新疆假龙胆的化学成分研究与含量测定  

Study on Chemical Composition and Xanthones Content Determination of Gentianella turkestanorum (Gand.) Holub

作　　者：邹德志[1,2,3] 杨丹[1] 王建华[4] 韩华锐 白小荣[1,2,3] 张春红[1,2,3] 李旻辉[1,2,3,5] 

机构地区：[1]包头医学院,内蒙古包头014060 [2]内蒙古自治区特色药用植物培育与保护工程技术研究中心,内蒙古包头014060 [3]内蒙古自治区特色道地药材资源保护与利用重点实验室,内蒙古包头014060 [4]内蒙古医科大学药学院,内蒙古呼和浩特010110 [5]内蒙古自治区中医药研究所,内蒙古呼和浩特010020

出　　处：《中国现代中药》2017年第6期758-763,共6页Modern Chinese Medicine

基　　金："十二五"国家科技支撑计划项目(2012BAI28B02);国家自然基金项目(81060372);内蒙古自治区科技计划项目(蒙药资源保护与开发利用科研创新平台)

摘　　要：目的:对新疆假龙胆全草进行化学成分初步研究,并对分离得到酮类化类物进行定量分析。方法:采用75%乙醇回流法对新疆假龙胆全草进行提取,粗提物经石油醚、乙酸乙酯、正丁醇依次梯度萃取制备不同极性部分,将石油醚部分和乙酸乙酯部分浸膏分别用硅胶柱层析和葡聚糖凝胶LH-20柱层析分离纯化,所得单体化合物经EI-MS、~1H-NMR、^(13)C-NMR等光谱法进行结构鉴定;建立高效液相测定方法测定新疆假龙胆中3个酮类化合物的含量。结果:从新疆假龙胆中分离得到6个化合物,分别为1,8-二羟基-3,5-二甲氧基酮(1)、1-羟基-3,5,8-三甲氧基酮(2)、1-羟基-3,5-二甲氧基酮(3)、木犀草素(4)、胡萝卜素(5)和β-谷甾醇(6);含量测定方法学结果表明1,8-二羟基-3,5-二甲氧基酮、1-羟基-3,5,8-三甲氧基酮和1-羟基-3,5-二甲氧基酮3个酮化合物分离度较好,分别在35.7~713.4、32~1280、34.3~686 ng时与峰面积呈良好的线性关系,精密度试验RSD分别为0.31%、0.27%、0.25%,稳定性实验的RSD分别为1.05%、1.33%、1.58%,重复性实验的RSD分别为2.48%、0.82%、2.63%,加样回收率分别为103.1%(RSD=1.25%)、100.02%(RSD=0.93%),95.10%(RSD=2.62%);1,8-二羟基-3,5-二甲氧基酮等3个化合物的含量范围分别为0.21%~0.28%、0.65%~0.77%、0.19%~0.15%。结论:新疆假龙胆含有黄酮类、酮类和甾醇类化合物;经方法学考察,本研究建立的高效液相测定方法适合新疆假龙胆中1,8-二羟基-3,5-二甲氧基酮等3个化合物的测定;新疆假龙胆中1,8-二羟基-3,5-二甲氧基酮等3个化合物的含量较高。Objective： To preliminarily study on the chemical constituents of Gentianella turkestanorum （Gand.） Holub and analyze the content of xanthones by HPLC for quantitative analysis. Methods： The herbal material of G. turkestanorum was reflux-extracted by 75% ethanol, the crude extracts were fractionated with petroleum ether, ethyl acetate, and n-BuOH, respectively. The petroleum ethert and ethyl acetate part were extracted by silica gel column chromatogra- phy and Sephadex LH-20 column chromatography gradually to obtain the purified compounds, which were identified by spectral data EI-MS,^1H-NMR and ^13C-NMR. An HPLC method for the content determination of Xanthones compounds 1-3 was estab- lished. Results： Six compounds were isolated and identified from G. turkestanorum. , respectively, swerchirin （1） , 1-hydrox- y-3, 5, 8-trimethoxyxanthone （2） , 1-hydroxy-3, 5- demethoxyxanthone （3） , luteolin （4） , daucosterol （5） and fl- sitos- terol （6）. The resuhs showed that the conditions of the experiment exhibited better performance of separation for compounds 1- 3. Compounds 1-3 formed a good linear relationship at 35. 7 - 713. 4, 32 - 1280, 34. 3 - 686 ng, respectively. Precision RSD were 0. 31%, 0. 27%, 0. 25% and the stability experiments of RSD were 1.05%, 1.33%, 1.58%, respectively. Repeated experiments RSD were 2.48% , 0. 82% and 2. 63%. Meanwhile, the recovery rat were 103. 1% （RSD = 1.25% ）, 100. 02% （RSD =0. 93% ）, 95. 10% （ RSD = 2.62% ）, respectively. The content of compounds 1-3 were 0. 21% - 0. 28%, 0. 65% ~ 0. 77%, 0. 19% ~0. 15%, respectively. Conclusion： The chemical compositions of G. Turkestanorum were mainly flavonoids, xanthones and sterols. The established HPLC method is suitable for the determination of compounds 1-3 isolated from G. turkestanorum.Moreover, the contents of compounds 1-3 were shown in the higher level.

关 键 词：新疆假龙胆 化学成分 黄酮 (口山)酮 含量测定 

分 类 号：R284.1[医药卫生—中药学]