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 Efficient Counter-Current Chromatographic Isolation and Structural Identification of Two New Cinnamic Acids from Echinacea Purpurea

2012 ◽  
Vol 7 (10) ◽  
pp. 1934578X1200701
Author(s):  
Ying Lu ◽  
JiaYin Li ◽  
MiLu Li ◽  
Xia Hu ◽  
Jun Tan ◽  
...  
Keyword(s):  
High Speed ◽  
Echinacea Purpurea ◽  
Aqueous Acetic Acid ◽  
Ionization Mass ◽  
Separation And Purification ◽  
Cinnamic Acids ◽  
Lower Phase ◽  
Isolation And Purification ◽  
Chemical Structures ◽  
Counter Current

Two new cinnamic acids, 2- O-caffeoyl-3- O-isoferuloyltartaric (3), and 2, 3-di- O-isoferuloyltartaric acid (5), along with three known caffeic acids, cichoric acid (1), 2- O-caffeoyl-3- O-feruloyltartaric acid (2) and 2- O- caffeoyl-3- O-p-coumaroyltartaric acid (4), have been successfully isolated and purified from Echinacea purpurea. In this study, we investigated an efficient method for the preparative isolation and purification of cinnamic acids from E. purpurea by high-speed counter-current chromatography (HSCCC). The separation was performed using a two-phase solvent composed of n-hexane-ethyl-acetate-methanol-0.5% aqueous acetic acid (1:3:1:4, v/v). The upper phase was used as the stationary phase and the lower phase as the mobile phase, with a flow rate of 1.6 mL/min. From 250 mg of crude extracts, 65.1 mg of 1, 8.3 mg of 2, 4.0 mg of 3, 4.5 mg of 4, and 4.3 mg of 5 were isolated in one-step, with purities of 98.5%, 97.7%, 94.6%, 94.3%, and 98.6%, respectively, as evaluated by HPLC-DAD. The chemical structures were identified by electro spray ionization mass spectrometry (ESI-MS) and one- and two-dimensional NMR spectra. HSCCC was very efficient for the separation and purification of the cinnamic acids from E. purpurea.

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 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).

Advances in Separation and Purification of Bioactive Polysaccharides through High-speed Counter-Current Chromatography

2020 ◽  
Vol 58 (10) ◽  
pp. 992-1000
Author(s):  
Yu Yang ◽  
Bilal Muhammad Khan ◽  
Xiping Zhang ◽  
Yongjie Zhao ◽  
Kit-Leong Cheong ◽  
...  
Keyword(s):  
Natural Products ◽  
High Speed ◽  
Solvent System ◽  
Future Research ◽  
Phase System ◽  
Separation And Purification ◽  
Two Phase ◽  
Bioactive Substances ◽  
Efficient System ◽  
Counter Current

Abstract Polysaccharides, with an extensive distribution in natural products, represent a group of natural bioactive substances having widespread applications in health-care food products and as biomaterials. Devising an efficient system for the separation and purification of polysaccharides from natural sources, hence, is of utmost importance in the widespread applicability and feasibility of research for the development of polysaccharide-based products. High-speed counter-current chromatography (HSCCC) is a continuous liquid–liquid partitioning chromatography with the ability to support a high loading amount and crude material treatment. Due to its flexible two-phase solvent system, HSCCC has been successfully used in the separation of many natural products. Based on HSCCC unique advantages over general column chromatography and its enhanced superiority in this regard when coupled to aqueous two-phase system (ATPS), this review summarizes the separation and purification of various bioactive polysaccharides through HSCCC and its coupling to ATPS as an aid in future research in this direction.

Age-Related Differences in Throwing Techniques Used by the Catcher in Baseball

1994 ◽  
Vol 6 (3) ◽  
pp. 225-235 ◽  
Author(s):  
Shinji Sakurai ◽  
Bruce Elliott ◽  
J. Robert Grove
Keyword(s):  
High Speed ◽  
High Performance ◽  
Age Groups ◽  
Three Dimensional ◽  
Transformation Method ◽  
High Speed Photography ◽  
Two Phase ◽  
Ball Speed ◽  
Age Related ◽  
Release Speed

Three-dimensional (3-D) high speed photography was used to record the overarm throwing actions of five open-age, four 18-year-old, six 16-year- old, and six 14-year-old high-performance baseball catchers. The direct linear transformation method was used for 3-D space reconstruction from 2-D images of the catchers throwing from home plate to second base recorded using two phase-locked cameras operating at a nominal rate of 200 Hz. Selected physical capacity measures were also recorded and correlated with ball release speed. In general, anthropometric and strength measures significantly increased through the 14-year-old to open-age classifications, while a range of correlation coefficients from .50 to .84 was recorded between these physical capacities and ball speed at release. While many aspects of the kinematic data at release were similar, the key factors of release angle and release speed varied for the different age groups.

scholarly journals Isolation and Identification of Anthocyanin Component in the Fruits of Acanthopanax Sessiliflorus (Rupr. & Maxim.) Seem. by Means of High Speed Counter Current Chromatography and Evaluation of Its Antioxidant Activity

Molecules ◽  
2020 ◽  
Vol 25 (8) ◽  
pp. 1781 ◽  
Author(s):  
Liang Chen ◽  
Xiulan Xin ◽  
Hui Feng ◽  
Shuangshi Li ◽  
Qiguang Cao ◽  
...  
Keyword(s):  
Antioxidant Activity ◽  
High Speed ◽  
Radical Scavenging ◽  
Ionization Mass ◽  
Anthocyanin Content ◽  
Separation And Purification ◽  
Isolation And Identification ◽  
Antioxidant Power ◽  
Acanthopanax Sessiliflorus ◽  
Counter Current

Acanthopanax sessiliflorus (Rupr. & Maxim.) Seem. (Araliaceae) is one of the most abundant species of genus Acanthopanax. The fruits of A. sessiliflorus are used in traditional medical protocols as an analgesic, tonic, antidiabetic, antihypertensive, anti-inflammatory, antitumor, and immune-stimulating agent. In this work, we carried out a comprehensive investigation into the anthocyanin components in the fruits of A. sessiliflorus. The anthocyanin content in the fresh fruits of A. sessiliflorus was determined by high performance liquid chromatography-diode array detection (HPLC/DAD), and the anthocyanin component was isolated from these using high-speed counter-current chromatography (HSCCC) and elucidated by electro-spray ionization-mass spectrometry (ESI/MS), 1H- and 13C-NMR. Its antioxidant activity was evaluated by ferric-reducing antioxidant power (FRAP) and 2,2-diphenyl-1-picrylhydrazyl (DPPH). We found that A. sessiliflorus contained a gross anthocyanin content of 121.35 mg/100 g. HSCCC was successfully used for separation and purification of the primary anthocyanin component, cyanidin 3-xylosyl-galactoside. The antioxidant and radical scavenging tests indicated that cyanidin 3-xylosyl-galactoside is a potent antioxidant.

Chemical Constituents of the Lichen Cladina macaronesica

1991 ◽  
Vol 46 (1-2) ◽  
pp. 12-18 ◽  
Author(s):  
Antonio G . González ◽  
Jaime Bermejo Barrera ◽  
Elsa Ma Rodríguez Pérez ◽  
Consuelo E. Hernández Padrón
Keyword(s):  
Natural Products ◽  
Phenolic Compounds ◽  
Silver Nitrate ◽  
Silica Gel ◽  
Column Chromatography ◽  
Chemical Constituents ◽  
Usnic Acid ◽  
Acetone Extract ◽  
First Time

Column chromatography of the acetone extract of the lichen Cladina macaronesica (Sephadex LH-20, silica gel and silver nitrate-im pregnated silica gel) afforded eight triterpenes identified by chemical and spectral m eans. α-Amyrenone, lupenone, taraxerol, taraxerone and /so-arborinol acetate were isolated for the first time from lichens and (-)-usnic acid and five mononuclear phenolic compounds were also obtained, four for the first time as natural products. The possible transformation of perlatolic acid into these phenolic compounds is briefly outlined.

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