玳玳黄酮自微乳化微丸含量测定及HPLC特征图谱分析  

Determination of the self-microemulsifying pellet of Daidai flavones and analysis of the HPLC characteristic chromatograms

作　　者：吴晓青[1] 陈丹[1] 黄庆德[1] 程清[1] 任瑞琴[1] 曾令军[1] 郑利[1] 

机构地区：[1]福建中医药大学药学院,福州350108

出　　处：《药物分析杂志》2012年第8期1379-1384,共6页Chinese Journal of Pharmaceutical Analysis

基　　金：福建省科技计划重点项目(2010Y0030);福建省科技计划项目(2010Y2004);福建省自然科学基金项目(2010J01189)

摘　　要：目的:建立玳玳黄酮自微乳化微丸中柚皮苷、新橙皮苷HPLC含量测定方法和HPLC特征图谱,为玳玳黄酮自微乳化微丸的质量控制提供有效的方法。方法:含量测定采用Agilent-C18色谱柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.1%磷酸水溶液(22∶78),流速为1.0 mL.min-1,柱温为室温。HPLC特征图谱测定采用250-4 Lichrocart C18色谱柱(250 mm×4.0mm,5μm),流动相为甲醇-乙腈-0.1%的磷酸水溶液,梯度洗脱,流速1.0 mL.min-1,柱温30℃。检测波长均为283 nm。结果:柚皮苷浓度在4.48～17.92μg.mL-1范围内线性关系良好(r=0.9998),平均加样回收率为97.5%(RSD=1.0%);新橙皮苷浓度在5.92～23.68μg.mL-1范围内线性关系良好(r=0.9997),平均加样回收率为98.8%(RSD=0.82%)。在此条件下所建立的特征图谱中各成分得到有效分离,各批玳玳黄酮自微乳化微丸的相似度在0.900～1.000间。结论:HPLC法同时测定玳玳黄酮自微乳化微丸中柚皮苷和新橙皮苷含量的方法简便、准确,建立的HPLC特征图谱可用于评价微丸的物质组成及有效物质群的质量变化,可作为玳玳黄酮自微乳化微丸质量控制的依据。Objective：To provide an effective way for quality control of the self-microemulsifying pellet of Daidai flavones by establishing HPLC methods for the determination of naringin and neohesperidin and analyzing the characteristic chromatograms.Methods：Determination was performed on an Agilent-C18 column（250 mm×4.6 mm,5 μm） using acetonitrile-0.1% phosphoric acid water（22∶ 78） as mobile phase with a flow rate of 1.0 mL· min-1 at room temperature.Characteristic chromatograms were obtained using a 250-4 Lichrocart C18 column（250 mm×4.0 mm,5 μm） with a gradient elution program using methanol,acetonitrile and 0.1% phosphoric acid water as mobile phases.The flow rate was 1.0 mL· min-1 and the column temperature was 30 ℃.The detection wavelength was set at 283 nm.Results：The linear ranges of naringin and neohesperidin were 4.48-17.92 μg·mL-1（r=0.9998） and 5.92-23.68 μg·mL-1（r=0.9997）,and the average recoveries were 97.5% and 98.8% with RSD of 1.0% and 0.82%,respectively.The components of the self-microemulsifying pellet of Daidai flavones were effectively separated under the HPLC conditions for characteristic chromatograms,and the similarity of the samples was in range of 0.900-1.000.Conclusion：The HPLC determination method of naringin and neohesperidin is convenient and accurate.HPLC characteristic chromatograms can be used to evaluate the components of the pellet and quality changes in the active material groups,this method can therefore be used for the quality control of the self-microemulsifying pellet of Daidai flavones.

关 键 词：玳玳黄酮微丸 柚皮苷 橙皮苷 新橙皮苷 特征图谱 

分 类 号：R917[医药卫生—药物分析学]