公开(公告)号：US20240344954A1

公开(公告)日：2024-10-17

申请号：US18657771

申请日：2024-05-07

申请人： TIANJIN UNIVERSITY ,  ZHEJIANG HUAKANG PHARMACEUTICAL CO., LTD. ,  ZHEJIANG INSTITUTE OF TIANJIN UNIVERSITY (SHAOXING)

发明人： Junbo GONG ,  Mian LI ,  Mingyang CHEN ,  Wulong YANG ,  Jiahui LI ,  Mingxuan LI ,  Qiang WU ,  Baohong HOU ,  Qiuxiang YIN

IPC分类号： G01N15/06

CPC分类号： G01N15/06

摘要： The present disclosure provides a technology field of caking of crystal particles, and in particular relates to a method for predicting a critical caking cycle of crystal particle. The method includes: establishing a CHS crystal bridge growth model database of a crystal particle with a same type of crystal particle to be predicted firstly, selecting existed data in the corresponding CHS crystal bridge growth model database based on an equivalent particle radius, a stored ambient temperature, and an environmental high and low humidity cycle condition of the crystal particle to be predicted, respectively, and calculating the critical caking cycle according to experience calculation equations, wherein a result obtained by calculation is a predicted critical caking cycle of the crystal particle to be predicted. The present disclosure has characteristics of time-saving, convenience, good universality, and high prediction accuracy, which can quickly predict the critical caking cycle of multi-particle crystal particle products under different humidity storage conditions within a week, resulting in greatly reducing time costs and providing guidance for storage of industrial crystal particle products.

公开(公告)号：US20170197937A1

公开(公告)日：2017-07-13

申请号：US15304861

申请日：2015-11-20

申请人： TIANJIN UNIVERSITY ,  HAINAN LINGKANG PHARMACEUTICAL CO., LTD

发明人： Hongxun HAO ,  Linggang TAO ,  Shen JIANG ,  Yongli WANG ,  Jingkang WANG ,  Jun LV ,  Qiuxiang YIN ,  Baohong HOU ,  Zhao XU ,  Chuang XIE ,  Zhao WANG

IPC分类号： C07D401/12

CPC分类号： C07D401/12 ,  A61K9/0019 ,  A61K31/4439 ,  C07B2200/13

摘要： A novel crystalline form is defined by using diffraction angle 2θ° 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.

公开(公告)号：US20210300892A1

公开(公告)日：2021-09-30

申请号：US17208043

申请日：2021-03-22

申请人： Tianjin University

发明人： Ying BAO ,  Feng ZHANG ,  Peihua LIANG ,  Baohong HOU ,  Chuang XIE ,  Ting ZHANG ,  Yinghui CHAI

IPC分类号： C07D401/04

摘要： The disclosure relates to etoricoxib solvates and a preparation method thereof. A solvent is a hydrogen bond donor solvent with a polarity value π* ranging from 60 to 100 or a hydrogen bond acceptor solvent with a polarity value π* ranging from 92 to 100. Solvents with a polarity value π* within the above range all can form corresponding etoricoxib solvates with etoricoxib. The etoricoxib solvate can be prepared by cooling crystallization or suspension crystallization. A 1,2-propanediol solvate of etoricoxib and a dimethyl sulfoxide (DMSO) solvate of etoricoxib provided in the present disclosure have high thermal stability, unique crystal form, large size, concentrated distribution, and prominent flowability and is safe, pharmaceutically acceptable, and not easy to agglomerate. Compared with etoricoxib, the etoricoxib solvates exhibit significantly improved solubility. Moreover, preparation of the solvates requires low consumption in time, energy, and solvent, and has high efficiency, with a molar yield higher than 90%.

公开(公告)号：US20170044137A1

公开(公告)日：2017-02-16

申请号：US15305653

申请日：2015-11-20

申请人： TIANJIN UNIVERSITY ,  HAINAN LINGKANG PHARMACEUTICAL CO., LTD

发明人： Ying BAO ,  Linggang TAO ,  Long LI ,  Hongxun HAO ,  Jun LV ,  Baohong HOU

IPC分类号： C07D401/12

CPC分类号： C07D401/12 ,  C07B2200/13

摘要： 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 2θ 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.

摘要翻译： 本发明公开了奥美拉唑钠半水合物及其制备方法，其中每摩尔奥美拉唑钠半水合物含有0.5摩尔水，其X射线衍射图包含衍射角2θ为6.26°±0.1°，11.10°±0.1°的特征峰 °，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°和28.08°±0.1°。 将奥美拉唑钠水合物的原料加入到有机溶剂中，在25〜60℃的恒温下搅拌2〜9小时，然后过滤并干燥后提供奥美拉唑钠半水合物。

公开(公告)号：US20170044184A1

公开(公告)日：2017-02-16

申请号：US15304824

申请日：2015-11-20

申请人： TIANJIN UNIVERSITY ,  HAINAN LINGKANG PHARMACEUTICAL CO., LTD

发明人： Hongxun HAO ,  Linggang TAO ,  Zhihong SUN ,  Baohong HOU ,  Jun LV ,  Qiuxiang YIN ,  Yongli WANG ,  Junbo GONG ,  Chuang XIE ,  Ying BAO

IPC分类号： C07D501/60

CPC分类号： C07D501/60 ,  C07B2200/13 ,  C07D501/12 ,  C07D501/28

摘要： 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.

摘要翻译： 尖晶石化合物的新型结晶形式及其制备方法，其X射线粉末衍射图和差示扫描量热法热分析图表征。 在溶剂中在30〜45℃的温度下溶解纯度为98％以上的头孢硫脒化合物，形成浓度为0.05〜0.2g / mL的溶液，然后加入溶剂 溶剂，其中溶剂量为溶剂量的3〜5倍（体积）; 然后以0.2〜1℃/分钟的速度将溶液冷却至0〜10℃; 继续搅拌1〜3小时，分离得到的固液悬浮液，干燥后提供新型的头孢噻肟化合物结晶形式。

公开(公告)号：US20170037054A1

公开(公告)日：2017-02-09

申请号：US15302944

申请日：2014-12-31

申请人： SHENZHEN SALUBRIS PHARMACEUTICALS CO., LTD ,  Tianjin University

发明人： Junbo GONG ,  Qi WANG ,  Qiuxiang YIN ,  Jingkang WANG ,  Xiaopeng Song ,  Baohong HOU ,  Liting LIAO ,  Duanming TAN ,  Ziyuan DI

IPC分类号： C07D495/04

CPC分类号： C07D495/04 ,  A61K31/425 ,  A61K31/4365 ,  A61K31/4743 ,  C07B2200/13

摘要： This invention provides a new preparation method of Clopidogrel Hydrogen Sulfate spherical crystal form I, using single 2-butanol as solvent, controlling the concentration, addition way and addition speed of sulfuric acid used to salify to shorten the process time, thus separating out Clopidogrel Hydrogen Sulfate from solution system stably with spherality. And the Clopidogrel Hydrogen Sulfate obtained complies with the requirements of the follow-up process on residual solvent, bulk density and mobility.

摘要翻译： 本发明提供了使用单一2-丁醇作为溶剂的氯吡格雷硫酸氢盐球形晶体I的新制备方法，控制用于成盐的硫酸的浓度，添加方式和加入速度以缩短处理时间，从而分离氯吡格雷氢 硫酸盐溶液体系稳定，具有球形度。 获得的氯吡格雷硫酸氢盐符合残留溶剂，体积密度和流动性的后续过程的要求。

公开(公告)号：US20170050982A1

公开(公告)日：2017-02-23

申请号：US15305661

申请日：2015-11-20

申请人： TIANJIN UNIVERSITY ,  HAINAN LINGKANG PHARMACEUTICAL CO., LTD

发明人： Hongxun HAO ,  Linggang TAO ,  Fang He ,  Baohong HOU ,  Jingkang WANG ,  Jun LV ,  Qiuxiang YIN ,  Yongli WANG ,  Junbo GONG ,  Chuang XIE ,  Ying Bao

IPC分类号： C07D501/36 ,  C07D501/12

CPC分类号： C07D501/36 ,  C07B2200/13 ,  C07D501/12

摘要： A novel crystalline form is defined by diffraction angle 2θ° 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.

摘要翻译： 新型结晶形式由X射线粉末衍射图的衍射角2θ°和差示扫描量热法（DSC）的特征峰定义。 头孢丹多奈非糖酸盐的新型结晶形式如下制备：将固体状态的头孢马替奈啡钠加入到有机溶剂中，形成浓度为0.04〜0.3g / ml的悬浮液，在40〜50℃下搅拌悬浮液一段时间 的时间，然后以一定的冷却速度冷却至5〜15℃，继续搅拌一段时间，然后抽滤所得悬浮液，得到的滤饼为头孢丹多，作为湿产品干燥至恒定 重量，以提供新颖的头孢曼陀螺Nafate的结晶形式作为最终产品。