复方钩藤口服液的质量标准研究  

Study on quality standard of Compound Uncaria hirsute Havil(Gouteng)Oral Liquid

作　　者：周卿 陆莹华 燕飞 Zhou Qing;Lu Yinghua;Yan Fei(Teaching and Research Section of Pharmaceutical Analysis,School of Pharmacy,Zunyi Medical University,Zunyi Guizhou 563099,China;Class of 2014,School of Pharmacy,Zunyi Medical University,Zunyi Guizhou 563099,China)

机构地区：[1]遵义医科大学药学院药物分析教研室,贵州遵义563099 [2]遵义医科大学药学院,贵州遵义563099

出　　处：《遵义医科大学学报》2020年第3期373-379,共7页Journal of Zunyi Medical University

基　　金：贵州省剑河中药材产业科技合作计划项目(NO:剑科合字201401);遵义医科大学大学生创新创业训练计划项目(NO:201610661034)。

摘　　要：目的建立复方钩藤口服液的质量标准。方法采用薄层色谱法(TLC)对复方钩藤口服液中的钩藤、天麻、酸枣仁进行定性鉴别;采用高效液相色谱法(HPLC)对复方钩藤口服液中的钩藤碱进行含量测定,色谱柱Agilent Eclipse Plus-C18;流动相为乙腈-0.05%冰醋酸缓冲液(加三乙胺调节pH为7.5),梯度洗脱;流速1.0 mL/min;检测波长243 nm;柱温为25℃;进样量20μL。采用高效液相色谱法(HPLC)对复方钩藤口服液中的天麻素进行含量测定,色谱柱Agilent ZORBAX SB-Aq;流动相为乙腈-水(3∶97,V/V);流速1.0 mL/min;检测波长220 nm;柱温为30℃,进样量20μL。结果口服液中3种指标成分的对照品与样品在相同位置显相同颜色斑点,阴性对照无干扰。钩藤碱和天麻素分别在0.92~18.40μg/mL(r=0.9992)、13.25~265.00μg/mL(r=0.9998)范围内线性关系良好;精密度、稳定性、重复性实验的RSD均小于≤3.0%;定量限分别为0.92、1.33μg/mL,检测限分别为0.18、0.26μg/mL;平均加样回收率分别为98.91%、99.50%(RSD=0.50%,1.02%)。结论本研究建立的复方钩藤口服液的质量标准准确可靠,可用于复方钩藤口服液的质量控制。Objective To establish the quality standard for Compound Uncaria hirsute Havil.oral liquid(CUHOL).Methods Thin layer chromatography(TLC)was used for qualitative identification of Uncaria hirsute Havil.,Gastrodia elata Bl.and Semen Ziziphi Spinosae in CUHOL.High performance liquid chromatography(HPLC)was adopted to determine the rhynchophylline in CUHOL.The determination was performed on Agilent Eclipse Plus-C18 column with mobile phase consisted of acetonitrile-0.05%glacial acetic acid buffer(added triethylamine to pH 7.5)(gradient elution)at a flow rate of 1.0 ml/min.The detection wavelength was 243 nm and the column temperature was 25℃.The sample size was 20μl.Meanwhile,the content of gastrodin in CUHOL was also determined by HPLC.The determination was performed on Agilent ZORBAX SB-Aq column with mobile phase consisted of acetonitrile-water(3∶97,V/V)at the flow rate of 1.0 ml/min.The detection wavelength was 220 nm and the column temperature was 30℃.The sample size was 20μl.Results TLC chromatograms of 3 medicinal materials showed the same color spot at the corresponding position with the reference substance and the samples,and the negative control had no interference.The linear range of rhynchophylline and gastrodin were 0.92~18.40μg/ml(r=0.9992)and 13.25~265.00μg/mL(r=0.9998),respectively.RSDs of precision,stability,and reproducibility tests were all less than 3.0%.The limits of quantitation were 0.92 and 1.33μg/mL,and then the limits of detection were 0.18 and 0.26μg/mL.Average recoveries were 98.91%and 99.50%(RSD=0.50%,1.02%).Conclusion Established quality standard of CUHOL was accurate and reliable,and can be used for quality control of the Compound Uncaria hirsute Havil.oral liquid.

关 键 词：复方钩藤口服液 质量标准 薄层色谱法 高效液相色谱法 钩藤碱 天麻素 

分 类 号：R917[医药卫生—药物分析学]