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作 者:吴明侠[1] 王晶娟[2] 张贵君[2] 孙素琴[3]
机构地区:[1]河南中医学院,郑州450008 [2]北京中医药大学,北京100102 [3]清华大学化学系,北京100084
出 处:《中国实验方剂学杂志》2010年第14期54-57,共4页Chinese Journal of Experimental Traditional Medical Formulae
基 金:河南中医学院博士科研基金(BSJJ2009-11)
摘 要:目的:建立测定野菊花中蒙花苷含量的方法,并且与其红外光谱进行对比研究。方法:以不同产地的供试品为载体,采用HPLC法测定含量,Diamonsil C18色谱柱(4.6mm×250 mm,5μm);流动相A相为0.5%磷酸水溶液,B相为乙腈,进行梯度洗脱,在0~10 min,B相从10%线性改变至20%,10~30 min,B相从20%线性改变至30%;30~40 min,B相从30%线性改变至40%;流速1.0 mL.min-1;检测波长326 nm;柱温35℃。IR光谱采用傅里叶变换红外光谱技术,获得野菊花的红外谱,二阶导数谱和二维相关红外谱。结果:蒙花苷的线性范围为0.262~5.24μg(r=0.999 91),回收率为98.75%,RSD为1.02%。不同产地野菊花由于其中所含蒙花苷含量的差异,在IR二阶导数谱上1 700~1 400 cm-1及二维红外光谱在1 800~800 cm-1波段均有明显区别。结论:建立的HPLC方法测定蒙花苷含量准确、快速、重复性好,适合于测定野菊花中黄酮类成分的含量。野菊花中蒙花苷含量的不同在IR光谱上可以看出差异,可以作为鉴别其质量的参考指标之一。Objective:To develop an HPLC method for determination of Buddleoside from Flos Chrysanthemi Indici. The result was compared with IR spectrums. Method:Flos Chrysanthemi Indici from various habitats were used as test sample and HPLC was used. The chromatographic separation was performed on a Diamonsil C18(4. 6 mm × 250 mm,5 μm) column gradient eluted with a mobile phase of 0. 5% H3PO4(A)-acetonitrile(B),B changed from 10% to 20% in the first 10 min,in the next 20 min,when B changed from 20% to 30% ,and in the last 10 min,B changed to 40% . The detection wavelength was set at 326 nm and column temperature was set at 35 ℃ . The FTIR spectrums,the second-order derivative spectrogram and the two-dimensional infrared correlation spectrograms were used. Result:Buddleoside was linear within the range of 0. 262-5. 24 μg (r = 0. 999 91). The average recovery was 98. 75% ,with RSD 1. 02% (n = 5). There were differences of samples on the second-order derivative spectrogram of Flos Chrysanthemi Indici. in 1 700-1 400 cm -1 and the two-dimensional infrared correlation spectrograms could be classified between frequency range 1 800-800 cm -1. Conclusion:The method was accurate,repetable and suitable to determine buddleoside from Flos Chrysanthemi Indici. The method can be used for quality control of Flos Chrysanthe- mi Indici. IR spectrum can also be used to identify the flavonoids from Flos Chrysanthemi Indici.
关 键 词:高效液相色谱法 傅里叶变换红外光谱法 野菊花 蒙花苷
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