五味子宁神合剂的质量控制
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摘要
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 C_(18) SPE cartridge. The column was Waters C_(18)(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.
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 C_(18) SPE cartridge. The column was Waters C_(18)(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.
引文
1常翠,饶曼妮,杨宏图,等.五昧子宁神合剂治疗失眠的临床观察[J].中国医疗前沿,2007,11(22):118-119
2 付学军,常翠,赵奎.五味子宁神合剂治疗中青年失眠临床研究[J].医学研究杂志,2007,5(5):107-108
3 杨宏图,常翠,饶曼妮.五味子宁神口服液的含量测定[J].现代医院,2005,11(1):64-65
4 周芳,孙成,刘浩.改进固相萃取预处理操作过程的探讨[J].江苏环境科技,2008,21(1):71-78
5 中国药典[S]. 2015年版.四部. 5759
2 付学军,常翠,赵奎.五味子宁神合剂治疗中青年失眠临床研究[J].医学研究杂志,2007,5(5):107-108
3 杨宏图,常翠,饶曼妮.五味子宁神口服液的含量测定[J].现代医院,2005,11(1):64-65
4 周芳,孙成,刘浩.改进固相萃取预处理操作过程的探讨[J].江苏环境科技,2008,21(1):71-78
5 中国药典[S]. 2015年版.四部. 5759