Counter-current chromatography with off-line detection by ultra high performance liquid chromatography/high resolution mass spectrometry in the study of the phenolic profile of Lippia origanoides

被引：25

作者：

Leitao, Suzana Guimaraes ^{[1
]}

Leitao, Gilda Guimaraes ^{[2
]}

Vicco, Douglas K. T. ^{[1
]}

Barreto Pereira, Joao Paulo ^{[2
]}

Simao, Gustavo de Morais ^{[1
]}

Oliveira, Danilo R. ^{[1
]}

Celano, Rita ^{[3
]}

Campone, Luca ^{[3
]}

Piccinelli, Anna Lisa ^{[3
]}

Rastrelli, Luca ^{[3
]}

机构：

[1] Univ Fed Rio de Janeiro, Fac Farm, CCS, Bloco A,2 Andar, BR-21941590 Rio De Janeiro, RJ, Brazil

[2] Univ Fed Rio de Janeiro, Inst Pesquisas Prod Nat, CCS, Bloco H, BR-21941902 Rio De Janeiro, RJ, Brazil

[3] Univ Salerno, Dipartimento Farm, Via Giovanni Paolo 2, I-84084 Fisciano, Italy

来源：

JOURNAL OF CHROMATOGRAPHY A | 2017年 / 1520卷

关键词：

High-speed counter-current chromatography; HILIC; Monolitic reversed phase; Particulate reversed phase; UHPLC-MS; Flavonoids; HPLC-PDA-MS; HYDROALCOHOLIC EXTRACT; NMR CHARACTERIZATION; FLAVONOIDS; STRATEGY; LEAVES; DERIVATIVES; IONIZATION; SEPARATION; PRODUCTS;

D O I：

10.1016/j.chroma.2017.09.004

中图分类号：

Q5 [生物化学];

学科分类号：

071010 ; 081704 ;

摘要：

Lippia origanoides (Verbenaceae) is an important Brazilian medicinal plant, also used for culinary purposes. Most chemical studies with this plant have been focused on its volatile composition. In this work, we combined High-Speed Counter-current Chromatography (HSCCC) and High Performance Liquid Chromatography coupled to Ultra Violet detection and High Resolution Mass Spectrometry (HPLC-UV-HRMS9 methodologies to access the non-volatile chemical composition of L. origanoides. The crude ethanol extract of L. origanoides (LOEF) was first analyzed by HPLC-UV-HRMSn and allowed the identification of 7 major compounds. Among them, eriodictyol, naringenin and pinocembrin, were determined and are phytochemical markers of this plant. However, owing to the complexity of this plant matrix, LOEF was fractionated by HSCCC (hexane-ethanol-water, 4:3:1) as a tool for preparative pre-purification, affording a fiavonoid-rich fraction. A column screening with the chromatographic stationary phases ZIC-HILIC, monolithic and particulate RP18 was performed. The best column separation was achieved with a Puraspher STAR RP18e, which was used for HPLC-DAD-HRMS" studies. By this approach 12 compounds were further identified in addition to the major ones identified in the raw extract. Two of them, 6,8di-C-hexosyl-luteolin and 6,8-di-C-glucosyl-apigenin, are being reported for the first time in the family Verbenaceae. This work shows the integration of HSCCC as a preparative tool for the fractionation and purification of natural products from a complex plant extract with other analytical techniques, with the purpose of showing each technique's potential. (C) 2017 Elsevier B.V. All rights reserved.

引用

页码：83 / 90

页数：8