参黄搽剂的质量标准研究

Study on Quality Standard of Shenhuang Liniment

目的:为参黄搽剂质量标准的建立提供参考。方法:按2015 年版《中国药典》(四部)中薄层色谱法(TLC)对参黄搽剂中的苦参、黄柏、大黄、黄芩进行定性鉴别;采用高效液相色谱法(HPLC)测定参黄搽剂中苦参碱和氧化苦参碱的含量[色谱柱为Phenomenex Luna NH2,流动相为乙腈-无水乙醇-3%磷酸水溶液(80 ∶10 ∶10,V/V/V),柱温为45 ℃,流速为1.0 mL/min,检测波长为220 nm,进样量为5 μL]。结果:TLC结果显示,各供试品色谱与对照药材/对照品色谱相应位置上有相同颜色的对应斑点,且斑点清晰、比移值适中、分离度高,阴性对照无干扰。HPLC结果显示,苦参碱、氧化苦参碱分别在进样量为203.60~1 221.60 ng(r=0.999 4)、210.08~840.30 ng(r=0.999 7)范围内与其峰面积呈现出良好的线性关系;精密度、稳定性、重复性试验的RSD均小于3.0%(n=6);平均加样回收率分别为96.03%、100.93%,RSD分别为2.55%、2.69%(n=9)。结论:所建立方法专属性强、准确度高、重现性好,可用于参黄搽剂的质量控制。

OBJECTIVE:To provide reference for the establishment of quality standard of Shenhuang liniment. METHODS: Qualitative identification of Sophora flavescens,Phellodendron chinense,Rhei Radix Et Rhizoma and Scutellaria baicalensis in Shenhuang liniment were carried out by TLC according to the method of 2015 edition of Chinese Pharmacopeia(part Ⅳ). HPLC method was used to determine the contents of matrine and oxymatrine in Shenhuang liniment [Phenomenex Luna NH2 column, mobile phase consisting of acetonitrile-absolute ethanol-3% phosphoric acid aqueous solution (80 ∶ 10 ∶ 10,V/V/V),column temperature of 45 ℃,flow rate of 1.0 mL/min,detection wavelength of 220 nm,sample size of 5 μL]. RESULTS:Results of TLC showed that the corresponding spots of the same color were found in the corresponding positions of the chromatograms for test samples and reference substance/substance control;and the spots were clear,retardation factor was moderate,the separation degree was high,and the negative control had no interference. Results of HPLC showed that the linear range of matrine and oxymatrine were 203.60-1 221.60 ng(r=0.999 4)and 210.08-840.30 ng(r=0.999 7),respectively. RSDs of precision,stability and reproducibility tests were all lower than 3.0%(n=6). Average recovery rates were 96.03% and 100.93%,and RSDs were 2.55% and 2.69%(n=9). CONCLUSIONS:Established method is specific,accurate and reproducible,and can be used for quality control of Shenhuang liniment.