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作 者:高必兴 齐景梁 马璐琳 苟琰 李倩 连艳[3] 蒋桂华[3] 蒋运斌 GAO Bixing;QI Jingliang;MA Lulin;COU Yan;LI Qian;LIAN Yan;JIANG Guihua;JIANG Yunbin(Sichuan Institute for Drug Control/Key Laboratory of Quality Evaluation of Chinese Patent Medicines,NMPA,Chengdu 611731 Sichuan,China;Chengdu Pidu District Hospital of TCM,Chengdu 611730 Sichuan,China;School of Pharmacy,Chengdu University of Traditional Chinese Medicine,Chengdu 610072 Sichuan,China;College of Pharmaceutical Sciences and Chinese Medicine,Southwest University,Chongqing 400715,China)
机构地区:[1]四川省药品检验研究院/国家药品监督管理局中成药质量评价重点实验室,四川成都611731 [2]成都市郫都区中医医院,四川成都611730 [3]成都中医药大学药学院,四川成都610072 [4]西南大学药学院中医药学院,重庆400715
出 处:《中药新药与临床药理》2023年第11期1600-1607,共8页Traditional Chinese Drug Research and Clinical Pharmacology
基 金:国家食药监总局药化司专项“特色民族药材检验方法示范性研究”(2021-KYRW-001);四川省药品监督管理局科技计划项目(2021002)。
摘 要:目的建立测定洪连类药材环烯醚萜苷类成分(梓醇、桃叶珊瑚苷、栀子新苷、京尼平苷酸、玉叶金花苷酸、8-表马钱子苷酸、乔木状车前苷酸)的HPLC-DAD含量测定方法,比较不同基原洪连的含量差异,为其质量控制研究提供依据。方法采用Waters Atlantis T3 C_(18)(4.6 mm×250 mm,5μm)色谱柱;流动相为乙腈-0.1%磷酸溶液,梯度洗脱;流速:1.0 mL·min^(-1);检测波长:205 nm(0~42 min)、236 nm(42~80 min);柱温:30℃;进样量:10μL。根据测定结果,使用含量范围、平均值、总量及正交偏最小二乘法判别分析(OPLS-DA)进行比较研究。结果7种基原77批次洪连样品各环烯醚萜苷类成分色谱峰分离度及线性关系均良好。通过比较含量范围、平均值及总量的结果可知,不同基原所含的单体成分既有共性也有差异,而总含量无明显差异;云南兔耳草所含各单体成分均最高。OPLS-DA结果显示,云南兔耳草为一类,短穗兔耳草与全缘兔耳草聚为一类,圆穗兔耳草、短筒兔耳草与紫叶兔耳草聚为一类。结论建立的环烯醚萜苷类分析方法可针对不同基原洪连进行定量分析,为洪连的质量控制及资源开发提供了依据。Objective A HPLC-DAD method was established to determinate iridoid glycosides(catalpol,aucubin,gardoside,geniposidic acid,mussaenosidic acid,8-epiloganic acid,arborescosidic acid)in Lagotidis Herba.To compare the difference of iridoid glycosides of Lagotidis Herba from different origins,and to provide basis for its quality control.Methods The HPLC analysis was performed on Waters Atlantis T3 C_(18)(4.6 mm×250 mm,5μm)using acetonitrile and 0.1%phosphoric acid solution as the mobile phase at a flow rate of 1.0 mL·min^(-1).The detection wavelength was 205 nm(0-42 minutes)and 236 nm(42-80 minutes),the column temperature was30℃and the injection volume was 10μL.According to the results of the determination,a comparative study was conducted by using content range,average value,total amount and partial least squares discriminant analysis(OPLS-DA).Results The chromatographic peak resolution and linear relationship of iridoid glycosides in 77 batches of samples from 7 different producing areas were both good.By comparing the results of content range,average value and total amount,it can be concluded that there were commonalities and differences of iridoid ingredients in different producing areas.But there was no significant difference in total amount.The iridoid glycosides contents in Lagotis yunnanensis W.W.Smith.were the highest.OPLS-DA results showed that Lagotis yunnanensis W.W.Smith belongs to one category,Lagotis brachystachya Maxim.and Lagotis.integra W.W.Smith belong to another category,Lagotis ramalana Batalin,Lagotis brevituba Maxim and Lagotis praecox W.W.Smith belong to the third category.Conclusion The established quantitative analysis method of iridoid glycosides could effectively analyze a variety of Lagotidis Herba.It provided an effective basis for the quality control and utilization of its resources.
关 键 词:洪连 环烯醚萜苷类 高效液相色谱法 含量测定 正交偏最小二乘法判别分析
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