Preparative separation of rhein from Chinese traditional herb by repeated high-speed counter-current chromatography

Seven diterpene lactones, andrographolide (1), isoandrographolide (2), neo-andrographolide (3), 14-deoxy-11,12-didehydroandrographolide (4), 14-deoxyandrographiside (5), 14-deoxy-11,12-didehydroandrographiside (6), 3,14-dideoxyandrographolide (10), and three flavones, andrographidine C (7), andrographidine A (8), 5-hydroxy-7,8-dimethoxyflavanone (9) have been successfully and efficiently isolated from A. paniculata using an off-line two dimensional (2D) high-speed counter-current chromatography (HSCCC) method for the first time. For the first dimension HSCCC separation, petroleum ether-ethyl acetate-methanol-water 3:7:5:5 (v/v) was employed to isolate 14.4 mg of compound 1, 3.1 mg of compound 2, 7.8 mg of compound 3, and 18.0 mg of compound 4 from 200 mg of the A. paniculata extract. For the second dimension HSCCC separation, petroleum ether-ethyl acetate-methanol-water 2:8:1:9 (v/v) and 5:5:6:4 (v/v) were employed to isolate the collected fractions ranged from 55 to 79 min and the flow out fraction, respectively, which led to 5.1 mg of compound 5, 4.4 mg of compound 6, 2.4 mg of compound 7, 3.3 mg of compound 8, 4.0 mg of compound 9, 7.0 mg of compound 10. The structures of these diterpene lactones and flavones were elucidated by extensive spectroscopic methods.

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Development of online-storage inner-recycling counter-current chromatography for the preparative separation of complex components of alkylphenols from sarcotesta of Ginkgo biloba L.

RSC Advances ◽

10.1039/c8ra05618h ◽

2018 ◽

Vol 8 (60) ◽

pp. 34321-34330 ◽

Cited By ~ 2

Author(s):

Daijie Wang ◽

Xiangyun Song ◽

Huijiao Yan ◽

Mengmeng Guo ◽

Ruiming Fu ◽

...

Keyword(s):

Natural Products ◽

Ginkgo Biloba ◽

High Speed ◽

Separation Method ◽

Preparative Separation ◽

Online Storage ◽

Counter Current ◽

Complex Components

High-speed counter-current chromatography (HSCCC) is becoming an effective and non-absorptive separation method from natural products.

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Quick Preparative Separation of Natural Naphthopyranones with Antioxidant Activity by High-Speed Counter-Current Chromatography

Zeitschrift für Naturforschung C ◽

10.1515/znc-2002-11-1217 ◽

2002 ◽

Vol 57 (11-12) ◽

pp. 1051-1055 ◽

Cited By ~ 7

Author(s):

Gilda G. Leitão ◽

Suzana G. Leitão ◽

Wagner Vilegas

Keyword(s):

Antioxidant Activity ◽

Ethyl Acetate ◽

High Speed ◽

Ethanolic Extract ◽

Solvent System ◽

Spectrophotometric Assay ◽

Preparative Separation ◽

Dpph Radical ◽

Preparative Scale ◽

Counter Current

The natural naphthopyranones paepalantine (1), paepalantine-9O-β-ᴅ-glucopyranoside (2) and paepalantine-9-O-β-ᴅ-allopyranosyl-(1→6)-O-β-ᴅ-glucopyranoside (3) were separated in a preparative scale from the ethanolic extract of the capitula of Paepalanthus bromelioides by high-speed counter-current chromatography (HSCCC). The solvent system used was composed of water-ethanol-ethyl acetate-hexane (10:4 : 10:4, v/v/v/v). This technique led to the separation of the three different naphthopyranone glycosides in pure form in approximately 7 hours. Paepalantine showed a good antioxidant activity when assayed by the DPPH radical spectrophotometric assay.

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