Recrystallization and Micronization of 10-Hydroxycamptothecin by Supercritical Antisolvent Process

Recrystallization and Micronization of 10-Hydroxycamptothecin by Supercritical Antisolvent Process
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超临界反溶剂法重结晶和微粉化10-羟基喜树碱

DOI:
10.1021/ie2020334
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发表时间:
2012-01
期刊:
Industrial & Engineering Chemistry Research
影响因子:
--
通讯作者:
Wang, Wei
Wang, Wei
中科院分区:
其他
文献类型:
--
作者:
Jiang, Yanbin;Sun, Wenli;Wang, Wei

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使用二氯甲烷和乙醇的混合物作为溶剂,超临界二氧化碳(sc-CO2)作为反溶剂,在超临界反溶剂(SAS)工艺中研究了10-羟基喜树碱(HCPT)的重结晶和微粉化。使用选定的 OA16 (45) 正交阵列设计对五个因素(即混合溶剂的体积比、溶液中 HCPT 的浓度、HCPT 溶液的流速、沉淀压力和温度)进行了优化。使用激光衍射粒度分析、傅里叶变换红外 (FT-IR) 光谱、顶空气相色谱、扫描电子显微镜 (SEM)、粉末 X 射线衍射 (XRD)、差示扫描量热法 (DSC) 和热重分析 (TGA) 对未加工和加工的 HCPT 颗粒进行表征。结果表明,在最佳条件下,微粉化HCPT表现出更小的粒径,并且发现微粉化HCPT的质量中值直径...
Recrystallzation and micronization of 10-hydroxycamptothecin (HCPT) was investigated in a supercritical antisolvent (SAS) process using the mixture of dichloromethane and ethanol as the solvent, with supercritical carbon dioxide (sc-CO2) as the antisolvent. Five factors—i.e., the volume ratio of the mixed solvent, the concentration of HCPT in the solution, the flow rate of HCPT solution, the precipitation pressure, and the temperature—were optimized using a selected OA16 (45) orthogonal array design. The unprocessed and processed HCPT particles were characterized using laser diffraction particle size analysis, Fourier transform infrared (FT-IR) spectroscopy, headspace gas chromatography, scanning electron microscopy (SEM), powder X-ray diffraction (XRD), differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA). The results indicated that the micronized HCPT exhibited a much smaller particle size under the optimal conditions, and the mass median diameter of the micronized HCPT was foun...
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