穿心莲内酯超临界CO_2重结晶工艺初探

Primary study on the technology of andrographolide recrystallization by using supercritical CO_2

采用单因素实验法探讨超临界CO2重结晶压力、温度、时间对穿心莲内酯的纯度和结晶率的影响,并借助扫描电镜进行晶体形貌考察,利用高效液相色谱仪进行纯度检测。结果表明,采用超临界CO2重结晶技术得到的穿心莲内酯晶体形貌更加细小,并呈絮状分布在结晶板上;选择较佳纯化工艺参数为重结晶压力14MPa,温度55℃,时间60min,CO2流量20L/min时,得到的穿心莲内酯纯度达90%以上,结晶率超过45%。

The effect of pressure, temperature and time of secondary grads crystallization on the purity and the crystal ratio of andrographolide were investigated via single factor experiments, observing shape of crystal with scanning electron microscopy(SEM), determining purity of andrographolide by high pressure liquid chromatography(HPLC). The result showed that the particle of andrographolide was much smaller, moreover, the crystal of andrographolide was distributed in floccule on crystallization board; When the optimized parameters(pressure 14 MPa, temperature 55℃, time 60 min) were selected the content of andrographolide was more than 90%, the crystal ratio was more than 45%.