中药“洗一号”涂膜剂定性、定量质量研究

Study on the qualitative and quantitative analysis on the herbal medicinal film called wash No.1

目的建立中药"洗一号"涂膜剂中主药成分的定性、定量研究方法。方法采用薄层色谱法(TLC)分析制剂中的成分,主要包括黄柏、大黄、黄芪和黄连药材,采用高效液相色谱法(HPLC)测定制剂中大黄素和大黄酸的含量,色谱柱为Diamonsil C18,流动相为甲醇-体积分数0.1%磷酸溶液,流速为1.0 mL·min-1,检测波长为254 nm,柱温为40℃,进样量为20μL。结果大黄、黄连、黄芩和黄柏药材的TLC图点清晰,分离度好,阴性对照无干扰。大黄酸、大黄素检测质量浓度线性范围为0.16μg~0.49μg(r=0.9999)、0.17μg~0.51μg(r=0.9999);定量限为0.096 mg;加样回收率为95.0%~105.0%(RSD为1.2%,n=6);进样精密度、稳定性、重复性试验的RSD均小于2%。结论该研究所建标准可用于中药"洗一号"涂膜剂的质量控制。

Objective The aim of our research is to establish methods including qualitative and quantitative analysis on the herbal medicinal film called wash No.1.Methods TLC was used to identify rheum officinale,Coptis chinensis,Scutellaria baicalensis,golden cypress,qualitatively.The content of rheinic acid and rheum emodin in rheum officinale was determined by HPLC.The determination was performed on Diamonsil(2)C18 column with mobile phase consisted of methanol-0.1%phosphoric acid solution(gradient elution)at the flow rate of 1.0 mL·min-1.The detection wavelength was set at 254 nm,and column temperature was 40℃.The sample size was 20μL.Results TLC spots of rheum officinale,Coptis chinensis,Scutellaria baicalensis,golden cypress,qualitatively were clear and well-separated without interference from negative control.The range of rheinic acid and rheum emodin in rheum officinale were 0.16μg~0.49μg(r=0.9999)and 0.17μg~0.51μg(r=0.9999).The limit of quantitation was 0.096 mg;the recoveries were 95.0%~105.0%(RSD=1.2%,n=6).RSD of inter-precision,stability and reproducibility tests were all lower than 2%.Extensive test well.Conclusion The qualitative and quantitative analysis method we established is suitable for the quality control of herbal wash No.1.