乙醇-水溶液中非达霉素结晶工艺研究

Crystallization process of fidaxomicin in the ethanol-water solvent

目的：开发一种非达霉素晶体制备方法。方法：以乙醇-水为结晶溶剂，使用梅特勒-托利多结晶仪对结晶浓度、温度、搅拌速度及降温曲线进行优选。结果：在乙醇．水比例为70％，结晶温度为2～8℃，搅拌速度为5～10r·min^-1时，可以得到非达霉素晶体，该晶体的X射线粉末衍射光谱特征峰以20表示位于3．324，7．745，9．989，10．607，13．954，14．475，15．355，15．855，18．800，19．999，20．321，22．245，23．104，24．028，24．446处，熔点为153．7oC。结论：建立了一种非达霉素晶体的制备方法，该方法操作简单，溶剂易回收，适合工业化生产。

Objective： To develop a preparation method of fidaxomicin crystals. Methods： In the ethanolwater solvent, the crystal concentration, temperature, stirring speed and cooling curves were optimized using a Met- tler Toledo crystal instrument. Results： Under the conditions of crystalline concentration 70% , temperature 2 8 ℃ and stirring speed 5 - 10 r. min^-1, fidaxomiein crystals were obtained. The X-ray powder diffraction spectrum characteristic peaks of the crystal with 20 were found at 3. 324, 7. 745, 9. 989, 10. 607, 13. 954, 14. 475, 15. 355, 15. 855, 18. 800, 19. 999, 20. 321, 22. 245, 23. 104, 24. 028, and 24. 446. The melting point was 153.7 ~C. Conclusion： The preparation method of fidaxomicin crystals is set up, and it is simple operation, easy to recycle solvent and suitable for industrial production.