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.
作者
王起文
陈东东
马赟
李祥
陈建伟
WANG Qi-wen CHEN Dong-dong MA Yun LI Xiang CHEN Jian-wei(Nanjing University of Chinese Medicine, Nanjing 210023, China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
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)
