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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。
Jiulixiang is one of the two primordial plants of traditional Chinese medicine Ji Li Xiang genus. In this study, a rapid and effective HPLC analysis method was established to determine the simultaneous determination of two coumarins, nine spirulina lactones (1), and orange lactone (2) in nine minutes in 20 minutes, And a polymethoxyflavonoid, 3,5,6,7,3 ’, 4’, 5’-heptamethoxyflavone (3). The chromatographic conditions were isocratic elution with DIKMA Spursil C18 column, acetonitrile-water (50:50, v / v), column temperature 25 oC, flow rate 1 m L / min and detection at 320 nm. The three main components were well separated and had good linearity within the test range with r> 0.999. The precision, repeatability and stability were good. The average recoveries were between 100.52% and 101.97% with RSD less than 2%. The method was used to determine the contents of nine Jiuxiang herbs in 20 batches of different origins. The contents of three main components were in the range of 1.55-7.45 mg / g. In addition, different parts of Jiuli such as the main stem, collateral, twigs and leaves, and harvesting of different herbs were measured. The results showed that the three main components in the twigs and leaves were significantly higher than the main stem or collateral, so the pharmacopoeia stipulated that nine leaves and twigs as medicinal parts is reasonable; June or October is the most Good harvest; produced in Guangdong Maoming City, Shenzhen, Nanning, Guangxi, Tian’e City and Zhangzhou City, Fujian Province, the main active ingredient content more than other areas. The method is highly efficient and easy to use and can be used for quality control of Jiulixiang herbs and related products.