旱柳叶中三种黄酮类成分及水杨苷含量的高效液相色谱法测定

Simultaneous Determination of Four Active Compounds in Salix matsudan(Koidz) by HPLC

目的建立同时测定旱柳叶中木樨草素-7-O-葡萄糖苷、水杨苷、芹菜素-3'-氧乙基-7-O-葡萄糖苷及杨梅酮含量的高效液相色谱(HPLC)方法。方法 Nucleosil C18(4.6 mm×250 mm,5μm)色谱柱,以乙腈-水(5∶95)-(30∶70)为梯度流动相;流速为1.0 ml.min-1;检测波长为246 nm;柱温为25℃。结果木樨草素-7-O-葡萄糖苷在0.02～0.1 mg范围内与峰面积呈良好线性关系,R=0.999 0,平均回收率为97.81%,RSD为2.93%;水杨苷在0.03～0.15 mg范围内与峰面积呈良好线性关系,R=0.998 8,平均回收率为97.54%,RSD为1.62%;芹菜素-3'-氧乙基-7-O-葡萄糖苷在0.008～0.04 mg范围内与峰面积呈良好线性关系,R=0.999 1,平均回收率为97.41%,RSD为1.37%;杨梅酮在0.04～0.2 mg范围内与峰面积呈良好线性关系,R=0.9977,平均回收率为97.91%,RSD为1.03%。结论此法简便快速,结果准确可靠、重复性好,可用于药材中木樨草素-7-O-葡萄糖苷、水杨苷、芹菜素-3'-氧乙基-7-O-葡萄糖苷及杨梅酮含量的同时测定。

Objective To establish the HPLC method for the determination of luteolin-7-O-glucoside,salicin,apigenin-3＇-Oxyethyl-7-O-glucoside and myricetin in the leaves of Salix matsudan. Methods The column was Nucleosil C18（4.6 mm×250 mm,5 μm） column,the mobile phase for gradient elution was acetonitrile and water（5∶95）-（30∶70）,the flow rate was 1.0 ml·min-1,the detection wavelength was 246nm and the column temperature was 30℃. Results The calibration curves were linear with correlation coefficients of 0.999 0,0.998 8,0.999 1,0.997 7 for luteolin-7-O-glucoside,salicin,apigenin-3＇-Oxyethyl-7-O-glucoside and myricetin,respectively.The RSDs were2.93%,1.62%,1.37%,1.03% in the concentration ranges of 0.02～0.1 mg,0.03～0.15 mg,0.008～0.04 mg,0.04～0.2 mg and the recoveries were 97.81%,97.54%,97.41%,97.91% for luteolin-7-O-glucoside,salicin,apigenin-3＇-Oxyethyl-7-O-glucoside and myricetin,respectively. Conclusion The developed HPLC method is an attractive alternative for the simultaneous quantitative determination of luteolin-7-O-glucoside,salicin,apigenin-3＇-Oxyethyl-7-O-glucoside and myricetin with regard to the simplicity,accuracy,and repeatability.