原位预处理-薄层扫描法同时测定女贞子中齐墩果酸与熊果酸的含量

Simultaneous determination of oleanolic acid and ursolic acid in Fructus Ligustri Lucidi by in situ pretreatment-TLCS

目的:建立原位预处理-薄层扫描法分离测定女贞子中齐墩果酸和熊果酸含量。方法:样品溶液点样后,以1%碘-二氯甲烷溶液对斑点进行预处理后,以环己烷-二氯甲烷-乙酸乙酯-冰醋酸(20∶5∶8∶0.1)为展开剂,以10%硫酸乙醇溶液为显色剂,105℃加热显色,采用双波长薄层扫描法,λs=530nm,λR=700nm,测得峰面积积分值,外标两点法计算含量,并进行了方法学验证。结果:齐墩果酸和熊果酸薄层色谱分离度为1.3,二者点样量在0.2～3.9μg范围内与扫描峰面积呈良好的线性关系(r齐墩果酸=0.9996,r熊果酸=0.9994,n=6);回收率(n=3)分别为95.8%～99.7%和98.5%～100.8%。结论:本文采用薄层色谱法对女贞子中齐墩果酸、熊果酸进行检测,解决了多年来困扰实验工作者的二者混淆的问题,方法简便、易行,准确。

Objective：To develop an in situ pretreatment -TLCS for separateation and determination of oleanolic acid and ursolic acid. Method： The samples were treated directly on the chromatographic plate by 1% iodine solution in methylene dichloride, and developed with the mobile phase consisting of cyclohexane - methylene dichloride -ethyl acetate - glacial acetic acid （20： 5： 8： 0：1 ,v/v/v/v）. The plates were sprayed with 10% ethanol solution of sulfuric acid and heated to 105 ℃ for 5 min. Double wavelengths TLCS was adopted, λs = 530 nm ,λR = 700 nm. Results ：The TLC resolution of oleanolic acid and ursolic acid was 1.3. The methodological study showed a good linearity correlation at the range between 0. 2 - 3.9 IJ, g of oleanolic and ursolic acids （ roleanolic acid = 0. 9996, rursolic acid =0. 9994,n =6）. The average recoveries（n =3） of oleanolic acid and ursolic acid were 95.8% -99.7% and 98. 5% - 100. 8%. Conclusion：This method is validated for assay. It is simple and accuracy.