水调散质量标准研究

Study on the Quality Standard for Shuitiao Powder

目的:进行水调散质量标准研究。方法:采用薄层色谱法,对制剂中的黄柏进行专属性鉴别;采用高效液相色谱法对处方黄柏中有效成分盐酸小檗碱进行含量测定。色谱柱为Diamonsil C_(18)(200 mm×4.6 mm,5μm);流动相为乙腈-0.1%磷酸溶液(50∶50)(每100 ml加十二烷基磺酸钠0.1 g),流速为1.0 ml·min^(-1),检测波长为265 nm,柱温为室温,进样量为10μl。结果:黄柏的TLC图谱特征斑点清晰,分离度好,阴性对照无干扰。盐酸小檗碱在4.26~272.44μg·ml^(-1)的浓度范围内呈良好线性关系(r=0.999 9),平均加样回收率为100.32%,RSD=0.56%(n=6)。结论:所建立的质量标准准确、重复性良好,可用于水调散质量控制。

Objective： To establish the quality standard for Shuitiao powder. Methods： Phellodendri Chinese Cortex was identified by TLC. The content of berberine hydrochloride was determined by HPLC. An HPLC method for berberine hydrochloride was adopted on a Diamonsil C1s（200 mm ×4.6 mm, 5 μm） column with acetonitrile-0.1% H3PO4（50： 50） as the mobile phase （0.1 g sodium dodecyl sulphate was added into the 100 ml mobile phase）, the flow rate was 1.0 ml ·min-1, the detection wavelength was 265 nm, the column temperature was ambient and the injection volume was 10 μl. Results： The TLC spots were clear with good resolution and without interference from negative samples. There was good linearity within the range of 4.26-272.44 μg · ml-l. The average recovery of berberine hydrochloride was 100.32% and RSD was 0.56% （n = 6）. Conclusion： The method is simple, accurate and reproducible. It can be used as the quality control method for Shuitiao powder.