九里香是传统中药九里香属植物的两个基原植物之一。本研究建立了一种快速、有效的HPLC分析方法,能够实现在20分钟内同时测定九里香中两个香豆素类化合物,海南九里香内酯(1)和橙皮内酯(2),以及一个多甲氧基黄酮类化合物,3,5,6,7,3′,4′,5′-七甲氧基黄酮(3)。色谱条件为采用DIKMA Spursil C18色谱柱,乙腈–水(50:50,v/v)等度洗脱,柱温25 oC,流速1 m L/min,320 nm检测。三个主要成分分离度良好,在测试范围内线性关系良好,r〉0.999;精密度、重复性、稳定性良好;平均加样回收率在100.52%–101.97%之间,RSD值小于2%。采用该方法对20批不同产地的九里香药材进行含量测定,三个主要成分的含量和在1.55–7.45 mg/g。此外,还对九里香不同部位如主茎、侧枝、嫩枝和叶,及不同采收期的药材进行了测定。结果表明,三个主要成分在嫩枝及叶中的含量明显高于主茎或侧枝中,所以药典规定以九里香的叶及嫩枝作为药用部位是合理的;六月或十月为最佳采收期;产自广东茂名市、深圳市、广西南宁市、天峨市和福建漳州市的九里香中主要活性成分的含量高于其他产地。该方法具有高效、简便的特点,可用于九里香药材及其相关产品的质量控制。
Murraya exotica L. is one of the two official source species of traditional Chinese medicine Murrayae Folium et Cacumen. At present, a rapid HPLC analysis method to simultaneously determine two major coumarins, hainanmurpanin (1) and meranzin (2), and one main flavonoid, 3,5,6,7,3',4',5'-heptamethoxyflavone (3), from the leaves and twigs of M. exotica was established. The analysis was performed on a DIKMA Spursil C18 column (4.6 minx250 mm, 5 ~m) at a flow rate of 1 mL/min, using acetonitrile-H20 (5:5, v/v) as mobile phase. The column temperature was 25 ~(2, and the detected wavelength was at 320 nm. The three analytes (1-3) were separated well with good linearity, precision, stability and repeatability. The average recoveries were in the range of 100.52%-101.97%, with RSD less than 1.73%. Twenty batches of M. exotica from different habitats were detected, and the sum of the contents of 1-3 was in the range of 1.55-7.45 mg/g, respectively. Besides, the contents of these three analytes were also determined for the samples from different medicinal parts (stems, lateral branches, mixture of twigs and leaves) and different harvest times. The results showed that the contents of these three analytes in leaves and twigs are much higher than those in the stems or lateral branches; the plants harvested from June or October contain more active compounds than those from the other months. The above results proved that this high performance and simple HPLC assay can be readily utilized as a practical method for the quality control of M. exotica.