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基于薄层色谱和指纹图谱的百合成分差异性研究

Compositional Differences of Lilii Bulbus Based on Thin Layer Identification and Fingerprint
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摘要 目的:建立卷丹、百合、细叶百合3个基原药材及对应蜜百合鉴别的薄层色谱法(TLC)和指纹图谱方法,对各基原药材所含有的化学成分进行差异性研究。方法:采用Ultimate XB C18色谱柱(250 mm×4.6 mm,5μm),以乙腈(A)-0.1%磷酸水溶液(B)为流动相,梯度洗脱;建立21批不同基原百合药材高效液相色谱法指纹图谱,并进行相似度评价、聚类分析、主成分分析、正交偏最小二乘法-判别分析,评价不同基原百合的异同。同时采用硅胶G薄层色谱板,分别以乙酸乙酯-甲醇-甲酸-水(18∶2∶1.5∶1)、乙醚-正丁醇-冰乙酸(3∶9∶6)为展开剂,建立不同基原百合药材及蜜百合的薄层色谱区分方法,全面展现不同基原百合及蜜百合中化学成分特点。结果:指纹图谱结果显示,不同基原百合药材差异明显,卷丹、百合、细叶百合样品分别标定8、12、8个峰,共有成分为高泛酸、王百合苷H、王百合苷A,而王百合苷I存在于百合、细叶百合中,2-乙酰王百合苷A存在于卷丹中;不同基原百合的相似度评价结果(均小于0.50)显示其成分差异较大;经统计分析发现,不同基原百合分别聚为一类;峰12(2-乙酰王百合苷A)、峰13、峰14、峰11(王百合苷I)、峰3(高泛酸)是卷丹、百合、细叶百合的差异性成分。TLC结果表明,不同基原百合的色谱斑点存在明显差异,可与指纹图谱结果相互印证;而蜜百合TLC存在蔗糖、果糖、葡萄糖斑点,百合药材仅存在蔗糖斑点,这种成分差异来源于炼蜜。结论:所建立的指纹图谱及TLC可对百合药材进行质量评价,且能快速、准确、直观地反映不同基原百合药材及蜜百合中含有的成分差异,为不同基原百合药材和蜜百合的质量控制及区分鉴别提供参考。 Objective:To establish thin-layer chromatography(TLC)and fingerprint methods for the identification of three original medicinal materials(Lilium lancifolium Thunb.,L.brownii F.E.Brown var.viridulum Baker,and L.pumilum DC.)of Lilii Bulbus and their corresponding honey-processed products and to study the differences in their chemical components.Methods:The study employed an Ultimate XB C18 chromatographic column(250 mm×4.6 mm,5μm)with a mobile phase of acetonitrile(A)and 0.1%phosphoric acid aqueous solution(B)in a gradient elution.High-performance liquid chromatography(HPLC)fingerprint profiles were established for 21 batches of different original medicinal materials of Lilii Bulbus.Similarity evaluation,cluster analysis,principal component analysis,and orthogonal partial least squaresdiscriminant analysis(OPLS-DA)were performed to assess the similarities and differences among different Lilium species.For TLC,silica gel G plates were used with ethyl acetate-methanol-formic acid-water(18:2:1.5:1)and ether-n-butanol-glacial acetic acid(3:9:6)as the developing agents to establish differentiation methods for different original Lilium medicinal materials and honey-processed products.This comprehensive approach aimed to display the chemical composition characteristics of different original Lilium species and honey-processed products.Results:The fingerprint profiles showed significant differences among the different original Lilium medicinal materials.Samples of L.lancifolium Thunb.,L.brownii F.E.Brown var.viridulum Baker,and L.pumilum DC.had 8,12,and 8 peaks,respectively.Common components included homopantothenic acid,regaloside H,and regaloside A.Regaloside I existed in L.brownii F.E.Brown var.viridulum Baker,and L.pumilum DC.,while 2-acetate regaloside A existed in L.lancifolium Thunb..The similarity evaluation results(all less than 0.50)indicated considerable differences in their components.Statistical analysis revealed that the different original Lilium species were clustered into distinct groups.Peaks 12(2-acetyl regaloside A),13,14,11(regaloside I),and 3(homopantothenic acid)were identified as differential components among L.lancifolium Thunb.,L.brownii F.E.Brown var.viridulum Baker,and L.pumilum DC.TLC results demonstrated significant differences in chromatographic spots among different original Lilium species,which corroborated the fingerprint profile results.Additionally,TLC of honey-processed products showed spots for sucrose,fructose,and glucose,while Lilium medicinal materials only had sucrose spots,indicating the differences arising from the honey-processing.Conclusion:The established fingerprint and TLC methods can effectively evaluate the quality of Lilium medicinal materials.These methods provide a quick,accurate,and intuitive way to reflect the differences in components among different original Lilium species and honey-processed products,offering reference standards for quality control and differentiation of various Lilium medicinal materials and honey-processed products.
作者 魏家保 唐双燕 谢嘉慧 詹智洪 蔡素琴 黄凯伟 赵伟志 张辉 谭沛 WEI Jia-bao;TANG Shuang-yan;XIE Jia-hui;ZHAN Zhi-hong;CAI Su-qin;HUANG Kai-wei;ZHAO Wei-zhi;ZHANG Hui;TAN Pei(China Resources Sanjiu Modern Chinese Medicine Pharmaceutical Co.,Ltd.,Huizhou 516000,China;Anhui Provincial Key Laboratory of Chinese Medicine Formulation Granules,Huaibei 235000,China;China Resources Sanjiu Pharmaceutical Co.,Ltd.,Shenzhen 518000,China)
出处 《中国现代中药》 CAS 2024年第9期1503-1510,共8页 Modern Chinese Medicine
基金 深圳市科技计划项目(JSGG20191129093418578)。
关键词 百合 蜜炙 不同基原 薄层色谱法 指纹图谱 区分鉴别 Lilii Bulbus processing with honey different origins TLC fingerprint distinguish and identify
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