中医学报2018，Vol.33Issue(2)：286-290,5.DOI:10.16368/j.issn.1674-8999.2018.02.069
超高效液相色谱法检测二仙汤中淫羊藿黄酮类成分的含量
Study on the Ultra-High Performance Liquid Chromatography (UPLC) Method Determination the Content of Flavonoids from Epimedii Folium in Erxian Tang
摘要
Abstract
Objective:To establish a ultra-high performance liquid chromatography (UPLC) method determination the content of flavonoids from Epimedii folium in Erxian Tang.Methods:Chromatographic column:ZORBAX Eclipse Plus-C1s column (3.0 mm × 150 mm,3.5 μm);0.1％ formic acid and 5 mmol · L-1 ammonium acetic acid solution (A phase) and methanol (B phase) were used as mobile phase to perform linear gradient elution;Gradient elution program:0.0-0.5 min with keeping 95％ A phase,0.5-1.5 min with A phase ratio from 95％ to 70％,1.5-3.5 min with A phase ratio from 70％ to 50％,3.5-6 min with A phase ratio from 50％ to 30％,6-12 min with A phase ratio from 30％ to 10％,12-15 min with A phase ratio from 10％ to 5％.The flow rate was 0.45 mL · min-1,the injection volume was 1 μL,column temperature was 40 ℃.Detection wavelength was at 270 nm.The epimedin B,epimedin C,icariin and icariside Ⅱ in the control product mixture,water of Erxian Tang and 50％ ethanol extracting solution.Results:In the determinations of epimedin B,epimedin C,icariin and icariside Ⅱ with the UPLC method,the RSD of interday and intraday precision were respectively 0.21％-0.40％ and 0.54％-0.89％,the RSD of stability and average recovery rate were respectively 0.26％-0.90％ and 104.8％-116.7％.The main flavonoids from Epimedii folium in the same extracting solution of Erxian Tang were obviously different and ranked for epimedin C ＞ icariin ＞ epimedin B ＞ icariside Ⅱ;the main flavonoids from Epimedii folium in the 50％ ethanol extracting solution were significantly higher than those in the water extracting solution,their differences were statistically significant (all P ＜0.O1).Conclusion:The UPLC method has very good precision,stability and recovery,which could meet the requirements of method validation to be used for the content determination of the main flavonoids from Epimedii folium in Erxian Tang and provide the foundations for quality control of Erxian Tang.关键词
淫羊藿/二仙汤/超高效液相色谱法/朝藿定B/朝藿定C/淫羊藿苷/淫羊藿次苷Ⅱ/含量测定Key words
Epimedii folium/Erxian Tang/ultra-high performance liquid chromatography/epimedin B/epimedin C/icariin/icariside Ⅱ/content determination分类
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郭红霞,腊贵晓,代丹丹,理向阳,杨铁钢..超高效液相色谱法检测二仙汤中淫羊藿黄酮类成分的含量[J].中医学报,2018,33(2):286-290,5.基金项目
河南省农业科学院科研发展专项资金项目{豫财预[2017]76-2} （）
