摘要
建立妇科千金胶囊的HPLC特征图谱,并测定其主要成分的含量。采用Kromasil 100-5-C18色谱柱(4. 6 mm×250mm,5μm),流动相为乙腈(A)-0. 1%磷酸水溶液(B),梯度洗脱,流速1. 0 m L·min-1,检测波长254 nm,柱温30℃,进样量10μL;并对染料木苷、药根碱、穿心莲内酯和脱水穿心莲内酯的含量测定方法进行方法学考察。在特征图谱研究中,确定了妇科千金胶囊HPLC特征图谱8个共有峰,通过与混合对照品比较,确定它们分别为染料木苷、药根碱、巴马汀、小檗碱、穿心莲内酯、脱水穿心莲内酯、藁本内酯和Z-3-丁烯基苯酞。利用相似度软件对20批样品特征图谱进行分析,各批样品相似度均在0. 95以上。在建立的色谱条件下,定量分析的4个成分分离度良好,方法精密度和重复性RSD均<1. 5%,供试品溶液在72 h内稳定,各成分具有良好的线性关系和较宽线性范围。20批妇科千金胶囊中,染料木苷、药根碱、穿心莲内酯和脱水穿心莲内酯的质量分数分别在28. 66～56. 04,94. 77～197. 92,1 705. 33～4 148. 93,462. 16～1 225. 96μg/粒。所建立的妇科千金胶囊HPLC图谱检测和定量测定分析方法可靠、准确、灵敏,能有效地评价妇科千金胶囊的质量。
To establish an HPLC characteristic fingerprint method of Fuke Qianjin Capsules,and determine the contents of its main components.The analysis was carried out on a Kromasil 100-5-C18 analytical column(4.6 mm×250 mm,5μm)with gradient elution by acetonitrile(A)-0.1%phosphoric acid aqueous solution(B),a flow rate at 1.0 m L·min-1 and the detection wavelength of 254 nm.The column temperature was 30℃,and the injection volume was 10μL.The determination method of genistin,jatrorrhizine,andrographolide and 14-deoxy-11,12-didehydroandrographolide index components were studied methodologically.The common mode of the characteristic fingerprint of Fuke Qianjin Capsules was set up with 8 common peaks,which were identified as genistin,jatrorrhizine,palmatine,berberine,andrographolide,14-deoxy-11,12-didehydroandrographolide,Z-ligustilide,and Z-3-butylidenephthalide,respectively,in comparison with the references.The similarities of 20 batches of Fuke Qianjin Capsules samples were above 0.95.All of the above-mentioned 4 analytes could be well separated under the optimized chromatographic conditions.RSD of precision and repeatability experiment were both less than 1.5%,and the sample solution was stable during 72 h.All of the compounds had a good linearity and linear range.The contents of genistin,jatrorrhizine,andrographolide,and 14-deoxy-11,12-didehydroandrographolide in 20 batches of Fuke Qianjin Capsules samples were 28.66-56.04,94.77-197.92,1 705.33-4 148.93 and 462.16-1 225.96μg in each capsule,respectively.The developed HPLC characteristic fingerprint and quantitative analysis methods were reliable,accurate and sensitive,and could be used effectively evaluate the quality of Fuke Qianjin Capsules samples.
作者
王康华
张英涛
杨秀伟
徐嵬
张鹏
彭开锋
李伏君
龚云
刘逆夫
WANG Kang-hua;ZHANG Ying-tao;YANG Xiu-wei;XU Wei;ZHANG Peng;PENG Kai-feng;LI Fu-jun;GONG Yun;LIU Ni-fu(State Key Laboratory of Natural and Biomimetic Drugs,Department of Natural Medicines,School of Pharmaceutical Sciences,Peking University,Beijing 100191,China;Zhuzhou Qianjin Pharmaceutical Co.,Ltd.,Zhuzhou 412000,China)
出处
《中国中药杂志》
CAS
CSCD
北大核心
2019年第8期1564-1572,共9页
China Journal of Chinese Materia Medica
基金
国家中药标准化项目(2YB2H-C-HUN-21)
关键词
妇科千金胶囊
HPLC特征图谱
多指标成分定量分析
染料木苷
药根碱
穿心莲内酯
脱水穿心莲内酯
质量
Fuke Qianjin Capsules
HPLC characteristic fingerprint
multi-index quantitative analysis
genistin
jatrorrhizine
andrographolide
14-deoxy-11,12-didehydroandrographolide
quality control
