远志中远志[口山]酮Ⅺ、远志[口山]酮Ⅲ和3,6’-二芥子酰基蔗糖含量的同时测定  

Simultaneous quantification of polygalaxanthone Ⅺ,polygalaxanthone Ⅲ and 3,6’-disinapoylsucrose in Polygalae Radix

作　　者：赵鑫 李娜 陈玥 谢元彪 谷丽华[1,2] 杨莉 詹常森[4] 王峥涛 ZHAO Xin;LI Na;CHEN Yue;XIE Yuan-biao;GU Li-hua;YANG Li;ZHAN Chang-sen;WANG Zheng-tao(MOE Key Laboratory of Standardization of Chinese Medicines,Institute of Chinese Materia Medica,Shanghai University of Traditional Chinese Medicine,Shanghai 201203,China;Shanghai R&D Centre for Standardization of Chinese Medicines,Shanghai 201203,China;Institute of Interdisciplinary Integrative Medicine Research,Shanghai University of Traditional Chinese Medicine,Shanghai21203,China;Shanghai Hutchison Pharmaceuticals Co.,Ltd.,Shanghai 201401,China)

机构地区：[1]上海中医药大学中药研究所中药标准化教育部重点实验室、国家中医药管理局中药新资源与质量评价重点实验室,上海201203 [2]上海中药标准化研究中心,上海201203 [3]上海中医药大学交叉科学研究院,上海201203 [4]上海和黄药业有限公司,上海201401

出　　处：《药物分析杂志》2023年第10期1709-1717,共9页Chinese Journal of Pharmaceutical Analysis

基　　金：上海市自然基金项目(19ZR1457200)。

摘　　要：目的:建立HPLC法同时测定远志中远志[口山]酮Ⅺ、远志[口山]酮Ⅲ和3,6’-二芥子酰基蔗糖的含量,其中远志[口山]酮Ⅺ是从远志[口山]酮Ⅲ色谱峰中新发现的位置异构体,为远志质量标准的修订提供参考。方法:采用Agilent InfinityLab Poroshell 120 EC-C_(18)(150 mm×4.6 mm,2.7μm)色谱柱,以乙腈(A)-0.1%磷酸水(B)为流动相,梯度洗脱(0~18 min,10%A→13%A;18~35 min,13%A→19%A;35~45 min,19%A→20%A),流速1.0 mL·min^(-1),柱温30℃,检测波长320 nm,进样量10μL。结果:建立的方法经过系统方法学验证,精密度、重复性、稳定性试验结果的RSD均<1%,远志[口山]酮Ⅺ、远志[口山]酮Ⅲ和3,6’-二芥子酰基蔗糖平均加样回收率分别为90.6%、94.4%和94.0%,RSD依次为1.8%、2.7%和3.6%,结果均在规定范围内;在不同色谱柱、仪器、柱温、流速和流动相pH条件下含量测定结果的RSD均<5%,表明该方法耐受性良好。采用该方法对21批远志样品中远志[口山]酮Ⅺ、远志[口山]酮Ⅲ和3,6’-二芥子酰基蔗糖含量进行测定,含量范围分别为0.04%~0.11%、0.06%~0.17%和0.39%~0.82%,根据数据建议远志[口山]酮Ⅲ与远志[口山]酮Ⅺ含量之和不得低于0.12%。结论:该方法对3,6’-二芥子酰基蔗糖、异构体远志[口山]酮Ⅲ与远志[口山]酮Ⅺ的色谱分离度均良好,方法重复性良好,定量准确,为远志质量标准的修订提供参考。Objective:To establish an HPLC method for simultaneous determination of polygalaxanthone Ⅺ,polygalaxanthone Ⅲ and 3,6'-disinapoylsucrose in Polygalae Radix,providing reference for the revision of quality standard of Polygalae Radix.Wherein,polygalanone Ⅺ is a newly discovered positional isomer from the peak of polygalanone Ⅲ.Methods:Chromatographic separation was achieved using a commercial Agilent InfinityLab Poroshell 120 EC-C_(18)column(150 mm×4.6 mm,2.7μm).Acetonitrile(A)and 0.1%phosphoric acid water(B)were used as the mobile phase with gradient elution(0-18 min,10%A→13%A;18-35 min,13%A→19%A;35-45 min,19%A→20%A),the flow rate was 1.0 mL·min~(-1),the column temperature was set at 30℃,the detection wavelength was 320 nm,and the injection volume was 10μL.Results:The established method was verified by systematic methodology.The RSD values of precision,repeatability and stability experimental results were all below 1%,and the average recoveries for polygalaxanthone Ⅺ,polygalaxanthone Ⅲ and 3,6'-disinapoylsucrose were 90.6%,94.4%,and 94.0%,respectively,with RSDs of 1.8%,2.7%,and 3.6%,all of which met the requirements of Chinese Pharmacopoeia 2020.The RSD values of the contents from various parameters including different chromatographic columns,instruments,column temperatures,flow rates,and pH value of mobile phase,were all below 5%,indicating good tolerance of this method.As a result,the method was used for determining polygalaxanthone Ⅺ,polygalaxanthone Ⅲ and 3,6'-disinapoylsucrose in 21 bathes of Polygalae Radix samples,their contents were in range of 0.04%-0.11%,0.06%-0.17% and 0.39%-0.82%,respectively.The content limit was finally recommended that the content sum of polygalaxanthoneⅪand polygalaxanthone Ⅲ should not less than 0.12% according to the data.Conclusion:The optimized method supplying good separation for 3,6'-disinapoylsucrose and two positional isomers polygalaxanthone Ⅲ and polygalaxanthoneⅪwas more accurate for evaluation of the quality of Polygalae Radix than th

关 键 词：远志 远志[口山]酮 位置异构体 3 6’-二芥子酰基蔗糖 [口山]酮 寡糖酯 含量测定 色谱条件优化 质量标准修订 

分 类 号：R917[医药卫生—药物分析学]