scholarly journals Target-Guided Isolation of Three Main Antioxidants from Mahonia bealei (Fort.) Carr. Leaves Using HSCCC

Molecules ◽  
2019 ◽  
Vol 24 (10) ◽  
pp. 1907 ◽  
Author(s):  
Weicheng Hu ◽  
Jing Zhou ◽  
Ting Shen ◽  
Xinfeng Wang
Keyword(s):  
Ethyl Acetate ◽  
High Speed ◽  
High Performance ◽  
Solvent System ◽  
Antioxidant Compounds ◽  
Antioxidant Enzyme Activities ◽  
Chemical Structures ◽  
Integrative System ◽  
Pure Compounds ◽  
Mahonia Bealei

Mahonia bealei (Fort.) Carr. is an economically important plant that is widely cultivated in Southwest China. Its leaves are commonly used for tea and contain an abundance of antioxidant compounds. However, methods of the systematic purification of antioxidants from M. bealei are lacking. In this study, antioxidants from this plant were effectively and rapidly enriched. First, antioxidants were screened using online 1,1-diphenyl-2-picryl-hydrazyl radical (DPPH)–high performance liquid chromatography (HPLC), followed by separation using high-speed countercurrent chromatography with an optical solvent system composed of n-hexane/ethyl acetate/methanol/water (1:5:1:5, v/v/v/v). Three phenolics—chlorogenic acid (1, 8.3 mg), quercetin-3-O-β-d-glucopyranoside (2, 20.5 mg), and isorhamnetin-3-O-β-d-glucopyranoside (3, 28.4 mg)—were obtained from the ethyl acetate-soluble fraction (240 mg) by one-step separation. The chemical structures of the phenolics were characterized by MS and NMR techniques, and the purity of each compound was >92.0% as determined by HPLC. The isolated compounds were assessed by scavenging activities on DPPH and superoxide radicals as well as cytoprotective assays, all of which showed similar trends regarding the antioxidant capacities of the compounds. Moreover, compounds 1–3 significantly attenuated the lipid peroxidation and antioxidant enzyme activities in H2O2-treated RAW264.7 cells. Our study demonstrated the efficiency of a newly developed integrative system for the comprehensive characterization of pure compounds from M. bealei, which will allow their use as reference substances.

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.

Purification of Four Caffeoylquinic Acid Derivatives from the Flowers of Gynura Procumbens by HSCCC

2021 ◽  
Author(s):  
Ming-yuan Cao ◽  
Ju-wu Hu ◽  
Zhen Gu ◽  
Wei Xiong ◽  
Lei Wu ◽  
...  
Keyword(s):  
High Speed ◽  
High Performance ◽  
Solvent System ◽  
Ionization Mass ◽  
Preparative Scale ◽  
Complex Samples ◽  
Chemical Structures ◽  
Caffeoylquinic Acid ◽  
One Step ◽  
First Time

Abstract Four caffeoylquinic acid derivatives from the Gunura procumbens flowers (GPF) were successfully isolated and purified by high-speed counter-current chromatography (HSCCC). Ethyl acetate–methanol–water (3:1:3, v/v/v) was the optimum biphasic solvent system, which was selected by high-performance liquid chromatography (HPLC) and run on a preparative scale where the lower aqueous phase was used as the mobile phase with a head-to-tail elution mode. Chlorogenic acid (3.83 mg), Isochlorogenic acid A (6.51 mg), Isochlorogenic acid B (4.38 mg) and Isochlorogenic acid C (4.47 mg) were obtained for the first time in an one-step HSCCC separation from 800 mg of the crude extracts. The purities of four compounds were determined to be >95% by HPLC. Chemical structures of each isolated compounds were identified by nuclear magnetic resonance and electrospray ionization mass spectrometry methods. It is worth noting that all the four compounds were isolated here for the first time from GPF and this work confirms the effectiveness of HSCCC for the separation of compounds contained in complex samples, and provides a foundation for further exploitation of G. procumbens.

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.

Liquid and Gas Chromatographic Analysis of Diethyl Phthalate in Water and Sediment

1981 ◽  
Vol 64 (6) ◽  
pp. 1403-1407
Author(s):  
William R Payne ◽  
Jacquelyn E Benner
Keyword(s):  
Liquid Chromatography ◽  
Electron Capture ◽  
High Speed ◽  
High Performance ◽  
Detection System ◽  
Solvent System ◽  
Diethyl Phthalate ◽  
Electron Capture Detection ◽  
Gas Liquid Chromatography ◽  
Water And Sediment

Abstract Diethyl phthalate was determined in water and sediment by high performance liquid chromatography (HPLC) and in water by gas-liquid chromatography with electron capture detection (GLC-ECD). Water samples were extracted with hexane, using a high-speed homogenizer-ultrasonic apparatus and a test tube mixer. Sediments were Soxhlet-extracted using acetonitrile. For HPLC, diethyl phthalate was determined in normal phase mode using a Zorbax-CN column, a 2% isopropanol-hexane solvent system, and a UV variable wavelength detector. For GLC-ECD, a 3% SE-30 Gas-Chrom Q column with a 63Ni electron capture detection system was used. Recoveries from fortified samples ranged from 93.9 to 98.0% for water atO.Ol-0.50 ppm, and from 90.0 to 93.6% for sediment atO.2-2.Oppm.

A Novel Methodology that Combined Fast Chromatography and Antioxidant Activities Screening in Baimai Prescription Research

2013 ◽  
Vol 699 ◽  
pp. 349-353
Author(s):  
Zi Qian Zhang ◽  
Xiao Yu Chen ◽  
Yun Xia Duan ◽  
Fang Liang ◽  
Qing Shan Liu ◽  
...  
Keyword(s):  
Ethyl Acetate ◽  
High Speed ◽  
Antioxidant Activities ◽  
Radical Scavenging ◽  
Absorption Spectrometry ◽  
Gradient Elution ◽  
Solvent System ◽  
Difficult Problem ◽  
Flash Chromatography

To tackle the difficult problem of large ethnomedicine compound prescription research in a fast and efficient way, high-speed separation of Baimai prescriptions was performed by automated flash chromatography on 100-g Si flash columns at a flow-rate of 40 mL/min. Petroleum ether, methylene dichloride, ethyl acetate, methanol and water were used in gradient elution solvent system. 69 fractions were obtained as an ethnodrug compounds library. Separation degree of partial fractions were determined by HPLC-UV absorption spectrometry. Antioxidant activities screening of the fractions in 96 well plates was carryied out. Distribution range of fractions with strong scavenging effect of free radical DPPH was identified. Fraction 5-18 and 20 extracted from ethyl acetate exert the strongest antioxidant activities in vitro, and are identified as effective-composite of the prescription in radical scavenging. The results reported here suggest that the methods used may lead to improvements in the research and development of large ethnomedicine compound prescription.

scholarly journals Systematic Separation and Purification of Alkaloids from Euchresta tubulosa Dunn. by Various Chromatographic Methods

Processes ◽  
2019 ◽  
Vol 7 (12) ◽  
pp. 924
Author(s):  
Wei-Xin Li ◽  
Huan Wang ◽  
Ai-Wen Dong
Keyword(s):  
Natural Products ◽  
Silica Gel ◽  
Column Chromatography ◽  
High Speed ◽  
High Performance ◽  
Ionization Mass ◽  
Separation And Purification ◽  
Two Phase ◽  
Rapid Separation ◽  
Chemical Structures

High-speed countercurrent chromatography (HSCCC) and silica gel column chromatography were used to separate and purify alkaloids from Chinese herbal medicine Euchresta tubulosa Dunn. The purpose of this study is to provide a system mode for rapid separation of alkaloids from natural products. In the experiment, the eluent of silica gel column chromatography was screened by thin layer chromatography (TLC) to obtain four components with different polarity. Then, the two-phase solvent systems of different components were selected and purified by HSCCC. Four alkaloids with relatively high content were obtained by this mode successfully, including matrine (28 mg), oxymatrine (32 mg), N-formyl cytisine (24 mg), and cytisine (58 mg). The purity was higher than 91% by high performance liquid chromatography–ultraviolet (HPLC-UV) and their chemical structures were identified by nuclear magnetic resonance (NMR) and electron ionization mass spectrometry (EI-MS). The results showed that the combination of HSCCC and silica gel column chromatography could make alkaloids from natural products separate systematically.

scholarly journals Rapid Identification of Aldose Reductase Inhibitory Compounds fromPerilla frutescens

2013 ◽  
Vol 2013 ◽  
pp. 1-8 ◽  
Author(s):  
Ji Hun Paek ◽  
Kuk Hyun Shin ◽  
Young-Hee Kang ◽  
Jae-Yong Lee ◽  
Soon Sung Lim
Keyword(s):  
Ethyl Acetate ◽  
Chlorogenic Acid ◽  
Aldose Reductase ◽  
Rosmarinic Acid ◽  
High Speed ◽  
Soluble Fraction ◽  
Biological Activities ◽  
Methanol Extracts ◽  
Chemical Structures ◽  
Inhibitory Compounds

The ethyl acetate (EtOAc) soluble fraction of methanol extracts ofPerilla frutescens(P. frutescens) inhibits aldose reductase (AR), the key enzyme in the polyol pathway. Our investigation of inhibitory compounds from the EtOAc soluble fraction ofP. frutescenswas followed by identification of the inhibitory compounds by a combination of HPLC microfractionation and a 96-well enzyme assay. This allowed the biological activities to be efficiently matched with selected HPLC peaks. Structural analyses of the active compounds were performed by LC-MSn. The main AR inhibiting compounds were tentatively identified as chlorogenic acid and rosmarinic acid by LC-MSn. A two-step high speed counter current chromatography (HSCCC) isolation method was developed with a solvent system of n-hexane-ethyl acetate-methanol-water at 1.5 : 5 : 1 : 5, v/v and 3 : 7 : 5 : 5, v/v. The chemical structures of the isolated compounds were determined by1H- and13C-nuclear magnetic resonance spectrometry (NMR). The main compounds inhibiting AR in the EtOAc fraction of methanol extracts ofP. frutescenswere identified as chlorogenic acid (2) (IC50= 3.16 μM), rosmarinic acid (4) (IC50= 2.77 μM), luteolin (5) (IC50= 6.34 μM), and methyl rosmarinic acid (6) (IC50= 4.03 μM).

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).

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