摘要
目的建立补气通窍合剂的质量标准。方法采用薄层色谱(TLC)法对制剂中甘草、辛夷、荆芥进行定性鉴别;采用高效液相色谱(HPLC)法同时测定制剂中10种成分的含量,色谱柱为Agilent Zorbax SB-C18柱(250 mm×4.6 mm,5µm),流动相为乙腈-0.1%磷酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长分别为326 nm(绿原酸、咖啡酸)、260 nm(毛蕊异黄酮葡萄糖苷、甘草苷、橙皮苷、迷迭香酸、芒柄花苷、甘草酸铵、芒柄花素)、278 nm(木兰脂素),柱温为27℃,进样量为10µL。结果甘草、辛夷、荆芥的TLC斑点显色清晰,且阴性对照无干扰。绿原酸、咖啡酸、毛蕊异黄酮葡萄糖苷、甘草苷、橙皮苷、迷迭香酸、芒柄花苷、甘草酸铵、芒柄花素、木兰脂素的质量浓度分别在13.10~131.00µg/mL、7.10~71.00µg/mL、9.50~95.00µg/mL、90.80~908.00µg/mL、28.60~286.00µg/mL、37.70~377.00µg/mL、6.52~65.20µg/mL、112.80~1128.00µg/mL、1.28~12.80µg/mL、19.20~192.00µg/mL范围内与其峰面积线性关系良好(r≥0.9995,n=7);精密度、稳定性、重复性试验结果的RSD均小于3%(n=6);平均加样回收率分别为98.77%,97.89%,98.27%,99.10%,98.07%,98.00%,97.86%,97.32%,99.30%,97.96%,RSD分别为3.51%,2.87%,3.37%,3.04%,2.39%,2.88%,2.80%,2.70%,3.89%,2.69%(n=6)。10批样品中上述10种成分的含量分别为0.0887~0.1130 mg/mL,0.0385~0.0496 mg/mL,0.0356~0.0469 mg/mL,0.3876~0.5082 mg/mL,0.1417~0.1899 mg/mL,0.1316~0.1653 mg/mL,0.0344~0.0473 mg/mL,0.4322~0.5834 mg/mL,0.0030~0.0039 mg/mL,0.0702~0.0963 mg/mL。结论该方法操作简便、专属性强、灵敏度高、结果准确,可用于补气通窍合剂的质量控制。
Objective To establish the quality standard of Buqi Tongqiao Mixture.Methods Thin-layer chromatography(TLC)method was used for qualitative identification of Glycyrrhizae Radix et Rhizoma,Magnoliae Flos,and Schizonepetae Herba in the preparation.High-performance liquid chromatography(HPLC)method was used for simultaneous determination of 10 components in the preparation,the chromatographic column was Agilent Zorbax SB-C_(18) column(250 mm×4.6 mm,5μm),and the mobile phase was acetonitrile-0.1%phosphoric acid solution(gradient elution),the flow rate was 1.0 mL/min,the detection wavelength was set at 326 nm for chlorogenic acid and caffeic acid,260 nm for calycosin-7-glucoside,glycyrrhizin,hesperidin,rosinic acid,ononin,ammonium glycyrrhizinate,and formononetin,and 278 nm for magnolin,the column temperature was 27℃,and the injection volume was 10μL.Results The TLC spots of Glycyrrhizae Radix et Rhizoma,Magnoliae Flos,and Schizonepetae Herba were clear,and the negative control had no interference.The linear ranges of chlorogenic acid,caffeic acid,calycosin-7-glucoside,glycyrrhizin,hesperidin,rosinic acid,ononin,ammonium glycyrrhizinate,formononetin,and magnolin were 13.10-131.00μg/mL,7.10-71.00μg/mL,9.50-95.00μg/mL,90.80-908.00μg/mL,28.60-286.00μg/mL,37.70-377.00μg/mL,6.52-65.20μg/mL,112.80-1128.00μg/mL,1.28-12.80μg/mL,19.20-192.00μg/mL(r≥0.9995,n=7),respectively.The RSDs of precision,stability,and repeatability test results were all lower than 3%(n=6).The average recoveries of the above 10 components were 98.77%,97.89%,98.27%,99.10%,98.07%,98.00%,97.86%,97.32%,99.30%,and 97.96%,with RSDs of 3.51%,2.87%,3.37%,3.04%,2.39%,2.88%,2.80%,2.70%,3.89%,and 2.69%(n=6),respectively.The contents of the above 10 components in the 10 batches of samples were 0.0887-0.1130 mg/mL,0.0385-0.0496 mg/mL,0.0356-0.0469 mg/mL,0.3876-0.5082 mg/mL,0.1417-0.1899 mg/mL,0.1316-0.1653 mg/mL,0.0344-0.0473 mg/mL,0.4322-0.5834 mg/mL,0.0030-0.0039 mg/mL,and 0.0702-0.0963 mg/mL,respectively.Conclusion This method is simple,highly specific,sensitive,and accurate,which can be used for the quality control of Buqi Tongqiao Mixture.
作者
吕建伟
赵凤仙
梁晓莲
李德仁
陈勇
桂雄斌
LYU Jianwei;ZHAO Fengxian;LIANG Xiaolian;LI Deren;CHEN Yong;GUI Xiongbin(The First Affiliated Hospital of Guangxi University of Chinese Medicine,Nanning,Guangxi 530023,China;Jingxi People's Hospital,Baise,Guangxi 533800,China;School of Pharmacy,Guangxi University of Chinese Medicine,Nanning,Guangxi 530200,China;Wuzhou Traditional Chinese Medicine Hospital,Wuzhou,Guangxi 543099,China)
出处
《中国药业》
2026年第5期109-114,共6页
China Pharmaceuticals
基金
国家自然科学基金[82460955]。
