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

2002 ◽  
Vol 57 (11-12) ◽  
pp. 1051-1055 ◽  
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.

scholarly journals Preparative Separation of Diterpene Lactones and Flavones from Andrographis paniculate Using Off-Line Two-Dimensional High-Speed Counter-Current Chromatography

Molecules ◽  
2019 ◽  
Vol 24 (3) ◽  
pp. 620 ◽  
Author(s):  
Xiaowei Sun ◽  
Huijiao Yan ◽  
Yujie Zhang ◽  
Xiao Wang ◽  
Dawei Qin ◽  
...  
Keyword(s):  
Ethyl Acetate ◽  
Petroleum Ether ◽  
High Speed ◽  
Spectroscopic Methods ◽  
Two Dimensional ◽  
Preparative Separation ◽  
Counter Current ◽  
First Time

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.

Preparative Separation and Purification of Lancifodilactone C from Schisandra Chinensis (Turcz.) Baill by High-Speed Counter-Current Chromatography

2013 ◽  
Vol 634-638 ◽  
pp. 1502-1505
Author(s):  
Bin Li ◽  
Xian Jun Meng ◽  
Li Jie Zhu ◽  
Xin Yao Jiao
Keyword(s):  
High Speed ◽  
Solvent System ◽  
Butyl Alcohol ◽  
Structure Identification ◽  
Schisandra Chinensis ◽  
Preparative Separation ◽  
Separation And Purification ◽  
Two Phase ◽  
H Nmr ◽  
Counter Current

High-speed counter-current chromatography (HSCCC) was successfully applied to the preparative separation and purification of lancifodilactone C from the crude extracts of Schisandra chinensis (Turcz.) Baill. Following an initial cleaning-up step on the AB-8 macroporous resin, a preparative high-speed counter-current chromatography (HSCCC) with a two-phase solvent system composed of Chloroform- n-Butyl alcohol- methanol -water(10:0.5:8:4，v/v) was used to isolate and separate lancifodilactone C from Schisandra Chinensis(Turcz.) Baill. A total of 101 mg lancifodilactone C with purities of 98.2% were obtained from 1000 mg crude extract in one-step elution and less than 1 h, and the structure identification was performed by UV, IR, MS,1H NMR and13C NMR.

scholarly journals Preparative isolation and purification of seven compounds from Hibiscus mutabilis L. leaves by two-step high-speed counter-current chromatography

2015 ◽  
Vol 21 (2) ◽  
pp. 331-341 ◽  
Author(s):  
Zhuoni Hou ◽  
Xianrui Liang ◽  
Feng Su ◽  
Weike Su
Keyword(s):  
Ethyl Acetate ◽  
High Speed ◽  
Solvent System ◽  
Ionization Mass ◽  
Two Phase ◽  
Purification Method ◽  
Isolation And Purification ◽  
Chemical Structures ◽  
13C Nuclear Magnetic Resonance ◽  
Counter Current

Seven compounds from Hibiscus mutabilis L. leaves were first successfully achieved by two-step high-speed counter-current chromatography with two-phase solvent system composed of n-butanol-ethyl acetate-water (1:6:9, v/v/v) and n-hexane-ethyl acetate-methanol-water (3:5:3:5, v/v/v/v/). The critical experimental parameters of first-step separation were optimized with response surface methodology as follows: flow rate was 1.1 mL/min, revolution speed was 800 rpm and temperature was 30?C. Under the optimal conditions, around 5.0 mg of salicylic acid, 13.6 mg of rutin, 5.5 mg of genistein were obtained in 100 mg crude sample. Then, 9.2 mg of potengriffioside A, 4.7 mg of kaempferol 3-O-rutinoside, 3.0 mg of steppogenin and 2.5 mg of emodin were obtained by second-step separation. The purities of the seven compounds determined by UPLC were 96.2%, 93.8%, 95.4%, 94.3%, 98.0%, 94.1% and 90.8%, respectively. Their chemical structures were identified by electron spray ionization mass spectroscopy (ESI-MS) and 1H, 13C nuclear magnetic resonance (NMR). Furthermore, compound steppogenin and genistein were first reported from Hibiscus mutabilis L. The purification method was simple, efficient and evaded tedious separation process.

scholarly journals Isolation and purification of lignans from Schisandra chinensis by combination of silica gel column and high-speed counter-current chromatography

2013 ◽  
Vol 19 (3) ◽  
pp. 435-440
Author(s):  
Yu Sun ◽  
Shuangshuang Xu ◽  
Yanling Geng ◽  
Xiao Wang ◽  
Tianyou Zhang
Keyword(s):  
Ethyl Acetate ◽  
Petroleum Ether ◽  
Silica Gel ◽  
High Speed ◽  
Solvent System ◽  
Schisandra Chinensis ◽  
Two Phase ◽  
Chemical Structures ◽  
Gomisin A ◽  
Counter Current

Silica gel column combined with high-speed counter-current chromatography separation was successfully applied to the separation of schizandrin (I), angeloylgomisin H (II), gomisin A (III), schisantherin C (IV), deoxyschizandrin (V), ?-schisandrin (VI) and schisandrin C (VII) from the fruits of Schisandra chinensis (Turcz.) Baillon. The petroleum ether extracts of the fruits of S. chinensis were pre-separated first on a silica gel column and divided into two fractions as sample 1 and sample 2. 260 mg of sample 1 was separated by HSCCC using petroleum ether-ethyl acetate-methanol-water (10:8:10:8, v/v) as the two-phase solvent system and 18.2 mg of schizandrin, 15.7 mg of angeloylgomisin H, 16.5 mg of gomisin A and 16.7 mg of schisantherin C were obtained. 230 mg of sample 2 was separated using petroleum ether-ethyl acetate-methanol-water (10:0.5:10:1, v/v) as the two-phase solvent system and 19.7 mg of deoxyschizandrin, 23.4 mg of ?-schisandrin and 18.2 mg of schisandrin C were obtained. The purities of the separated compounds were all over 94% as determined by HPLC. The chemical structures of these compounds were confirmed by ESI-MS and 1H NMR.

scholarly journals Separation of avermectin components from Streptomyces avemitilis extraction using high-speed counter-current chromatography

2013 ◽  
Vol 19 (4) ◽  
pp. 563-571 ◽  
Author(s):  
Weike Su ◽  
Zhuoni Hou ◽  
Xianrui Liang
Keyword(s):  
High Speed ◽  
Solvent System ◽  
Ionization Mass ◽  
Two Phase ◽  
Preparative Scale ◽  
Chemical Structures ◽  
Peak Resolution ◽  
Ionization Mass Spectroscopy ◽  
13C Nuclear Magnetic Resonance ◽  
Counter Current

Three compounds of antibiotics-avermectins from fertilizing product of Streptomyces avemitilis are achieved by high-speed counter-current chromatography (HSCCC) with a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (6:4:5:5, v/v) on a preparative scale. The separation condition was: 1.5 mL/min (0 to 200 min) and 2.0 mL/min (200 to the end), 900 rpm and 20?C based on the peak resolution. About 11.9 mg of avermectin B1a, 1.0 mg of avermectin B1b and 9.6 mg of avermectin B2a from 50 mg of crude extract were obtained by one-step separation. The purities of the three compounds determined by HPLC were 99.7%, 96.2% and 97.6%, respectively. Their chemical structures were identified by electron spray ionization mass spectroscopy (ESI-MS), 1H, 13C nuclear magnetic resonance (NMR).

scholarly journals A Simple and Efficient Two-Dimensional High-Speed Counter-Current Chromatography Linear Gradient and Isocratic Elution Modes for the Preparative Separation of Coumarins from Roots of Toddalia asiatica (Linn.) Lam.

Molecules ◽  
2021 ◽  
Vol 26 (19) ◽  
pp. 5986
Author(s):  
Wenya Ma ◽  
Iftikhar Ali ◽  
Yali Li ◽  
Hidayat Hussain ◽  
Huanzhu Zhao ◽  
...  
Keyword(s):  
Ethyl Acetate ◽  
High Speed ◽  
Solvent System ◽  
Biological Properties ◽  
Two Dimensional ◽  
Linear Gradient ◽  
Anticancer Properties ◽  
Water Solvent ◽  
Toddalia Asiatica ◽  
Counter Current

Toddalia asiatica (L.) Lam. (Rutaceae) has shown a broad spectrum of biological properties, such as anti-inflammatory, antioxidant, antimicrobial, anti-HIV, and anticancer properties. The present study is concerned with the separation of the main components with broad partition coefficients (KD values) from T. asiatica, using linear gradient high-speed counter-current chromatography (LGCCC) combined with an off-line two-dimensional (2D) mode. Similar to the binary gradient HPLC, the LGCCC mode is operated by the adjustment of the proportion between the mobile phase of 5:5:1:9 (v/v) (pump A) and 5:5:4.5:5.5 (v/v) (pump B) in an n-hexane/ethyl acetate/methanol/water solvent system. The off-line 2D-CCC mode was used in this study for the secondary separation of two similar KD value compounds with n-hexane/ethyl acetate/methanol/water (5:5:4:6, v/v). Notably, six coumarins, namely, tomentin (1), toddalolactone (2), 5,7,8-trimethoxycoumarin (3), mexoticin (4), isopimpinellin (5), and toddanone (6), were efficiently separated. The structures of the pure compounds were elucidated by spectral techniques and compared with the literature.

HSCCC Separation of Three Main Compounds from the Crude Extract of Dracocephalum Tanguticum by Using Dimethyl Sulfoxide as Cosolvent

2020 ◽  
Author(s):  
Xue Yang ◽  
Yongling Liu ◽  
Tao Chen ◽  
Nana Wang ◽  
Hongmei Li ◽  
...  
Keyword(s):  
Acetic Acid ◽  
Ethyl Acetate ◽  
Dimethyl Sulfoxide ◽  
Efficient Method ◽  
Crude Extract ◽  
High Speed ◽  
Glacial Acetic Acid ◽  
Butyl Alcohol ◽  
Preparative Hplc ◽  
Counter Current

Abstract Separation of natural compounds directly from the crude extract is a challenging work for traditional column chromatography. In the present study, an efficient method for separation of three main compounds from the crude extract of Dracocephalum tanguticum has been successfully established by high-speed counter-current chromatography (HSCCC). The crude extract was directly introduced into HSCCC by using dimethyl sulfoxide as cosolvent. Ethyl acetate/n-butyl alcohol/0.3% glacial acetic acid (4: 1: 5, v/v) system was used and three target compounds with purity higher than 80% were obtained. Preparative HPLC was used for further purification and three target compounds with purity higher than 98% were obtained. The compounds were identified as chlorogenic acid, pedaliin and pedaliin-6″-acetate.

Sign in / Sign up

Export Citation Format

Share Document