五味子宁神合剂的质量控制

Quality Control of Wuweizi Ningshen Mixture

目的:采用固相萃取法与高效液相色谱法合用,去除五味子宁神合剂中影响测定的杂质,建立五味子醇甲含量测定,对处方中的黄芪进行TLC定性鉴别。方法:采用C_(18)SPE小柱纯化样品,Waters C_(18)色谱柱(150 mm×3. 9 mm,5μm);流动相:甲醇-水(55∶45);流速:1. 0 ml·min^(-1);检测波长:250 nm。TLC色谱定性鉴别采用硅胶G薄层板上,以氯仿-甲醇-水(15∶7∶2)为展开剂。结果:五味子醇甲在10～50μg·ml^(-1)范围内其线性关系良好(r=0. 999 4),平均回收率99. 34%,RSD=1. 55%(n=9)。黄芪与对照品色谱相应的位置上,显相同的颜色。结论:优化后的方法简便、准确、快速、重复性好。

Objective: To remove the impurities affecting the determination in Wuweizi Ningshen mixture,establish the determination method for schizandrin and qualitatively identify Astragali Radix by TLC. Methods: The sample was purified by using a C18 SPE cartridge. The column was Waters C18(150 mm × 3. 9 mm,5 μm). The mobile phase was methanol-water(55 ∶ 45). The flow rate was 1. 0 ml·min-1. The detection wavelength was 250 nm. The TLC was carried out on a silica gel G thin plate with chloroform-methanol-water(15 ∶ 7 ∶ 2) as the developing agent. Results: The linear range of schisandrin A was 10-50 μg·ml-1(r = 0. 999 4),the average recovery was 99. 34%,and the RSD was 1. 55%( n = 9). Astragalus and the reference standard showed the spot with the same color at the corresponding position in TLC. Conclusion: The optimized method is simple,accurate,fast and reproducible.