摘要
目的建立一测多评法同时对行气导滞方中6种成分的高效液相色谱测定方法。方法采用色谱柱Diamonsil C18(250mm×4.6mm,5μm);流动相:乙腈(A)-0.1%磷酸水溶液(B),梯度洗脱0~10min,20%→30%A;10~15min,30%→45%A;15~40min,45%→100%A。检测波长为0~13min,345nm;13~16min,283nm;16~25min,检测波长254nm,流速为1.0 mL/min,柱温:25℃,对行气导滞方中6种成分进行测试,并对其进行方法学及耐用性考察。以芍药苷为基准物,采用多点校正法计算相对校正因子(f_(k/s)),通过一测多评法计算各成分的量,并与外标法实测值的差异进行比较,以验证一测多评法的准确性和可行性。结果建立了行气导滞方中6种成分一测多评的测定方法;一测多评法与外标法实测值之间没有显著性差异。结论建立的行气导滞方中大黄素、大黄酚、厚朴酚、和厚朴酚、橙皮苷、盐酸小檗碱6种成分的同时测定方法简便,结果准确,可为行气导滞方相关新制剂的质量控制方法提供切实可行的检测方法。
Objective To establish a high-performance liquid chromatography(HPLC)method for the simultaneous determination of six components in Xingqi Daozhi Decoction(行气导滞方,XQDZD),including emodin,chrysophanol,magnolol,honokiol,hesperidin,and berberine hydrochloride,using quantitative analysis of multicomponents by single marker(QAMS).Methods The analysis was performed on a Diamonsil C18 column(250 mm×4.6 mm,5μm)using a mobile phase of acetonitrile(A)and 0.1%phosphoric acid(B)with the following gradient program:0-10 min,20%A to 30%A;10-15 min,30%A to 45%A;15-40 min,45%A to 100%A.The detection wavelengths were set at 345 nm(0-13 min),283 nm(13-16 min),and 254 nm(16-25 min).The flow rate was 1.0 mL/min,and the column temperature was maintained at 25℃.The six components in XQDZD were analyzed,and methodological validation including durability testing was carried out.With paeoniflorin as the internal reference substance,the relative correction factor(f_(k/s))was calculated using multi-point calibration.The contents of the components were calculated by the QAMS method and compared with those obtained by the external standard method(ESM)to verify the accuracy and feasibility of the QAMS approach.Results A method for the simultaneous determination of the six components in XQDZD based on QAMS was successfully established.The results obtained by QAMS showed no significant differences compared with those obtained by ESM.Conclusion The established method for the simultaneous determination of emodin,chrysophanol,?magnolol,honokiol,hesperidin,and berberine hydrochloride in XQDZD is simple and accurate,providing a feasible approach for the quality control of XQDZD-related preparations.
作者
仝立国
高炎
郝淑兰
郑晨
吉海杰
宋美卿
武云帆
冯玛莉
TONG Liguo;GAO Yan;HAO Shulan;ZHENG Chen;JI Haijie;SONG Meiqing;WU Yunfan;FENG Mali(Shanxi Academy of Traditional Chinese Medicine,Taiyuan 030012,China)
出处
《时珍国医国药》
北大核心
2025年第15期2876-2881,共6页
JOURNAL OF LI-SHIZHEN TRADITIONAL CHINESE MEDICINE
基金
国家中医药管理局高水平重点学科(中药化学)建设项目(2023)
山西省科技创新人才团队专项资助(202204051001032)
山西省中医药研究院中西医结合基础科技创新团队项目(2022)
山西省中医药重点研究室建设项目(ZYYYJS2024005)
山西省中医药管理局科研课题计划项目(2022ZYY002,2024ZYYAD005)。
关键词
行气导滞方
一测多评
大黄素
大黄酚
厚朴酚
和厚朴酚
橙皮苷
盐酸小檗碱
Xingqi Daozhi Decoction(行气导滞方)
Quantitative analysis of multicomponents by single-marker
Emodin
Chrysophanol
Magnolol
Honokiol
Hesperidin
Berberine hydrochloride
