Countercurrent chromatography separation of saponins by skeleton type from Ampelozizyphus amazonicus for off-line ultra-high-performance liquid chromatography/high resolution accurate mass spectrometry analysis and characterisation.

IF 1.2 4区材料科学 Q4 ELECTROCHEMISTRY Transactions of The Institute of Metal Finishing Pub Date : 2017-01-20 Epub Date: 2016-12-19 DOI:10.1016/j.chroma.2016.12.053

Fabiana de Souza Figueiredo, Rita Celano, Danila de Sousa Silva, Fernanda das Neves Costa, Peter Hewitson, Svetlana Ignatova, Anna Lisa Piccinelli, Luca Rastrelli, Suzana Guimarães Leitão, Gilda Guimarães Leitão

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引用次数: 16

Abstract

Ampelozizyphus amazonicus Ducke (Rhamnaceae), a medicinal plant used to prevent malaria, is a climbing shrub, native to the Amazonian region, with jujubogenin glycoside saponins as main compounds. The crude extract of this plant is too complex for any kind of structural identification, and HPLC separation was not sufficient to resolve this issue. Therefore, the aim of this work was to obtain saponin enriched fractions from the bark ethanol extract by countercurrent chromatography (CCC) for further isolation and identification/characterisation of the major saponins by HPLC and MS. The butanol extract was fractionated by CCC with hexane - ethyl acetate - butanol - ethanol - water (1:6:1:1:6; v/v) solvent system yielding 4 group fractions. The collected fractions were analysed by UHPLC-HRMS (ultra-high-performance liquid chromatography/high resolution accurate mass spectrometry) and MSⁿ. Group 1 presented mainly oleane type saponins, and group 3 showed mainly jujubogenin glycosides, keto-dammarane type triterpene saponins and saponins with C₃₁ skeleton. Thus, CCC separated saponins from the butanol-rich extract by skeleton type. A further purification of group 3 by CCC (ethyl acetate - ethanol - water (1:0.2:1; v/v)) and HPLC-RI was performed in order to obtain these unusual aglycones in pure form.

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逆流色谱法按骨架类型分离金丝楠木中的皂苷，用于离线超高效液相色谱/高分辨精确质谱分析和表征。

Ampelozizyphus amazonicus Ducke（鼠李科）是一种用于预防疟疾的药用植物，它是一种攀援灌木，原产于亚马逊地区，其主要化合物是苷皂苷。这种植物的粗提取物过于复杂，无法进行任何结构鉴定，而高效液相色谱分离法又不足以解决这一问题。因此，这项工作的目的是从树皮乙醇提取物中通过逆流色谱法（CCC）获得皂苷富集馏分，以便进一步分离，并通过 HPLC 和 MS 对主要皂苷进行鉴定/表征。丁醇提取物采用正己烷-乙酸乙酯-丁醇-乙醇-水（1:6:1:1:6；v/v）溶剂系统进行 CCC 分馏，共得到 4 组馏分。收集到的馏分采用 UHPLC-HRMS（超高效液相色谱/高分辨率精确质谱）和 MSn 进行分析。第 1 组主要为油烷型皂苷，第 3 组主要为大枣皂苷、酮-达玛烷型三萜皂苷和具有 C31 骨架的皂苷。因此，CCC 从富含丁醇的提取物中按骨架类型分离出了皂苷。通过 CCC（乙酸乙酯-乙醇-水（1:0.2:1; v/v））和 HPLC-RI 对第 3 组进行进一步纯化，以获得这些不同寻常的苷元的纯品。

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来源期刊

Transactions of The Institute of Metal Finishing 工程技术-材料科学：膜

CiteScore

3.40

自引率

10.50%

发文量

审稿时长

3 months

期刊介绍： Transactions of the Institute of Metal Finishing provides international peer-reviewed coverage of all aspects of surface finishing and surface engineering, from fundamental research to in-service applications. The coverage is principally concerned with the application of surface engineering and coating technologies to enhance the properties of engineering components and assemblies. These techniques include electroplating and electroless plating and their pre- and post-treatments, thus embracing all cleaning pickling and chemical conversion processes, and also complementary processes such as anodising. Increasingly, other processes are becoming important particularly regarding surface profile, texture, opacity, contact integrity, etc.