超高效液相色谱法同时测定固本消疹方中10个成分的含量  

Simultaneous determination of ten components in Guben Kangmin decoction by UPLC

作　　者：刘丽娟 赵亚 吴亚运 赵瑞芝 卢传坚 LIU Li-juan;ZHAO Ya;WU Ya-yun;ZHAO Rui-zhi;LU Chuan-jian(The Second Clinical Medical College of Guangzhou University of Chinese Medicine(Guangdong Academy of Traditional Chinese Medicine,Guangdong Provincial Hospital of Chinese Medicine),Guangzhou 510006,China;Guangdong Provincial Key Laboratory of Clinical Research on Traditional Chinese Medicine Syndrome,Guangzhou 510120,China)

机构地区：[1]广州中医药大学第二临床医学院,广东省中医院,广东省中医药科学院,广州510006 [2]广东省中医证候临床研究重点实验室,广州510120

出　　处：《药物分析杂志》2023年第3期516-524,共9页Chinese Journal of Pharmaceutical Analysis

基　　金：国家中医药管理局“岐黄工程”项目[国中医药办人教函(2019)62号];广东省科技计划项目(No.2017B030314166);广东省中医药局科研项目(No.20203005)。

摘　　要：目的:建立超高效液相色谱(UPLC)法同时测定固本消疹方中5-羟甲基糠醛、升麻素苷、毛蕊异黄酮苷、升麻素、5-O-甲基维斯阿米醇苷、毛蕊异黄酮、亥茅酚苷、6-姜酚、五味子醇甲和梣酮10个成分的含量,明确配伍对10个成分含量变化的影响。方法:应用UPLC梯度洗脱技术,采用ACQUITY UPLC BEH C_(18)色谱柱(2.1 mm×100 mm, 1.7μm),以乙腈-0.1%甲酸水溶液为流动相,流速为0.25 mL·min^(-1),检测波长为254 nm,柱温为30℃。结果:5-羟甲基糠醛、升麻素苷、毛蕊异黄酮苷、升麻素、5-O-甲基维斯阿米醇苷、亥茅酚苷、毛蕊异黄酮、6-姜酚、五味子醇甲和梣酮质量浓度分别在156.00~10 000、12.50~1 600、3.12~400、12.50~1 600、6.25~800、0.78~100、3.90~500、20.50~1 600、0.58~75、12.50~200 ng范围内与峰面积呈良好的线性关系(r=0.999 5~1.000),平均加样回收率在98.3%~102.3%(RSD<3%,n=6)。固本消疹方中6-姜酚、毛蕊异黄酮苷、5-羟甲基糠醛、五味子醇甲、梣酮含量显著增加(P<0.05或P<0.01);而毛蕊异黄酮、升麻素苷、升麻素、5-O-甲基维斯阿米醇苷和亥茅酚苷含量无明显变化。结论:该方法可用于固本消疹方及其制剂的质量控制,为其新药开发奠定基础,为其临床应用提供科学依据。Objective:To establish an UPLC method for simultaneous determination of 5-hydroxymethyl furfural-dehyde(5-HMF),cimicifugoside,calycosin-7-glucoside,cimicifugin,4’-O-beta-glucopyranosyl-5-O-methylvisamminol,calycosin,sec-O-glucosylhamaudol,6-gingerol,schisandrin and fraxinellone in Guben Kangmin decoction,so as to analyze the variation of the 10 ingredients after compatibility.Methods:The samples were separated on an ACQUITY UPLC BEH C_(18) column(2.1 mm×100 mm,1.7μm)by gradient elution with acetonitrile-0.1%formic acid aqueous solution at a flow rate of 0.25 m L·min^(-1).The detection wavelength was 254 nm.The column temperature was controlled at 30℃.Results:5-HMF,cimicifugoside,calycosin-7-glucoside,cimicifugin,4’-O-beta-glucopyranosyl-5-O-methyl-visamminol,calycosin,sec-O-glucosylhamaudol,6-gingerol,schisandrin and fraxinellone exhibited good linearity(r2=0.9995-1.000)among the ranges of 156.00-10000,12.50-1600,3.12-400,12.50-1600,6.25-800,0.78-100,3.90-500,20.50-1600,0.58-75 and 12.50-200 ng,respectively.The average recoveries(RSD<3%,n=6)were between 98.3%-102.3%.After the compatibility,the contents of 6-gingerol,caly-cosin-7-glucoside,5-HMF,schisandrin and fraxinellone increased significantly(P<0.05 or P<0.01),while there was no significant change in the contents of cimicifugoside,cimicifugin,4’-O-beta-glucopyrano-syl-5-O-methyl-visamminol,calycosin and sec-O-glucosylhamaudol.Conclusion:The method can be used for the quality control of Guben Kangmin decoction and its preparations,and can provide scientific basis for the clinical compatibility and application of Guben Kangmin decoction.

关 键 词：固本消疹方 6-姜酚 毛蕊异黄酮苷 5-羟甲基糠醛 干姜 黄芪 白鲜皮 含量测定 质量评价 配伍 

分 类 号：R917[医药卫生—药物分析学]