High-Purity Isolation of Trans-Resveratrol from Rhizma Polygoni Cuspidati by High-Speed Counter-Current Chromatography

2013 ◽  
Vol 690-693 ◽  
pp. 1335-1339
Author(s):  
Jian Chao Deng ◽  
Lai Hao Li ◽  
Xian Qing Yang ◽  
Su Ping Lu ◽  
Yan Yan Wu ◽  
...  
Keyword(s):  
High Speed ◽  
Solvent System ◽  
Separation And Purification ◽  
Two Phase ◽  
Dry Extract ◽  
H Nmr ◽  
Assisted Extraction ◽  
Solvent Systems ◽  
Counter Current ◽  
Chloroform Methanol

In this paper, high-speed counter-current chromatography (HSCCC) was established and successfully applied for the separation and purification of trans-resveratrol from Rhizma Polygoni Cuspidati. After extracted by microwave assisted extraction (MAE), the dry extract was directly dissolved in HSCCC solvent and introduced to HSCCC separation system. Two-phase solvent system of HSCCC was optimized. Trans-resveratrol was separated from extract of Rhizma Polygoni Cuspidati by high-speed counter-current chromatography in two-step using two different solvent systems composed of chloroform-methanol-water (4:3:2, v/v/v) and n-hexane-ethyl acetate-methanol-water (3:5:4:6, v/v/v/v). From 200 mg of crude extract, 2.5 mg of trans-resveratrol was obtained at over 99% purity by HPLC analyses, and its chemical structure was identified by ESI-MS, 1H NMR.

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 Separation of Four Major Bufadienolides from the Chinese Traditional Medicine, Chansu, Using High-Speed Counter-Current Chromatography

2010 ◽  
Vol 5 (7) ◽  
pp. 1934578X1000500 ◽  
Author(s):  
Xiu Lan Xin ◽  
Junying Liu ◽  
Xiao Chi Ma ◽  
Qing Wei ◽  
Li Lv ◽  
...  
Keyword(s):  
High Speed ◽  
Solvent System ◽  
Two Phase ◽  
Isolation And Purification ◽  
H Nmr ◽  
Chemical Structures ◽  
One Step ◽  
Counter Current ◽  
Chloroform Methanol ◽  
C Nmr

A preparative, high-speed, counter-current chromatographic (HSCCC) method for the isolation and purification of bufadienolides from Chansu was successfully developed by using stepwise elution with a two-phase solvent system composed of n-hexane: chloroform: methanol: water (4:1:2.5:5 and 4:1:4:5, v/v). A total of 7.5 mg of cinobufotalin (1), 8.0 mg of bufalin (2), 14.0 mg of cinobufagin (3) and 9.5 mg of resibufogenin (4) were obtained in a one-step separation from 80 mg of the crude extract with purities of 93.2%, 98.7%, 99.2%, and 99.4%, respectively. The chemical structures were determined from 1H NMR and 13C NMR spectroscopic data.

Isolation and Purification of Aloin a and Aloin B by High-Speed Counter-Current Chromatography

2013 ◽  
Vol 634-638 ◽  
pp. 1241-1246 ◽  
Author(s):  
Shi Rong Tang ◽  
Shang Long Chen ◽  
Sang Sang Lu ◽  
Xin Yang Hu
Keyword(s):  
High Speed ◽  
High Performance ◽  
Volume Ratio ◽  
Solvent System ◽  
Two Phase ◽  
Lower Phase ◽  
Isolation And Purification ◽  
Counter Current ◽  
Chloroform Methanol ◽  
Crude Methanol Extract

High-speed counter-current chromatography(HSCCC) was successfully used for isolation and purification of Aloin A and Aloin B from the crude methanol extract of Aloe with a two-phase solvent system composed of chloroform–methanol–n-butylalcohol-water at an optimized volume ratio of 4:3:1:2 (v/v/v/v). The lower phase was used as the mobile phase in the head to tail elution mode. The preparative HSCCC separation was performed on 180 mg of the crude extract yielding pure Aloin A(18mg) and Aloin B(16mg) at purities of 95.2% and 96.8%, respectively, as determined by high performance liquid chromatography (HPLC). HSCCC is a powerful technique for isolation and separation of chemical composition from aloe.

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.

Isolation and Purification of Five Phloroglucinol Derivatives From Agrimonia Pilosa Ledeb by Counter-Current Chromatography Using Non-Aqueous Solvent Systems

2020 ◽  
Author(s):  
Lulu Fu ◽  
Chenghua Lu ◽  
Shengqiang Tong ◽  
Min Xu ◽  
Lan Tang ◽  
...  
Keyword(s):  
Closed Loop ◽  
Solvent System ◽  
The Other ◽  
Second Step ◽  
Two Phase ◽  
Isolation And Purification ◽  
Aqueous Solvent ◽  
Phloroglucinol Derivatives ◽  
Solvent Systems ◽  
Counter Current

Abstract Five non-polar phloroglucinol derivatives, viz. pseudo-aspidin, α-kosin and agripinol A-C were isolated and purified from Agrimonia pilosa Ledeb by semi-preparative counter-current chromatography. The separation was performed by a two-step elution with non-aqueous solvent systems. In the first step, an elution mode of a two-phase solvent system consisting of n-hexane-acetonitrile-dichloromethane-methanol (6:6:0.5:0.5, v/v/v/v) was used. We obtained sample Ι containing three components (47.0 mg) and sample ΙΙ containing two components (24.8 mg) from crude extract (371.0 mg). In the second step, sample Ι was successfully separated by closed-loop recycling mode with a solvent system consisting of n-hexane-acetonitrile-dichloromethane (10:7:3, v/v/v), yielding 17.8 mg of pseudo-aspidin, 18.5 mg of α-kosin and 6.4 mg of agripinol A. The other two compounds—8.7 mg of agripinol B and 13.6 mg of agripinol C—were obtained from sample ΙΙ in the same manner. All the isolated compounds had a high purity exceeding 95%.

Use of O-carboxymethyl chitosan in high-speed counter-current chromatography: a novel additive for a biphasic solvent system

2014 ◽  
Vol 38 (3) ◽  
pp. 1150-1157 ◽  
Author(s):  
Yanjuan Liu ◽  
Gaohong Wang ◽  
Xinyi Huang ◽  
Yongfeng Liu ◽  
Duolong Di
Keyword(s):  
High Speed ◽  
Solvent System ◽  
Carboxymethyl Chitosan ◽  
Separation And Purification ◽  
Active Constituents ◽  
System P ◽  
Natural Plants ◽  
Counter Current

A novel additive,O-carboxymethyl chitosan, for high-speed counter-current chromatography was found and evaluated for the separation and purification of active constituents from natural plants.

scholarly journals Efficient Preparation of Bafilomycin A1 from Marine Streptomyces lohii Fermentation Using Three-Phase Extraction and High-Speed Counter-Current Chromatography

Marine Drugs ◽  
2020 ◽  
Vol 18 (6) ◽  
pp. 332
Author(s):  
Ye Yuan ◽  
Xiaoping He ◽  
Tingting Wang ◽  
Xingwang Zhang ◽  
Zhong Li ◽  
...  
Keyword(s):  
Crude Extract ◽  
High Speed ◽  
Solvent System ◽  
Bafilomycin A1 ◽  
Middle Phase ◽  
Two Phase ◽  
Rapid Separation ◽  
Lower Phase ◽  
Three Phase ◽  
Counter Current

An efficient strategy was developed for the rapid separation and enrichment of bafilomycin A1 (baf A1) from a crude extract of the marine microorganism Streptomyces lohii fermentation. This strategy comprises liquid−liquid extraction (LLE) with a three-phase solvent system (n-hexane–ethyl acetate–acetonitrile–water = 7:3:5:5, v/v/v/v) followed by separation using high-speed counter-current chromatography (HSCCC). The results showed that a 480.2-mg fraction of baf A1-enriched extract in the middle phase of the three-phase solvent system was prepared from 4.9 g of crude extract after two consecutive one-step operations. Over 99% of soybean oil, the main hydrophobic waste in the crude extract, and the majority of hydrophilic impurities were distributed in the upper and lower phase, respectively. HSCCC was used with a two-phase solvent system composed of n-hexane–acetonitrile–water (15:8:12, v/v/v) to isolate and purify baf A1 from the middle phase fraction, which yielded 77.4 mg of baf A1 with > 95% purity within 90 min. The overall recovery of baf A1 in the process was determined to be 95.7%. The use of a three-phase solvent system represents a novel strategy for the simultaneous removal of hydrophobic oil and hydrophilic impurities from a microbial fermentation extract.

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