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硫酸氢氯吡格雷的几个已报道的晶型中,相对于晶型II,晶型I的热稳定性较差,在高温高湿条件下会自发地转变为晶型I I,因而晶型I在生产中难以得到热稳定性好的产品。本文提出利用离心力辅助析晶的方法能生产出高纯度,稳定性好的晶型I产品。所得到的产品分别用粉末X射线衍射仪(PXRD),差示扫描热量仪(DSC)和扫描电镜显微镜(SEM)进行了表征。结果显示:离心力辅助析晶比用传统反溶剂析晶方法得到的晶型I结晶度有明显增加,晶粒生长得更大更完整。通过长期稳定性实验,证明新工艺所得到的产品具有较好的热稳定性,在高温高湿的环境下能长时间储存不变质。
In several of the reported crystalline forms of clopidogrel hydrogen sulfate, Form I is less thermostable with respect to Form II and spontaneously converts to Form II under conditions of high temperature and high humidity, thus Form I Difficult to get in the production of good thermal stability of the product. In this paper, the use of centrifugal force assisted crystallization method can produce high purity, good crystal form I products. The obtained products were characterized by powder X-ray diffractometer (PXRD), differential scanning calorimetry (DSC) and scanning electron microscopy (SEM). The results show that the crystallinity of Form I obtained by centrifugal assisted crystallization is obviously higher than that obtained by the traditional method of anti-solvent crystallization, and the grains grow bigger and more complete. Through the long-term stability experiment, it is proved that the product obtained by the new process has better thermal stability and can be stored for a long time without deterioration in a high-temperature and high-humidity environment.