摘要
目的:建立高效液相色谱-蒸发光散射检测器(HPLC-ELSD)方法测定羊踯躅药材中闹羊花毒素Ⅲ和Ⅵ(Rj-Ⅲ、Rj-Ⅵ)的含量,并对不同产地、批次的羊踯躅药材的不同药用部位进行质量研究。方法:热回流提取法制备供试品溶液。采用HPLC-ELSD法检测羊踯躅果实、花、根部位的Rj-Ⅲ和Rj-Ⅵ含量,并进行方法学考察。选用Agilent ZORBAX SB-C_(18)(4.6 mm×250 mm,5μm)色谱柱,以甲醇-0.1%甲酸水溶液为流动相进行梯度洗脱,流速0.8 ml/min,柱温30℃,ELSD漂移管温度75℃,进样量30μl。比较不同产地、批次的羊踯躅药材的不同药用部位中Rj-Ⅲ和Rj-Ⅵ含量差异。结果:Rj-Ⅲ在2.60~13.00μg、Rj-Ⅵ在3.39~28.25μg范围内,线性关系良好。重复性实验Rj-Ⅲ和Rj-Ⅵ的RSD分别为2.47%、1.59%;日内/日间精密度实验RSD均<2%;稳定性实验RSD均<2.70%;两者的平均加样回收率分别为99.06%、101.39%,RSD分别为4.46%、2.91%,均符合相关规定。含量测定结果表明,不同产地、批次的羊踯躅药材花部位的Rj-Ⅲ含量差异相对较大,果实部位Rj-Ⅲ和Rj-Ⅵ含量明显高于花及根。结论:该方法适用于羊踯躅药材不同药用部位Rj-Ⅲ和Rj-Ⅵ的含量检测。不同产地、批次的羊踯躅药材的不同药用部位中Rj-Ⅲ和Rj-Ⅵ含量存在差异。
Objective:To establish a high performance liquid chromatography-evaporative light scattering detector(HPLC-ELSD)method for the content determination of Rhodojaponin-Ⅲand Rhodojaponin-Ⅵ(Rj-Ⅲand Rj-Ⅵ)in Rhododendron mole G.Don,and compare the quality of different officinal parts of Rhododendron mole G.Don from different producing areas and batches.Methods:The test solution was prepared by hot reflux extraction.The contents of Rj-Ⅲand Rj-Ⅵin fruit,flower and root of Rhododendron mole G.Don were determined by HPLC-ELSD,and the methodological investigation was carried out.The determination was performed on an Agilent ZORBAX SB-C18 column(4.6 mm×250 mm,5μm)at flow rate of 0.8 ml/min with methanol-0.1%formic acid containing water(gradient elution).The column temperature was set at 30℃,the drift tube temperature of ELSD was 75℃,and the injection volume was 30μl.The differences of Rj-Ⅲand Rj-Ⅵcontents in different officinal parts of Rhododendron mole G.Don from different producing areas and batches were compared.Results:The linear ranges were 2.60-13.00μg for Rj-Ⅲand 3.39-28.25μg for Rj-Ⅵ.In replication test,the relative standard deviations(RSDs)of Rj-Ⅲand Rj-Ⅵwere 2.47%and 1.59%respectively;in intra-day/inter-day precision test,the RSDs were less than 2%;in stability test,the RSDs were less than 2.70%;the average recoveries of Rj-Ⅲand Rj-Ⅵwere 99.06%and 101.39%,and the RSDs were 4.46%and 2.91%,respectively.All data were conformed to the standard of determination.The content determination results showed that,there were significant differences on Rj-Ⅲcontent in flowers of Rhododendron mole G.Don from different producing areas and batches,and the contents of Rj-Ⅲand Rj-Ⅵin fruits of Rhododendron mole G.Don were obviously higher than those in flowers and roots.Conclusion:The established HPLC-ELSD method can be used for content determination of Rj-Ⅲand Rj-Ⅵin different officinal parts of Rhododendron mole G.Don.There are differences on the contents of Rj-Ⅲand Rj-Ⅵin different officinal parts of Rhododendron mole G.Don from different producing areas and batches.
作者
陈琪琪
房鑫
薛秋雯
何燕辰
梁爽
CHEN Qiqi;FANG Xin;XUE Qiuwen;HE Yanchen;LIANG Shuang(Engineering Research Center of Modern Preparation Technology of TCM,Ministry of Education,Innovation Research Institute of Traditional Chinese Medicine,Shanghai University of Traditional Chinese Medicine,Shanghai 201203,China)
出处
《上海中医药大学学报》
CAS
2020年第6期75-80,共6页
Academic Journal of Shanghai University of Traditional Chinese Medicine
基金
上海市科委科研计划项目(14401901400)。
