液-质联用分析锦锈杜鹃叶黄酮类成分

目的]采用高效液相色谱—电喷雾离子阱质谱技术对锦锈杜鹃叶中的黄酮类化合物进行分析和鉴定。方法]色谱条件为:Wa-ters C18色谱柱(4.6 mm×250 mm,5μm);流动相A相为水(含浓度0.1%甲酸),流动相B相为无水甲醇;梯度洗脱程序:0～24 min,31%～42%B;24～30 min,42%～50%B;30～35 min,50%～60%B;35～40 min,60%B;进样量20μl;流速为0.7 ml/min;柱温30℃;检测波长356 nm。质谱条件为:电离源:电喷雾离子源;负离子模式扫描;干燥气温度:350℃;干燥气体积流量(N2):10 L/min;雾化气压力275.8 KPa;毛细管电压:3.5 KV,毛细管出口电压100 V;质量扫描范围:m/z 200～700。使用ESI离子源,负离子模式下采集数据。结果]通过与文献数据和部分标准品对照,推断出锦锈杜鹃叶中含有5个黄酮类化合物,分别是金丝桃苷、异槲皮苷、广寄生苷、槲皮苷、槲皮素。结论]液质联用技术具有快速、准确、有效的特点,是一种相对较好的定性测定方法。其对锦锈杜鹃叶中的黄酮类化合物进行分析和鉴定,为今后锦锈杜鹃的应用提供了一定的理论依据。

Analysis of the Flavonoids in the Leaves of Rhododendron Pulchrum Sweet by HPLC-MS

Objective] To investigate the flavonoids in the leaves of Rhododendron pulchrum sweet by high performance liquid chromatograph-electrospray ionization tandem mass spectrometry.Method] The chromatographic separation was performed on a C18 column(4.6 mm ×250 mm,5 μm).The mobile phase A was water containing 0.1% formic acid and mobile phase B was anhydrous methanol.Gradient eluted program was: 0-24 min,31%-42% B;24-30 min,42%-50% B;30-35 min,50%-60% B;35-40 min,60% B.Injection volume was 20 μl,flow rate was 0.7 ml/min,column temperature was 30 ℃,and detection wavelength was 356 nm.Mass spectrometer conditions were ESI,negative ion mode scanning,drying gas temperature 350 ℃,drying gas volume flow(N2) 10 L/min,nebulizing gas pressure 275.8 KPa,capillary voltage 3.5 kV,capillary export voltage 100 V,mass scan range m/z 200-700.Data were collected in negative ion mode.Result] Compared with the standard references and literature data,five flavonoids components were identified as hyperoside,isoquercitrin,avicularin,quercitroside and quercetin.Conclusion] This method was rapid,accurate and effective which could be applied for the constituent identification of R.pulchrum,and provided theoretical basis for the application of R.pulchrum.