路路通药材中桦木酮酸定性定量方法的研究

目的:建立路路通药材中桦木酮酸的鉴别和含量测定方法。方法:薄层色谱法鉴别。药材用醋酸乙酯提取,在以羧甲基纤维素钠为粘合剂的硅胶G薄层板上,用石油醚(60～90℃)-丙酮(17∶3)展开,磷钼酸显色;高效液相色谱法进行含量测定。样品用无水乙醇超声提取。DiamonsilC₁₈柱,甲醇水冰醋酸(87∶13∶0.1)为流动相,流速1.0mL·min^-1,柱温35℃,蒸发光散射检测器蒸发管温度82℃,气体流速1.25L·min^-1。结果:薄层色谱鉴别重现性好;在上述液相色谱条件下,桦木酮酸获较好分离,进样量在0.65～3.25μg其对数与峰面积对数呈线性关系(r=0.9997),加样回收率为98.0%,重复性为2.5%。对收集的11批商品药材进行了定性鉴别和含量测定。结论:本研究为路路通质量标准的建立提供可借鉴的方法。

Qualitative and quantitative methods of betulonic acid in fruits of Liquidambar formosana

OBJECTIVE: To develop the identification and assay methods for betulonic acid in fruits of Liquidambar formosana. METHOD: TLC method was used for identification with silica gel G plate and petroleum ether(60-90 degrees C)-acetone (17:3) as a developing solvent. Betulonic acid in ethanol extract was separated on the ODS column with methanol-water-glacial acetic acid (87:13:0.1) as mobile phase. Flow-rate was 1.0 mL x min(-1), and column temperature 35 degrees C. ELSD drift-tube temperature was 82 degrees C, and gas flow 1.25 L x min(-1). RESULT: The qualitative method is repeatable. Betulonic acid in ethanol extracts is well separated, relationship of logarithms of injection amount and peak area is linear (r = 0.9997) within the range of 0.65-3.25 microg. The average recovery is 98.0% and RSD of repeatability is 2.5%. 11 crude drugs purchased from different areas in the country were identified and quantified with the methods. CONCLUSION: The methods and data could be used for quality control of fruits of L. formosana.