三叶木通活性成分的TLC鉴别及含量测定

目的：建立三叶木通药材中皂苷PH、皂苷PJ1的TLC鉴别和皂苷PH、akemisaponin E、皂苷PJ1和scheffoleoside A的HPLC含量测定方法。方法：TLC法，展开剂为三氯甲烷-甲醇-甲酸（20：10：1），显色剂为10%硫酸乙醇溶液；HPLC法，采用依利特C₁₈色谱柱（250 mm×4.6 mm，5 μm），以乙腈-水（21：79）为流动相，流速1.0 mL·min^-1，检测波长200 nm，柱温30℃。结果：三叶木通药材中皂苷PH、皂苷PJ1的TLC分离效果均较好；HPLC法测得皂苷PH、akemisaponin E、皂苷PJ1和scheffoleoside A的进样量分别在0.201~5.025 μg（r=0.999 9）、0.076~1.888 μg（r=0.999 9）、0.224~5.608 μg（r=1.000 0）和0.041~1.035 μg（r=0.999 9）范围内与峰面积呈现良好的线性关系；平均回收率（n=3）分别为99.8%、98.2%、99.5%、98.9%，RSD分别为0.46%、1.2%、0.40%和1.0%；5批样品中皂苷PH、akemisaponin E、皂苷PJ1和scheffoleoside A的含量范围分别为2.094~3.928、0.956~1.418、2.958~4.472和0.526~0.797 mg·g^-1。结论：此方法简便易行，重复性好，可作为三叶木通药材质量控制指标。

Objective:To establish TLC identification method of saponin PH and saponin PJ1, and HPLC determination method of saponin PH, akemisaponin E, saponin PJ1 and scheffoleoside A.in Akebia trifoliata (Thunb.) Koidz. Methods:TLC:Silica-G-CMCNa plate was used with chloroform-methanol-formic acid (20:10:1) as the developing solvent and 10% sulfuric acid ethanol solution as the colorimetric agent. HPLC:Separation was performed on an ELITE C₁₈ (250 mm×4.6 mm, 5 μm) column and the mobile phase composed of acetonitrile-water (21:79) at a flow rate of 1.0 mL·min^-1. The detection wavelength was 200 nm, and the column temperature was set at 30℃. Results:Saponin PH and saponin PJ1 in A. trifoliata (Thunb.) Koidz could be separated by TLC. The linear ranges of saponin PH, akemisaponin E, saponin PJ1 and scheffoleoside A were 0.201-5.025 μg (r=0.999 9), 0.076-1.888 μg (r=0.999 9), 0.224-5.608 μg (r=1.000 0) and 0.041-1.035 μg (r=0.999 9), respectively. The average recoveries (n=3) were 99.8% (RSD=0.46%), 98.2% (RSD=1.2%), 99.5% (RSD=0.40%) and 98.9% (RSD=1.0%). The contents of saponin PH, akemisaponin E, saponin PJ1 and scheffoleoside A in five batches of samples were 2.094-3.928, 0.956-1.418, 2.958-4.472 and 0.526-0.797 mg·g^-1. Conclusion:This method is specific, accurate and reproducible, and can be used in control the quality of A. trifoliata (Thunb.) Koidz.

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