微波辅助-旋转回流提取仪的组装及其在叶下珠有机酸提取中的应用

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800 W,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、67.4 μg/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.

Construction of Microwave-assisted Circumrotation Reflux Extraction Apparatus and Its Application in Extracting Organic Acid from Phyllanthus Urmaria L.

A new kind of microwave-assisted circumrotation reflux extraction device was constructed and used to extract the organic acid from Phyllanthus urmaria L.The device used the same extraction principle as the microwave-assisted solvent extraction except that using circumrotation techniques as auxiliary stirrer to accelerate the process.The experimental conditions were studied with orthogonal design.The extraction solvent,microwave power and irradiation time were investigated and optimized.Samples were analyzed with a capillary electrophoresis method to determine the yield of organic acids and the extraction efficiency of the method was evaluated.The results indicated that optimal extracting conditions were as follows:300 mL anhydrous ether as solvent,microwave power of 800 W,extracting for 4 min.Under the optimal conditions,five organic acids,e.g.succinic acid(SA),protocatechuic acid(PA),gallic acid(GA),caffeic acid(CA) and ferulic acid(FA),were extracted from Phyllanthus urmaria L. sample,and their average content were 42.2,103.5,436.2,123.8,67.4 μg/g,respectively,with RSDs in the range of 0.87%-3.7%.The recoveries of five compounds from the Phyllanthus urmaria L. sample were between 94%and 104%.Compared with other extraction methods such as reflux extraction and microwave-assisted extraction,the microwave-assisted circumrotation reflux extraction was simple and rapid,and showed high extraction efficiency and low consumption of solvent.