至宝三鞭酒的薄层色谱鉴别及马钱苷的含量测定

Identification of Zhibao Sanbian Jiu by TLC and determination of Ursolie acid in Zhibao Sanbian Jiu by HPLC

目的:建立有效控制至宝三鞭酒质量的薄层色谱鉴别及含量测定。方法:用薄层色谱法(TLC)鉴别处方中的当归、蛇床子、何首乌、补骨脂、白芍、山茱萸、枸杞子、白术。用高效液相色谱法(HPLC)测定至宝三鞭酒中马钱苷的含量:色谱柱:Hypersi柱(250mm×4.6mm,5μm);流动相:四氢呋喃-乙晴-甲醇-0.05%磷酸溶液(1:8:4:48);检测波长:236nm;进样量:对照品进样10μL,样品进样20μL。结果:在薄层色谱上可检出当归、蛇床子2种药材的特征斑点并且无阴性干扰,可收入质量标准中。HPLC法测定中,在此色谱条件下,马钱苷在进样量为0.0185-0.7380μg范围内与峰面积呈良好的线性关系(r=0.9999,n=6)。平均加样回收率为99.6%,RSD为1.55%(n=9)。结论:TLC法鉴别至宝三鞭酒中当归、蛇床子准确,重现性好,可用于至宝三鞭酒的质量控制。HPLC法可控制至宝三鞭酒中马钱苷的含量,准确度高,重现性好,操作简便。

Objective： To establish a new method for identification by TLC and a HPLC method for the determination of Ursolie acid in Zhibao Sanbian Jiu.Methods： A TLC method was established for identification of Angelica sinensis（Oliv.）Diels,Cnidium monnieri（L.）Cusson,Polygonum multiflorum Thunb.,Psoralea corylifolia L.,Cornus officinalis Sieb.et Zucc,Lycium chinese Mill.,Paeonia lactiflora Pall.,Atractylodes macrocephala Koidz..Determination of Ursolie acid in Zhibao Sanbian Jiu by HPLC： Hypersi 5μ,4.6mm×250mm was used as chromatographic colum with tetrahydrofuran-acetonitrile-Methanol-0.05% Orthophosphoric acid solution（1：8：4：48）as the mobile phase.The detection wavelength was 236nm.Results： Characteristic spot of Angelica sinensis（Oliv.）Diels and Cnidium monnieri（L.）Cusson can be found without other disturbance,which can be used in quality lever.The calibration curve was linear in the range of 0.0185-0.7380μg（r=0.9999,n=6）,the average recovery rate was 99.6%,RSD was 1.55%（n=9）.Conclusion： The method is simple,accurate and reliable.It can be used for the quality control of Zhibao Sanbian Jiu.