中空纤维膜液相微萃取-HPLC法测定复方穿心莲片中脱水穿心莲内酯含量

Determination of dehydroandrographolide in compound Chuanxinlian tablets by hollow fiber solvent microextraction-HPLC

目的:建立一种新方法—中空纤维膜液相微萃取-高效液相色谱法测定复方穿心莲片中脱水穿心莲内酯的含量。法:将样品用甲醇浸泡、超声、过滤后,配成样品溶液。经用装有正辛醇的中空纤维膜进行液相微萃取后,用 HPLC 法测定复穿心莲片中脱水穿心莲内酯的含量,色谱柱为 Waters symmetry C_(18)柱(150 mm×3.9 mm,5μm),流动相为甲醇-水(60:40结果:脱水穿心莲内酯浓度范围在100～8000 ng·mL^(-1)内线性关系良好,其加样回收率>96.0%,RSD<3.8%。结论:通液相微萃取后,能有效地去除检测复方穿心莲片中的干扰物质,样品处理无需经过中性氧化铝柱纯化,获得了较高的选择性该方法简便、快速,与不经过液相微萃取的液相色谱方法相比,灵敏度提高约128倍,是测定复方穿心莲片中脱水穿心莲内含量的一种好方法。

Objective： To develop a new method for the determination of the content of dehydroandrographolide （DAP） in compound Chuanxinlian tablets by HPLC following hollow fiber solvent microextraction. Method： The sample was immersed in methanol under sonication. Then a hollow fiber containing octanol inside was placed in the sample solution to perform microextraction. The extracted sample was analyzed by HPLC with UV detection. Chromatography was performed using a Symmetry C18 column （150 mm ×3. 9 mm,5 μm）. The mobile phase was a mixture of methanol and water（60：40）. Results：The calibration curves of DAP were linear in range of 100 to 8000 ng· mL^-1. The method recoveries were over 96. 0% with RSD less than 3. 8%. Conclusion：By using hollow fiber based microextraction, interference for the determination of dehydroandrographolide was eliminated effectively. This method is specific, simple, fast, sensitive and suitable for the determination of DAP in complex tablets with little solvent consumption.