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刊物信息

期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nicpbp.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

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三叶木通活性成分的TLC鉴别及含量测定

TLC identification and HPLC determination of the active constituents in Akebia trifoliata(Thunb.)Koidz.

作者(英文):
分类号:R917
出版年·卷·期(页码):2019,39 (4):638-643
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

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。

-----英文摘要:---------------------------------------------------------------------------------------

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.

-----参考文献:---------------------------------------------------------------------------------------

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