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组装了一种新型的微波辅助旋转回流装置,该装置的基本原理与微波辅助溶剂萃取的原理相同,但采用了旋转的技术以加速提取。应用该装置以正交实验筛选优化叶下珠中有机酸的提取工艺,并利用毛细管电泳技术分离测定了提取液中有机酸的含量以评价提取效果。最佳提取工艺:乙醚为溶剂,微波功率800W,提取时间4 min,溶剂用量300 mL。在该提取条件下,平行5次提取叶下珠中丁二酸、原儿茶酸、没食子酸、咖啡酸、阿魏酸的平均含量分别为42.2、103.5、436.2、123.8、67.4μg/g,相对标准偏差为0.87%~3.7%,加标回收率为94%~104%。将该法与常规的微波辅助提取法及回流提取法进行比较,结果表明,微波辅助旋转回流提取法提取效率明显优于其它2种方法。
A new type of microwave-assisted rotary reflux device has been assembled. The basic principle of this device is the same as that of microwave assisted solvent extraction, but a spin-on technique is used to speed up the extraction. The device was used to screen and optimize the extraction process of organic acids in Phyllanthus urinaria by orthogonal experiment. The content of organic acids in the extract was determined by capillary electrophoresis to evaluate the extraction efficiency. The best extraction process: ether as solvent, microwave power 800W, extraction time 4 min, the amount of solvent 300 mL. Under this extraction condition, the average contents of succinic acid, protocatechuic acid, gallic acid, caffeic acid and ferulic acid in Phyllanthus urinaria were 42.2,103.5,436.2,123.8,67.4μg / g, The relative standard deviations (RSDs) ranged from 0.87% to 3.7%. The spiked recoveries ranged from 94% to 104%. Comparing this method with the conventional microwave-assisted extraction and reflux extraction, the results show that the extraction efficiency of microwave-assisted rotary reflux extraction is obviously better than the other two methods.