蝉翼藤中4个酮类成分的分离及HPLC法同时测定其含量  

Isolation of four xanthones from S.inappendiculata Hassk. and simultaneous determination of their content by HPLC

作　　者：王起文[1] 陈东东[1] 马赟[1] 李祥[1] 陈建伟[1] WANG Qi-wen CHEN Dong-dong MA Yun LI Xiang CHEN Jian-wei(Nanjing University of Chinese Medicine, Nanjing 210023, China)

机构地区：[1]南京中医药大学药学院,南京210023

出　　处：《药物分析杂志》2016年第12期2168-2173,共6页Chinese Journal of Pharmaceutical Analysis

基　　金：江苏高校优势学科建设工程资助项目(DE63063683)

摘　　要：目的:建立蝉翼藤中4个酮类化合物的HPLC定量测定方法。方法:采用Symmetry-C_(18)(4.6 mm×250 mm,5μm)色谱柱,以甲醇(A)-0.1%甲酸水溶液(B)为流动相,梯度洗脱(0~25 min,50%A→55%A;25~35 min,55%A→65%A;35~40 min,65%A),流速1.0 m L·min^(-1),柱温30℃,检测波长265 nm。结果:7-羟基-1,2-二甲氧基(口山)酮、1,7-二羟基-4-甲氧基(口山)酮、2-羟基-1,7-二甲氧基(口山)酮、1,7-二羟基(口山)酮进样量分别在0.048 2~0.241、0.063~0.315、0.052 4~0.262和0.106 6~0.533μg范围内与峰面积呈良好线性关系(r>0.999 0);平均加样回收率分别为100.4%、98.9%、100.2%、101.1%,RSD为别为1.8%、1.7%、1.8%、2.0%。不同来源的3个样品中7-羟基-1,2-二甲氧基(口山)酮、1,7-二羟基-4-甲氧基(口山)酮、2-羟基-1,7-二甲氧基(口山)酮、1,7-二羟基(口山)酮的含量范围分别为47.37~54.73、65.72~99.69、64.05~87.26、163.2~195.6μg·g^(-1)。结论:经方法学验证,本法可用于蝉翼藤中4个酮的含量测定。Objective： To establish an HPLC method for simultaneous determination of four xanthones from S. inappendiculata Hassk.Methods： The analysis of S. inappendiculata Hassk.methanol extract was performed on a Symmetry-C18 （4.6 mm×250 mm, 5 μm）with mobile phase consisting of methanol （phase A）-0.1% formic acid solution （phase B）in a gradient elution manner （0-25 min, 50%A→55%A;25-35 min, 55%A→65%A;35-40 min, 65%A）at the flow rate of 1.0 mL·min-1, the column temperature was maintained at 30℃, and the detection wavelength was set at 265 nm. Results： 7-hydroxy-1, 2-dimethoxyxanthone, 1, 7-dihydroxy-4-methoxyxanthone, 2-hydroxy-1, 7-dimethoxyxanthone and 1, 7-dihydroxyxanthone had good linear relationship （r〉0.999 0）in the ranges of 0.048 2-0.241 μg, 0.063-0.315 μg, 0.052 4-0.262 μg and 0.106 6-0.533 μg, respectively.Their average recoveries respectively were 100.4% （RSD=1.8%）, 98.9% （RSD=1.7%）, 100.2% （RSD=1.8%）, and 101.1% （RSD=2.0%）.Their content ranges in 3 samples from different sources were 47.37-54.73, 65.72~99.69, 64.05~87.26 and 163.2-195.6 μg·g-1, respectively. Conclusion： The developed method is proved by methodology validation that it is suitable for the quantitative analysis of four xanthones in S. inappendiculata Hassk.

关 键 词：蝉翼藤 咄酮类化合物 7-羟基-1  2二甲氧基岫酮 1 7-二羟基-4-甲氧基咄酮 2-羟基-1  7-二甲氧基口山酮 1  7-二羟基咄酮 高效液相色谱 

分 类 号：R917[医药卫生—药物分析学]