HPLC法同时测定栀子类药材中10个主要有效成分的含量

Quantitative analysis of ten compounds in fruits of Gardenia by HPLC

目的：建立了同时测定22批栀子类药材中10个主要有效成分（京尼平苷酸、去乙酰基车叶草苷、羟基栀子苷、鸡矢藤次苷甲酯、京尼平龙胆双糖苷、京尼平苷、对香豆酰京尼平龙胆双糖苷、西红花苷-1、西红花苷-2、西红花苷-3）的高效液相色谱检测方法。方法：采用AgilentZorbaxSB—C18（4．6mm×250mm，5μm）色谱柱，以乙腈（A）-0．2％磷酸溶液（B）为流动相，梯度洗脱，流速1．0mL·min^-1；检测波长分别为238nm、440nm。结果：在优化的色谱条件下，10个有效成分浓度在2．16～905μg·mL^-1范围内线性关系良好，相关系数（r）不低于0．9998，检出限为0．02～0．20／μg·mL^-1。22批栀子类药材的含量测定结果表明。京尼平苷是最主要的环烯醚萜类成分，西红花苷-1是最主要的西红花苷类成分。不同产地18批栀子药材中10个成分的含量差异较大，其中京尼平苷、西红花苷-1含量分别为2．30％～4．69％、0．20％～1．06％。结论：该方法为栀子类药材的质量控制提供科学依据。

Objective： To develop an HPLC method for determination of 10 compounds （geniposidie acid, deacetylasperulosidic acid methyl ester, gardenoside, scandoside methyl ester, genipin - 1 - β - D - gentiobio- side, geniposide ,p - trans - coumaroylgenipin gentiobioside, crocin - 1, crocin - 2, croein - 3 ） in fruits of Gardenia. Methods：The HPLC separation was performed on an Agilent Zorbax SB -C18 （4.6mm×250mm,5μm） column eluted with the mobile phases of acetonitrile - 0.2 % phosphoric acid solution in a gradient mode at a flow rate of 1.0 mL · min^-1. The detection wavelength was 238 nm and 440 nm. Results： The chromatographic peaks of ten compounds and the corresponding spectra were ideal under the optimal conditions. The calibration curves of ten analytes were linear in the range of 2.16 - 905 μg·mL^-1, with correlation coeffi- cients more than 0. 9998. The limits of detection （LODs） of ten analytes were in the range of 0.02 - 0.20 μg·mL^-1. As the results of determination of 10 compounds of 22 batches of Gardenia showed, geniposide was the main iridoid substance;crocin - 1 was the most important crocin substance. There was a great difference in the contents of 10 compounds in 18 batches of Fruetus Gardeniae, the contents of geniposide were 2.30% - 4.69% , the contents of crocin - 1 were 0.20% - 1.06%. Conclusion： The method can provide reference for evaluating the quality of fruits of Gardenia. Key words： fruits of Gardenia; iridoids ; crocins ; high performance liquid ehromatography; quantitative analysis