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___

摘要 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的方法。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，以环已烷-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 °C加热显色，采用双波长薄层扫描法，λ_s=530 nm,λ_R=700 nm，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1.3，二者在0.2 μg～3.9 μg 点样量范围内与扫描峰面积值呈良好的线性关系 (r_齐墩果酸=0.9996，r_熊果酸=0.9994，n＝6)；回收率分别为97.7%和98.5%，RSD分别为2.9%和3.0%。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，解决了多年来一直困惑实验工作者的二者混杂的问题，方法简便、易行，准确。

Abstract Objectives: Create a in situ Pretreatment – TLCS to separate and determinate 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 °C for 5 min. Double wavelength TLCS was used, λ_s=530 nm,λ_R=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 μg of oleanolic and ursolic acids (r_{oleanolic acid}=0.9996，r_{ursolic acid}=0.9994，n＝6). The average recovery of oleanolic acid and ursolic acid were 97.7% and 98.5%, RSD were 2.10% and 3.0%. Conclusion The presented method was validated for assay. The results were found to be satisfactory.