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%.

scholarly journals Sugaring-out strategy for counter-current chromatography isolation: podophyllotoxins and flavones from Dysosma versipellis as examples

RSC Advances ◽  
2017 ◽  
Vol 7 (19) ◽  
pp. 11591-11600 ◽  
Author(s):  
Lihong Zhang ◽  
Yanyan Wang ◽  
Shihua Wu
Keyword(s):  
Solvent System ◽  
Two Phase ◽  
System P ◽  
Dysosma Versipellis ◽  
Solvent Systems ◽  
Counter Current

In this work, we introduced a sugaring-out strategy for optimizing two-phase solvent systems for counter-current chromatography by adding some sugars into the selected two-phase solvent system.

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 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.

Isolation and Purification of Ginkgo Flavonoids by High-Speed Counter-Current Chromatography

2013 ◽  
Vol 781-784 ◽  
pp. 741-745
Author(s):  
Sang Sang Lu ◽  
Hui Song ◽  
Jing Zhi Miao ◽  
Shi Rong Tang
Keyword(s):  
Mobile Phase ◽  
High Speed ◽  
High Performance ◽  
Leaf Extract ◽  
Volume Ratio ◽  
Solvent System ◽  
Two Phase ◽  
Lower Phase ◽  
Isolation And Purification ◽  
Counter Current

High-speed counter-current chromatography (HSCCC) was successfully used for isolation and purification of Ginkgo flavonoids from the Ginkgo biloba L. leaf extract (GBE) with a two-phase solvent system composed of n-hexaneethyl acetatemethanolwater at an optimized volume ratio of 4:6:5:5(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 200 mg of GBE yielding pure Quercetin (22mg), Kaempferol (15mg) and Isorhamnetin (4mg) at purities of 96.6%, 92.3% and 93.6%, respectively, as determined by high performance liquid chromatography (HPLC). HSCCC is a powerful technique for isolation and separation of chemical composition from GBE.

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.

Flow Split Relationships in Two-Phase Parallel Channel Flows

1982 ◽  
Vol 104 (4) ◽  
pp. 455-462
Author(s):  
O. C. Iloeje ◽  
J. A. Kervinen ◽  
J. Ireland ◽  
B. S. Shiralkar
Keyword(s):  
Single Phase ◽  
The Other ◽  
Simple Relationship ◽  
Two Phase ◽  
Void Fractions ◽  
Vapour Flux ◽  
Phase Liquid ◽  
Flow Quality ◽  
Counter Current ◽  
Phase Fluid

The observed flow combinations through the channels were: cocurrent upflow in both channels, cocurrent upflow in one and countercurrent flow in the other channel, and cocurrent upflow in one and single phase liquid downflow in the other channel. The flow regimes in each channel varied from churn-turbulent, through anular flow, to chugging counter-current flow, as the flow conditions were varied. It was observed that the flow combination obtained was history dependent. However, for given flow combinations, certain flow split relationships were established. With both channels in cocurrent upflow, the flow quality into each channel was approximately the same as the flow quality in the lower plenum at the flow split elevation. For the other flow combinations, a simple relationship between the void fractions at the bottom of the channels which had two phase fluid, and the average void fraction and vapour flux in the lower plenum at the flow split elevation, was established.

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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