超临界二氧化碳二次梯度结晶穿心莲内酯的研究

 探讨超临界CO2二次梯度结晶压力、温度、时间对穿心莲内酯纯度、结晶率的影响，并借助扫描电镜进行晶体形貌考察，利用高效液相色谱进行纯度检测。结果表明，超临界CO2二次梯度结晶穿心莲内酯的适宜工艺参数为压力14 MPa、温度55℃、时间60 min、CO2流量15 L·min-1，该工艺条件下得到的穿心莲内酯晶体形貌更加细小，在结晶板上呈絮状分布，纯度＞90%，最高达92.5%，结晶率为48.9%。

Study on Purifying Technology of Andrographolide by Supercritical Carbon Dioxide Secondary Gradient Crystallization

The effect of secondary gradient crystallizing pressure, temperature and time on the purity and the crystallization ratio of andrographolide was investigated via single factor experiments. The shape of crystal was observed with scanning electron microscopy (SEM). The purity of andrographolide was determined by high pressure liquid chromatography (HPLC). The result showed that the optimum parameters were pressure 14 MPa, temperature 55℃, time 60 min, and under these conditions the particle of andrographolide was much smaller, the crystal of andrographolide was distributed in floccule on crystal board, the purity of andrographolide was 92.5%, the crystallization ratio was 48.9%.