Ethyl acetate–n-butanol gradient solvent system for high-speed countercurrent chromatography to screen bioactive substances in okra

2014 ◽  
Vol 1359 ◽  
pp. 117-123 ◽  
Author(s):  
Hao Ying ◽  
Heyuan Jiang ◽  
Huan Liu ◽  
Fangjuan Chen ◽  
Qizhen Du
2002 ◽  
Vol 57 (11-12) ◽  
pp. 1051-1055 ◽  
Author(s):  
Gilda G. Leitão ◽  
Suzana G. Leitão ◽  
Wagner Vilegas

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.


2013 ◽  
Vol 699 ◽  
pp. 349-353
Author(s):  
Zi Qian Zhang ◽  
Xiao Yu Chen ◽  
Yun Xia Duan ◽  
Fang Liang ◽  
Qing Shan Liu ◽  
...  

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.


2020 ◽  
Vol 1629 ◽  
pp. 461426
Author(s):  
Xu Wang ◽  
Chen Liu ◽  
Qing-Yun Ma ◽  
Zhen-Hua Tian ◽  
Hai-Qiang Jiang ◽  
...  

Fermentation ◽  
2021 ◽  
Vol 7 (4) ◽  
pp. 230
Author(s):  
Huanzhu Zhao ◽  
Xiangyun Song ◽  
Iftikhar Ali ◽  
Manzoor Hussain ◽  
Andleeb Mehmood ◽  
...  

A silver ion high-speed counter-current chromatography ([Ag+]-HSCCC) was developed to separate and purify five sesquiterpenoids from germacrene A fermentation broth. The solvent system was consisted of n-hexane-methanol-silver nitrate (3 mol/L) solution (10:9.5:0.5, v/v). By employing this chromatographic protocol, five sesquiterpenoids named β-elemene (1; 54.1 mg), germacrene A (2; 28.5 mg), γ-selinene (3; 4.6 mg), β-selinene (4; 3.4 mg), and α-selinene (5; 1.3 mg) were obtained successfully from 500 mg extracted crude sample with purities of 97.1%, 95.2%, 98.2%, 96.3% and 98.5%, respectively, combined with preparative HPLC. The results reveal that the addition of metal ion in biphasic solvent system significantly improved the HSCCC separation factor of sesquiterpenoids. Meanwhile, our study also provided an alternate approach to separate the compounds with less polarity, also geometrical isomers and various natural product classes.


2015 ◽  
Vol 21 (2) ◽  
pp. 331-341 ◽  
Author(s):  
Zhuoni Hou ◽  
Xianrui Liang ◽  
Feng Su ◽  
Weike Su

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.


2013 ◽  
Vol 19 (3) ◽  
pp. 435-440
Author(s):  
Yu Sun ◽  
Shuangshuang Xu ◽  
Yanling Geng ◽  
Xiao Wang ◽  
Tianyou Zhang

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.


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