scholarly journals Preparative Purification of Delphinidin 3-0-sambubioside from Roselle (Hibiscus sabdariffa L.) Petals by fast Centrifugation Partition Chromatography

2010 ◽  
Vol 6 (2) ◽  
pp. 999-1004
Author(s):  
Hilaire Tanoh Kouakou ◽  
Laurent Kouakou Kouakou ◽  
Alain Decendit ◽  
Alain Badoc ◽  
Gregory Da-Costa ◽  
...  
Keyword(s):  
Ethyl Acetate ◽  
Amyloid Fibrils ◽  
Hibiscus Sabdariffa ◽  
Partition Chromatography ◽  
Centrifugal Partition Chromatography ◽  
Preparative Scale ◽  
Mobile Phases ◽  
Chromatographic Procedure ◽  
Solvent Systems ◽  
Liquid Chromatographic

Delphinidin 3-0-sambubioside, a Hibiscus anthocyanin, was isolated from MeOH/TFA dried flower of H. sabdariffa. Its purification on preparative scale was obtained by centrifugal partition chromatography (CPC) using the ternary biphasic solvent systems composed of ethyl acetate/1-butanol/water, acidified by 0.1% of TFA. Stationary phase was ethyl acetate/1-butanol/water (5:5:90; v/v). We tested 4 mobile phases and found that the system acetate/1-butanol/water (40:46:14; v/v) was the best to separate anthocyanin mentioned above. This support-free liquid-liquid chromatographic procedure made it possible to isolate delphinidin 3-0-sambubioside from flower of H. sabdariffa. The antiamyloidogenic activity of the isolated stilbenes was evaluated versus b-amyloid fibrils. delphinidin 3-0-sambubioside was found to be active with 67% inhibition at 10 mM.

Measurement of thiamylal and thiopental in plasma by electron capture and flame photometric gas-liquid chromatography.

1977 ◽  
Vol 23 (7) ◽  
pp. 1306-1309 ◽  
Author(s):  
R H Smith ◽  
J A MacDonald ◽  
D S Thompson ◽  
W E Flacke
Keyword(s):  
Liquid Chromatography ◽  
Ethyl Acetate ◽  
Electron Capture ◽  
Internal Standard ◽  
Chromatographic Column ◽  
Gas Liquid Chromatography ◽  
Unchanged Drug ◽  
Chromatographic Procedure ◽  
Isothermal Gas ◽  
Liquid Chromatographic

Abstract We describe an isothermal gas-liquid chromatographic procedure developed for measuring thiamylal and thiopental in plasma. The unchanged drug is extracted into ethyl acetate from acidified plasma, together with an internal standard. The solvent is removed, the residue methylated, aliquots, diluted with benzene, are injected into a 183-cm gas-liquid chromatographic column containing 3% OV-17. Sensitivity of detection is in the nanogram to picogram range.

Use of centrifugal partition chromatography for assessing partition coefficients in various solvent systems

1989 ◽  
Vol 469 ◽  
pp. 91-99 ◽  
Author(s):  
Nabil El Tayar ◽  
Andrew Marston ◽  
Antoine Bechalany ◽  
Kurt Hostettmann ◽  
Bernard Testa
Keyword(s):  
Partition Coefficients ◽  
Partition Chromatography ◽  
Centrifugal Partition Chromatography ◽  
Solvent Systems

A comprehensive classification of solvent systems used for natural product purifications in countercurrent and centrifugal partition chromatography

2015 ◽  
Vol 32 (11) ◽  
pp. 1556-1561 ◽  
Author(s):  
Krystyna Skalicka-Woźniak ◽  
Ian Garrard
Keyword(s):  
Natural Product ◽  
Partition Chromatography ◽  
Centrifugal Partition Chromatography ◽  
Solvent Systems ◽  
Comprehensive Classification

This review is a comprehensive classification of solvent systems used for natural product purifications in countercurrent and centrifugal partition chromatography.

THE IDENTIFICATION OF DIMETHYL-β-PROPIOTHETIN IN THE ALGAE SYRACOSPHAERA CARTERAE AND ULVA LACTUCA

1966 ◽  
Vol 44 (5) ◽  
pp. 519-522 ◽  
Author(s):  
C. S. Tocher ◽  
R. G. Ackman ◽  
J. McLachlan
Keyword(s):  
Thin Layer ◽  
Dimethyl Sulfide ◽  
Ulva Lactuca ◽  
Chromatographic Procedure ◽  
Solvent Systems ◽  
Liquid Chromatographic

Dimethyl-β-propiothetin (DMPT) has been reported to be present in some species of unicellular phytoplankton on the basis of the evolution of dimethyl sulfide (DMS), one of its breakdown products. The presence of DMPT in Syracosphaera carterae has now been confirmed by precipitation of it as the reineckate, with recovery and chromatographic analyses by paper and thin-layer techniques. Multicellular Ulva lactuca, which is known to contain DMPT, was used as a control. All steps were monitored by the gas–liquid chromatographic procedure for measuring DMS. Chromatograms were run in four solvent systems. All parts of the chromatograms were eluted, and tested for DMS. The only portion of any chromatogram that yielded DMS was that area corresponding to the RF value of authentic DMPT.

scholarly journals Bioassay-Guided Separation of Centipeda minima Using Comprehensive Linear Gradient Centrifugal Partition Chromatography

Molecules ◽  
2020 ◽  
Vol 25 (13) ◽  
pp. 3077
Author(s):  
Ji Hoon Kim ◽  
Eun Ju Jung ◽  
Yun Jung Lee ◽  
En Mei Gao ◽  
Ahmed Shah Syed ◽  
...  
Keyword(s):  
Ethyl Acetate ◽  
Gradient Elution ◽  
Solvent System ◽  
Luciferase Assay ◽  
Partition Chromatography ◽  
Centrifugal Partition Chromatography ◽  
Lower Phase ◽  
Linear Gradient ◽  
Centipeda Minima ◽  
Water Saturated

A comprehensive linear gradient solvent system for centrifugal partition chromatography (CPC) was developed for the bioassay-guided isolation of natural compounds. The gradient solvent system consisted of three different ternary biphasic solvents types: n-hexane–acetonitrile–water (10:2:8, v/v), ethyl acetate–acetonitrile–water (10:2:8, v/v), and water-saturated n-butanol–acetonitrile–water (10:2:8, v/v). The lower phase of the n-hexane–acetonitrile–water (10:2:8, v/v) was used as the stationary phase, while its upper phase, as well as ethyl acetate–acetonitrile–water (10:2:8), and water-saturated n-butanol–acetonitrile–water (10:2:8, v/v) were pumped to generate a linear gradient elution, increasing the mobile phase polarity. We used the gradient CPC to identify antioxidant response elements (AREs), inducing compounds from Centipeda minima, using an ARE-luciferase assay in HepG2 cells, which led to the purification of the active molecules 3-methoxyquercetin and brevilin A. The developed CPC solvent systems allow the separation and isolation of compounds with a wide polarity range, allowing active molecule identification in the complex crude extract of natural products.

Liquid Chromatographic Determination of Phenolic Impurities in Technical MCPA Using Electrochemical Detection (Coulometric Mode)

1988 ◽  
Vol 71 (2) ◽  
pp. 325-327
Author(s):  
Yuk Y Wigfield ◽  
Monique Lanouette
Keyword(s):  
Acetic Acid ◽  
Flow Rate ◽  
Chromatographic Determination ◽  
Gradient System ◽  
Mobile Phases ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Solvent Systems ◽  
Liquid Chromatographic

Abstract Fifteen samples of technical 4-chloro-2-methylphenoxy acetic acid (MCPA) from 6 manufacturers were analyzed for the presence of 13 different phenolic impurities. Reverse-phase liquid chromatography with an electrochemical (coulometric mode) detector was used for qualitative and quantitative determinations. The phenols were separated using a 40-70% methanol and 60-30% 0.02M KH2P04 (pH 4.0) 35 min gradient system on a Spheri-5-RP-18 column. Confirmation of the phenols present was done by retention time comparison with the corresponding standards, using 2 other isocratic mobile phases, methanol-0.2M acetic acid (60 + 40) at a flow rate of 1.3 mL/min and acetonitrile-0.02M KH2P04 (45 + 55) (pH 3.0) at a flow rate of 0.90 mL/min. The similarity of results on 3 different solvent systems demonstrates the absence of any interfering responses. 2-Methyl-4-chlorophenol (average 0.168%) and 2-methyl- 4,6-dichlorophenol (average 0.004%) were detected in all 15 samples. 3-Methylphenol (0.002%) and 2,6-dimethyl-4-chlorophenol (0.002%) were detected in one sample only. The minimum detectable amount ranged from 0.1 to 0.6 ng, depending on the phenol. This corresponds to less than 0.002% when expressed relative to the weight of sample. The coefficient of variation for multiple analyses of the same sample (n = 6) is 1% for 2-methyl-4-chlorophenol and 3% for 2-methy 1-4,6- dichlorophenol.

Liquid-chromatographic detection of thiazide diuretics in urine.

1980 ◽  
Vol 26 (6) ◽  
pp. 702-706 ◽  
Author(s):  
P A Tisdall ◽  
T P Moyer ◽  
J P Anhalt
Keyword(s):  
Liquid Chromatography ◽  
Ethyl Acetate ◽  
Spectrophotometric Method ◽  
Mobile Phase ◽  
Reversed Phase ◽  
Analytical Recovery ◽  
Two Samples ◽  
Chromatographic Procedure ◽  
Chromatographic Detection ◽  
Liquid Chromatographic

Abstract We describe a liquid-chromatographic procedure for detection in urine of all thiazide drugs currently used clinically. Urine is treated initially with NaBH4 to convert any chlorothiazide present to hydrochlorothiazide. The urine is acidified with NaH2PO4 (1.0 mol/L, pH 5), and thiazides are extracted with ethyl acetate. Interfering substances are then removed in two washes with 0.1 mol/L Na2HPO4 at pH 8. The ethyl acetate is evaporated and the residue redissolved in mobile phase. Thiazides are assayed by reversed-phase chromatography, with detection by ultraviolet absorption. Analytical recovery of thiazides ranged from 53 to 93%. Urines from 48 patients were so studied, and the results were compared with results by the currently used spectrophotometric method. The two methods agreed for 56% of samples. Evaluation of the discrepancies by review of patients’ histories clearly showed liquid chromatography to have correctly identified seven of eight positive urines that the spectrophotometric method failed to detect. Ultraviolet scanning incorrectly identified as positive two samples, whereas liquid chromatography did not falsely identify any urines as positive. Our method was more sensitive and more specific than the spectrophotometric method.

Sign in / Sign up

Export Citation Format

Share Document