
    Date of Patent: May 2, 2017
    Assignees: TIANJIN UNIVERSITY, HAINAN LINGKANG PHARMACEUTICAL CO., LTD
    Inventors: Hongxun Hao, Linggang Tao, Zhihong Sun, Baohong Hou, Jun Lv, Qiuxiang Yin, Yongli Wang, Junbo Gong, Chuang Xie, Ying Bao
  • Publication number: 20170050982
    Abstract: A novel crystalline form is defined by diffraction angle 2?° of X-ray powder diffraction pattern and characteristic peak of differential scanning calorimetry (DSC). The novel crystalline form of Cefamandole Nafate is prepared as follows: adding Cefamandole Nafate in solid state to an organic solvent to form a suspension with a concentration of 0.04˜0.3 g/ml, stirring the suspension at 40˜50° C. for a period of time, and then cooling to 5˜15° C. at certain cooling rate, continuing to stir for a period of time, then suction filtrating the obtained suspension, the resulting filer cake is Cefamandole Nafate as wet product, which is dried to constant weight to provide the novel crystalline form of Cefamandole Nafate as final product.
    Type: Application
    Filed: November 20, 2015
    Publication date: February 23, 2017
    Applicants: TIANJIN UNIVERSITY, HAINAN LINGKANG PHARMACEUTICAL CO., LTD
    Inventors: Hongxun HAO, Linggang TAO, Fang He, Baohong HOU, Jingkang WANG, Jun LV, Qiuxiang YIN, Yongli WANG, Junbo GONG, Chuang XIE, Ying Bao
  • Publication number: 20170044137
    Abstract: It discloses Omeprazole Sodium semihydrate and preparation method thereof, wherein every mole of Omeprazole Sodium semihydrate contains 0.5 mole of water, and it has an X-ray diffraction pattern comprising characteristic peaks at diffraction angles 2? of 6.26°±0.1°, 11.10°±0.1°, 12.20°±0.1°, 15.58°±0.1°, 16.02°±0.1°, 17.12°±0.1°, 19.08°±0.1°, 21.00°±0.1°, 22.68°±0.1°, 23.48°±0.1°, 24.08°±0.1°, 26.52°±0.1° and 28.08°±0.1°. A raw material of Omeprazole Sodium hydrate is added into an organic solvent, stirring for 2˜9 hours at constant temperature of 25˜60° C., thereafter Omeprazole Sodium semihydrate is provided after filtrating and drying.
    Type: Application
    Filed: November 20, 2015
    Publication date: February 16, 2017
    Applicants: TIANJIN UNIVERSITY, HAINAN LINGKANG PHARMACEUTICAL CO., LTD
    Inventors: Ying BAO, Linggang TAO, Long LI, Hongxun HAO, Jun LV, Baohong HOU
  • Publication number: 20170044184
    Abstract: A novel crystalline form of Cefathiamidine compound and its preparation method, characterizing in its X-ray powder diffraction pattern and differential scanning calorimetry thermogram. Dissolving Cefathiamidine compound with a purity of 98% or higher in a solvent at a temperature of 30˜45° C. to form a solution, whose concentration is controlled within 0.05˜0.2 g/mL, and then adding a solventing-out agent to the solution, wherein the amount of the solventing-out agent is 3˜5 times (in volume) of that of the solvent; followed by cooling the solution down to 0˜10° C. at a rate of 0.2˜1° C./min; continuing to stir for 1˜3 hours, and separating the obtained solid-liquid suspension to provide a novel crystalline form of Cefathiamidine compound after drying.
    Type: Application
    Filed: November 20, 2015
    Publication date: February 16, 2017
    Applicants: TIANJIN UNIVERSITY, HAINAN LINGKANG PHARMACEUTICAL CO., LTD
    Inventors: Hongxun HAO, Linggang TAO, Zhihong SUN, Baohong HOU, Jun LV, Qiuxiang YIN, Yongli WANG, Junbo GONG, Chuang XIE, Ying BAO
  • Patent number: 9090631
    Abstract: A method for treating cefotiam hydrochloride, comprises the following steps: step 1), dissolving the raw material cefotiam hydrochloride in water, treating it with an acidic salt, then cooling it, and filtering the precipitate to obtain an aqueous filtrate; step 2), adding a water-immiscible solvent to the above aqueous solution for extraction, and then separating the organic phase containing impurities to obtain an aqueous solution containing cefotiam hydrochloride; step 3) adding to the aqueous solution a poor solvent of cefotiam hydrochloride and controlling the temperature for recrystallization, washing the educed crystals by centrifugation, and drying them to obtain purified cefotiam hydrochloride. The cefotiam content of the refined cefotiam hydrochloride obtained by the method of the present invention is not less than 86%, the content of polymeric impurities is less than 0.3%, and the content of insoluble microparticles in the injection prepared therefrom is quite low.
    Type: Grant
    Filed: April 14, 2011
    Date of Patent: July 28, 2015
    Assignee: HAINAN LINGKANG PHARMACEUTICAL CO., LTD.
    Inventor: Linggang Tao
  • Patent number: 9024064
    Abstract: A process for preparing a pure alanylglutamine comprises the steps of: 1) reacting N-(?-chloro)-propionyl-glutamine and hydrazine compound to obtain an alanylglutamine crude product; 2) mixing anhydrous methanol and the alanylglutamine crude product to provide a filter cake; 3) dissolving the filter cake in water, heating, adding ethanol, and cooling to yield the pure alanylglutamine.
    Type: Grant
    Filed: December 27, 2011
    Date of Patent: May 5, 2015
    Assignee: Hainan Lingkang Pharmaceutical Co., Ltd.
    Inventor: Linggang Tao
  • Publication number: 20150038740
    Abstract: A process for preparing a pure alanylglutamine comprises the steps of: 1) reacting N-(?-chloro)-propionyl-glutamine and hydrazine compound to obtain an alanylglutamine crude product; 2) mixing anhydrous methanol and the alanylglutamine crude product to provide a filter cake; 3) dissolving the filter cake in water, heating, adding ethanol, and cooling to yield the pure alanylglutamine.
    Type: Application
    Filed: December 27, 2011
    Publication date: February 5, 2015
    Applicant: HAINAN LINGKANG PHARMACEUTICAL CO., LTD.
    Inventor: Linggang Tao
  • Patent number: 8927707
    Abstract: It discloses a process for refining Aztreonam, comprising the steps of 1) treating Aztreonam material with an alkali metal alkoxylate or an alkali earth metal alkoxylate under heating in the presence of a suitable solvent or a mixture of solvents, followed by adjusting the pH value with a suitable acid and cooling down to precipitate Aztreonam, which provides a primary purified Aztreonam; 2) adsorbing Aztreonam with strongly basic ion exchange resin, followed by eluting the resin and collecting the eluate, to provide a secondary purified Aztreonam after concentration under reduced pressure; 3) adjusting the pH value with a suitable acid to allow crystallization, followed by centrifuging and washing the resultant crystals, to provide a tertiary purified Aztreonam after drying. The refined Aztreonam product has a purity of no less than 99.2%, mostly no less than 99.5%, with little residue on ignition and significantly low content of heavy metals.
    Type: Grant
    Filed: March 17, 2011
    Date of Patent: January 6, 2015
    Assignee: Hainan Lingkang Pharmaceutical Co., Ltd.
    Inventor: Linggang Tao
  • Patent number: 8907100
    Abstract: A process for purifying lansoprazole comprises 1) loading crude lansoprazole material onto a macroporous resin column; 2) concentrating the eluate from the column in a crystallization vessel by vacuum; 3) seeding lansoprazole crystal; 4) crystallizing the lansoprazole; 5) separating the precipitated crystals. The process especially has large processing capacity, can be carried out continuously and therefore suitable for industrial production, improving the quality of formulated products and reducing side effects.
    Type: Grant
    Filed: December 27, 2011
    Date of Patent: December 9, 2014
    Assignee: Hainan Lingkang Pharmaceutical Co., Ltd.
    Inventor: Linggang Tao
  • Patent number: 8895728
    Abstract: A novel process for purifying Cefmenoxime hydrochloride comprises: 1) adding a solvent wherein Cefmenoxime hydrochloride is insoluble at the temperature less than 30° C., filtering after vigorous stirring, washing the filter cake with a solvent wherein Cefmenoxime hydrochloride is insoluble at a temperature less 20° C., and drying; 2) placing the filter cake into ammonium hydroxide, controlling the pH value less than 9 with a gentle agitation to obtain Cefmenoxime acid solution in ammonium hydroxide, and then filtering out the precipitate; 3) adding hydrochloric acid at a concentration of 0.5-4 mol/L to Cefmenoxime acid solution in ammonium hydroxide slowly and controlling the temperature between 30-60° C. and the final pH between 0.5-3.0, and then cooling down to a minimum of 10° C. and standing still to allow crystallization, filtrating and vacuum drying.
    Type: Grant
    Filed: August 11, 2011
    Date of Patent: November 25, 2014
    Assignee: Hainan Lingkang Pharmaceutical Co., Ltd.
    Inventor: Linggang Tao
  • Patent number: 8871927
    Abstract: A novel process for refining Ceftizoxime sodium compound, comprises the steps of: 1) dissolving crude Ceftizoxime sodium in water, and extracting with cyclohexane or ethyl acetate, followed by separating the organic phase containing impurities, producing an aqueous phase containing Ceftizoxime sodium; 2) adding ammonia or ammonium hydroxide into the above aqueous phase while stirring, followed by filtrating the precipitate, producing an aqueous filtrate containing Ceftizoxime sodium; 3) adding an alcoholic solvent in the aqueous solution and recrystallizing under controlled temperature, followed by centrifuging and washing the resultant crystals, producing the refined Ceftizoxime sodium after drying; and 4) optionally returning the mother liquid of the recrystallization process to step 3).
    Type: Grant
    Filed: August 11, 2011
    Date of Patent: October 28, 2014
    Assignee: Hainan Lingkang Pharmaceutical Co., Ltd.
    Inventor: Linggang Tao
  • Patent number: 8859761
    Abstract: It discloses a novel process for refining cefamandole nafate, comprising: 1) adsorbing cefamandole nafate with strongly acidic ion exchange resin, followed by eluting the resin and collecting the eluate, to provide a primary purified cefamandole acid after concentration under reduced pressure; 2) neutralizing the primary purified cefamandole acid with an aqueous solution of sodium hydroxide or an aqueous solution of basic salt of sodium, followed by adjusting the pH value and filtrating out the insoluble substances with heating, thereby providing a secondary purified aqueous solution of cefamandole nafate; and 3) adding ethanol in a volume ratio between ethanol and water of 4:6 into the aqueous solution, to allow recrystallization under controlling the temperature, to provide a tertiary purified cefamandole nafate. The refined cefamandole nafate product has a purity of no less than 99.5%, mostly no less than 99.6%, with significantly low content of heavy metals.
    Type: Grant
    Filed: March 17, 2011
    Date of Patent: October 14, 2014
    Assignee: Hainan Lingkang Pharmaceutical Co., Ltd.
    Inventor: Linggang Tao
  • Patent number: 8853389
    Abstract: The present invention relates to a novel process for refining Cefmetazole sodium, comprising the steps of: 1) dissolving Cefmetazole sodium material in water, and extracting after adding a water-immiscible organic solvent(s), followed by separating the organic phase containing impurities, to provide an aqueous phase containing Cefmetazole sodium; 2) treating by adding an alkoxide of alkali metal or alkaline earth metal into the above aqueous phase, followed by filtrating the precipitate, to provide an aqueous filtrate; and 3) adding ethanol or acetone in the aqueous solution and recrystallizing, followed by centrifuging and washing the resultant crystals, to provide the refined and purified Cefmetazole sodium after drying. The purity of Cefmetazole sodium material can be greatly improved by the process of the present invention.
    Type: Grant
    Filed: April 14, 2011
    Date of Patent: October 7, 2014
    Assignee: Hainan Lingkang Pharmaceutical Co., Ltd.
    Inventor: Linggang Tao
  • Publication number: 20140275550
    Abstract: A process for purifying lansoprazole comprises 1) loading crude lansoprazole material onto a macroporous resin column; 2) concentrating the eluate from the column in a crystallization vessel by vacuum; 3) seeding lansoprazole crystal; 4) crystallizing the lansoprazole; 5) separating the precipitated crystals. The process especially has large processing capacity, can be carried out continuously and therefore suitable for industrial production, improving the quality of formulated products and reducing side effects.
    Type: Application
    Filed: December 27, 2011
    Publication date: September 18, 2014
    Applicant: HAINAN LINGKANG PHARMACEUTICAL CO., LTD.
    Inventor: Linggang Tao