芥子碱的提取纯化及HPLC法含量测定

Extraction,purification and determination of sinapine from Semen Sinapis Albae by HPLC

目的:从白芥子中提取纯化芥子碱硫氰酸盐,并测定其含量,为中药外用制剂提供高纯度的天然透皮吸收促进剂。方法:白芥子脱脂,用不同浓度乙醇提取、浓缩物加20%硫氰酸钾溶液析晶,用蒸馏水反复重结晶。采用高效液相色谱法测定含量。色谱柱:Agilent TC-C18(4.6 mm×250 mm,5μm),流动相:2%醋酸-乙腈(15∶85),检测波长:326 nm,流速:1.0 m L/min,柱温:30℃。结果:用80%乙醇提取,蒸馏水和20%硫氰酸钾溶液比例为4∶1时,所得芥子碱呈浅黄色针状结晶,得率0.51%,含量95.70%。结论:采用本法提取纯化芥子碱,方法简单,纯度高,可为中药外用制剂选择天然透皮促进剂提供参考。

Objective:To extract and purify sinapine thiocyanate from Semen Sinapis Albae and determine its content,so as to provide provide high purity natural penetration enhancers for external application of Chinese herbal medicine.Methods:Semen Sinapis Albae was defatted by petroleum ether,extracted with different concentrations of alcohol,and crystallized by 20 %solution of potassium thiocyanate,then water and potassium thiocyanate solution were used to recrystallizated repeatedly.The separation was performed on Agilent TC-C18column(4.6 mm × 250 mm,5 μm) at 30 ℃ with a mobile phase of 2% acetic acid-acetonitrile(15 ∶85),and the flow rate was 1.0 m L/min,Photodiode Array Detector(PAD) was used and the wavelength of detector for sinapine thiocyanate was set at 326 nm.Results:The yield of sinapine thiocyanate was 0.51% with content of95.70% when it was extracted with 80% of ethanol,and the ratio of distilled water to 20% potassium thiocyanate was 4 ∶1.Conclusion:The method for sinapine thiocyanate extraction and purification is simple with high purity,which could provide a reference for choose natural penetration enhancers for external application of Chinese herbal medicine.