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目的建立五妙水仙膏的质量标准。方法采用薄层色谱法对处方中黄柏、五倍子、紫草3味药材进行定性鉴别;用高效液相法测定制剂中小檗碱的含量,采用AichromBond-AQ-C18色谱柱(4.6 mm×150 mm,5μm);流动相为乙腈-0.033 mol/L磷酸二氢钾(用磷酸调节pH值为3.0)-0.025 mol/L十二烷基硫酸钠(48∶30∶25),流速1.0 ml/min,柱温30℃;检测波长345 nm;进样量20μl。用高效液相法对所建立的小檗碱含量测定方法进行方法学验证,证明采用的含量测定方法适合于相应分析要求。验证内容有:线性关系考察,精密度实验,稳定性实验,专属性实验,重复性实验,以及加样回收率实验。结果薄层色谱专属性强;小檗碱的线性范围是0.07~0.28μg,r=0.999 5,平均加样回收率为98.11%,RSD为1.34%(n=6)。结论该方法简便、准确,重现性好,可作为五妙水仙膏质量控制的标准。
Objective To establish the quality standard of Wu Miao Shui Xian Ointment. Methods TLC was used to qualitatively identify the herbs of Phellodendron, Galla chinensis and Lithospermum erythrorhis and the content of berberine in the preparation was determined by HPLC. The chromatographic column AichromBond-AQ-C18 (4.6 mm×150 mm) was used. 5 μm); The mobile phase is acetonitrile-0.033 mol/L potassium dihydrogen phosphate (pH adjusted to 3.0 with phosphoric acid)-0.025 mol/L sodium dodecyl sulfate (48:30:25), flow rate 1.0 ml/min, Column temperature 30°C; detection wavelength 345 nm; sample volume 20 μl. The established method for the determination of berberine was validated by high-performance liquid-phase method, which proved that the determination method was suitable for the corresponding analysis requirements. The verification content includes: linear relationship investigation, precision experiment, stability experiment, specificity experiment, repeatability experiment, and sample recovery experiment. Results The specificity of TLC was strong. The linear range of berberine was 0.07-0.28 μg, r=0.999 5, the average recovery was 98.11%, and the RSD was 1.34% (n=6). Conclusion The method is simple, accurate, and reproducible. It can be used as a standard for quality control of Wu Miao Daffodil Cream.