scholarly journals Preparative Separation of Alkaloids from Stem of Euchresta tubulosa Dunn. by High-Speed Counter-Current Chromatography Using Stepwise Elution

Molecules ◽  
2019 ◽  
Vol 24 (24) ◽  
pp. 4602 ◽  
Author(s):  
Weixin Li ◽  
Huan Wang ◽  
Aiwen Dong
Keyword(s):  
High Speed ◽  
Methylene Chloride ◽  
Liquid Extraction ◽  
Preparative Separation ◽  
Target Compound ◽  
Two Phase ◽  
Chinese Herbal ◽  
Liquid Liquid Extraction ◽  
Counter Current ◽  
First Time

Euchresta tubulosa Dunn. is a Chinese herbal medicine with biological activity, but there are few studies on its components at present. Alkaloids in the stem of Euchresta tubulosa Dunn. were isolated and purified by high-speed counter-current chromatography (HSCCC) using stepwise elution. First of all, liquid-liquid extraction (methylene chloride-methanol-water, 5:1:4, v/v) was used for the preliminary enrichment. According to the partition coefficient (K) of a target compound in a series of different two-phase solvents, the final result was that carbon tetrachloride-methylene chloride-methanol-water (2:3:3:2, v/v) (1) and methylene chloride-methanol-water (5:3:2, v/v) (2) were suitable for the HSCCC using stepwise elution. As a result, the purity was all higher than 93% and matrine (1), oxymatrine (2), N-formyl cytisine (3), and N-acetyl cytisine (4) can be eluted at one time by this mode. Cytisine-type alkaloids were isolated for the first time in this plant. Finally, the applicability of the mode was verified.

scholarly journals Preparative Separation of Diterpene Lactones and Flavones from Andrographis paniculate Using Off-Line Two-Dimensional High-Speed Counter-Current Chromatography

Molecules ◽  
2019 ◽  
Vol 24 (3) ◽  
pp. 620 ◽  
Author(s):  
Xiaowei Sun ◽  
Huijiao Yan ◽  
Yujie Zhang ◽  
Xiao Wang ◽  
Dawei Qin ◽  
...  
Keyword(s):  
Ethyl Acetate ◽  
Petroleum Ether ◽  
High Speed ◽  
Spectroscopic Methods ◽  
Two Dimensional ◽  
Preparative Separation ◽  
Counter Current ◽  
First Time

Seven diterpene lactones, andrographolide (1), isoandrographolide (2), neo-andrographolide (3), 14-deoxy-11,12-didehydroandrographolide (4), 14-deoxyandrographiside (5), 14-deoxy-11,12-didehydroandrographiside (6), 3,14-dideoxyandrographolide (10), and three flavones, andrographidine C (7), andrographidine A (8), 5-hydroxy-7,8-dimethoxyflavanone (9) have been successfully and efficiently isolated from A. paniculata using an off-line two dimensional (2D) high-speed counter-current chromatography (HSCCC) method for the first time. For the first dimension HSCCC separation, petroleum ether-ethyl acetate-methanol-water 3:7:5:5 (v/v) was employed to isolate 14.4 mg of compound 1, 3.1 mg of compound 2, 7.8 mg of compound 3, and 18.0 mg of compound 4 from 200 mg of the A. paniculata extract. For the second dimension HSCCC separation, petroleum ether-ethyl acetate-methanol-water 2:8:1:9 (v/v) and 5:5:6:4 (v/v) were employed to isolate the collected fractions ranged from 55 to 79 min and the flow out fraction, respectively, which led to 5.1 mg of compound 5, 4.4 mg of compound 6, 2.4 mg of compound 7, 3.3 mg of compound 8, 4.0 mg of compound 9, 7.0 mg of compound 10. The structures of these diterpene lactones and flavones were elucidated by extensive spectroscopic methods.

scholarly journals A fully automated liquid–liquid extraction system utilizing interface detection

2000 ◽  
Vol 22 (6) ◽  
pp. 187-194 ◽  
Author(s):  
Eugene Maslana ◽  
Robert Schmitt ◽  
Jeffrey Pan
Keyword(s):  
High Speed ◽  
Methylene Chloride ◽  
Phase Interface ◽  
Liquid Extraction ◽  
Automated System ◽  
Extraction System ◽  
Wash Cycle ◽  
Large Sets ◽  
Liquid Liquid Extraction

The development of the Abbott Liquid-Liquid Extraction Station was a result of the need for an automated system to perform aqueous extraction on large sets of newly synthesized organic compounds used for drug discovery. The system utilizes a cylindrical laboratory robot to shuttle sample vials between two loading racks, two identical extraction stations, and a centrifuge. Extraction is performed by detecting the phase interface (by difference in refractive index) of the moving column of fluid drawn from the bottom of each vial containing a biphasic mixture. The integration of interface detection with fluid extraction maximizes sample throughput. Abbott-developed electronics process the detector signals. Sample mixing is performed by high-speed solvent injection. Centrifuging of the samples reduces interface emulsions. Operating software permits the user to program wash protocols with any one of six solvents per wash cycle with as many cycle repeats as necessary. Station capacity is eighty, 15 ml vials. This system has proven successful with a broad spectrum of both ethyl acetate and methylene chloride based chemistries. The development and characterization of this automated extraction system will be presented.

scholarly journals Identification of Transient Receptor Potential Vanilloid 3 Antagonists from Achillea alpina L. and Separation by Liquid-Liquid-Refining Extraction and High-Speed Counter-Current Chromatography

Molecules ◽  
2020 ◽  
Vol 25 (9) ◽  
pp. 2025 ◽  
Author(s):  
Shi-Wei Sun ◽  
Rong-Rong Wang ◽  
Xiao-Ying Sun ◽  
Jia-He Fan ◽  
Hang Qi ◽  
...  
Keyword(s):  
Ethyl Acetate ◽  
High Speed ◽  
Transient Receptor Potential ◽  
Receptor Potential ◽  
Ethanol Extract ◽  
Liquid Extraction ◽  
Transient Receptor Potential Vanilloid ◽  
Liquid Liquid Extraction ◽  
Transient Receptor ◽  
Counter Current

Bioassay-guided fractionation of the ethanol extract of whole herbs of Achillea alpina led to the isolation of isochlorogenic acids A and B as transient receptor potential vanilloid 3 (TRPV3) channel antagonists by using a calcium fluorescent assay. The structures were identified by spectroscopic analysis and the inhibitory activities of isochlorogenic acids A and B were confirmed by whole-cell patch clamp recordings of human embryonic kidney 293 (HEK293) cells expressing human TRPV3. Molecular docking results revealed that these two compounds reside in the same active pocket of human TRPV3 channel protein with lower binding energy than the agonist 2-aminoethoxydiphenyl borate (2-APB). High-speed counter-current chromatography (HSCCC) coupled with a liquid-liquid extraction approach was successfully established for the separation of isochlorogenic acids A and B from the whole herbs of A. alpina. Ethyl acetate and n-hexane-ethyl acetate-water (3:3:4 and 1:5:4, v/v/v) were selected as liquid-liquid extraction solvent systems to remove high- and low-polarity impurities in the mixture. Sixty g of ethanol extract was refined by solvent partition to yield 1.7 g of the enriched fraction, of which 480 mg in turn obtained 52.5 mg of isochlorogenic acid B (purity 98.3%) and 37.6 mg isochlorogenic acid A (purity 96.2%) after HSCCC with n-hexane-ethyl acetate-water containing 1% acetic acid (1:4:8, v/v/v).

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.

Preparative separation of flavonoid glycosides and flavonoid aglycones from the leaves of Platycladus orientalis by REV-IN and FWD-IN high-speed counter-current chromatography

2019 ◽  
Vol 11 (33) ◽  
pp. 4260-4266
Author(s):  
Qian Liu ◽  
Yanling Geng ◽  
Xiao Wang ◽  
Jia Li ◽  
Jinqian Yu
Keyword(s):  
High Speed ◽  
Flavonoid Glycosides ◽  
Preparative Separation ◽  
Flavonoid Aglycones ◽  
Platycladus Orientalis ◽  
Counter Current ◽  
First Time

Three flavonoid glycosides and four flavonoid aglycones were isolated and purified for the first time from the leaves of Platycladus orientalis via two different elution modes of high-speed counter-current chromatography.

Comparison of Sorption and Extraction Methods for Recovery of Trace Organics from Water

1983 ◽  
Vol 15 (6-7) ◽  
pp. 149-159 ◽  
Author(s):  
V C Blok ◽  
G P Slater ◽  
E M Giblin
Keyword(s):  
Solvent Extraction ◽  
Methylene Chloride ◽  
Extraction Methods ◽  
Liquid Extraction ◽  
Standard Mixture ◽  
Liquid Liquid Extraction ◽  
Trace Organics ◽  
Tenax Gc

Several commercially available adsorbents were compared with solvent extraction methods for their utility in recovering trace organics from water. The adsorbents examined included Amberlite XAD-2, XAD-4 and XAD-8, Ambersorb XE340 and XE348 and Tenax-GC. All were found to produce high artifact levels, even after extensive clean-up, making them unsuitable for the analysis of trace organics in water. Quantitatively, Likens-Nickerson or continuous liquid-liquid extraction with méthylene chloride gave better recoveries than the adsorbents. Qualitatively, extractive methods were preferred as they yielded much lower levels of impurities than the adsorbents. These methods of recovering trace organics were evaluated using a standard mixture of compounds added to the water at a level of 55 µg/l. Likens-Nickerson extraction gave comparable recoveries of this mixture at 55 µg/l and 11 µg/l.

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