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目的:用薄层色谱法和高效液相色谱法建立朱砂安神丸定性鉴别和定量测定的方法,建立朱砂安神丸的质量标准。方法:黄连、当归和甘草展开系统分别采用甲苯-醋酸乙酯-甲醇-异丙醇-水(12∶6∶4∶4∶0.6),正己烷-醋酸乙酯-甲醇(9∶1∶0.2)和醋酸乙酯-甲酸-冰醋酸-水(15∶1∶1∶2)。采用C18(4.6mm×250mm,5μm)色谱柱,流动相为乙腈-0.05%磷酸二氢钾(25∶75),流速1.0mL.min-1,检测波长264nm,进样量10μL,柱温30℃。结果:盐酸小檗碱进样量在0.0252~0.504μg范围内呈良好的线性关系,回归方程Y=3971.4X+9.9657,r=0.999 8(n=5).平均加样回收率为99.3%,RSD为0.69%。结论:本鉴别方法专属性强,定量方法简便可靠,可有效控制该药的质量标准。
OBJECTIVE: To establish qualitative identification and quantitative determination of cinnabar and Anshen pill by TLC and HPLC, and to establish the quality standard of Cinnabar and Anshen Pills. METHODS: Coptis chinensis, Angelica sinensis and Glycyrrhiza uralensis were extracted with toluene - ethyl acetate - methanol - isopropanol - water (12:6:4:4:0.6), n - hexane - ethyl acetate - methanol ) And ethyl acetate-formic acid-glacial acetic acid-water (15: 1: 1: 2). The mobile phase consisted of acetonitrile-0.05% potassium dihydrogen phosphate (25:75), flow rate 1.0 mL · min-1, detection wavelength 264 nm, injection volume 10 μL and column temperature 30 ℃. Results: The calibration curve of berberine hydrochloride showed good linearity in the range of 0.0252-0.504μg, the regression equation was Y = 3971.4X + 9.9657, r = 0.999 8 (n = 5) .The average recovery was 99.3% RSD is 0.69%. Conclusion: The identification method is highly specific and simple and reliable, which can effectively control the quality standard of this medicine.