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.

Colorimetric and Gas-Liquid Chromatographic Determination of Atropine-Hyoscyamine and Hyoscine (Scopolamine) in Solanaceous Plants

1975 ◽  
Vol 58 (5) ◽  
pp. 884-887
Author(s):  
Mohamed S Karawya ◽  
Samia M Abdel-Wahab ◽  
Mohamed S Hifnawy ◽  
Mohamed G Ghourab
Keyword(s):  
Citric Acid ◽  
Acetic Anhydride ◽  
Thin Layer ◽  
Chromatographic Determination ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Solanaceous Plants ◽  
Liquid Chromatographic ◽  
Colorimetric Methods

Abstract Two colorimetric micromethods are described for the determination of atropine-hyoscyamine and hyoscine (scopolamine), using p-dimethylaminobenzaldehyde and citric acid-acetic anhydride as the color reagents. These methods are sensitive to 60-1200 and 10-360 μg alkaloid/10 ml. The colorimetric methods were also successfully applied after a preliminary thin layer chromatographic separation of the alkaloids. A gasliquid chromatographic procedure was also developed, which yielded comparable results with the colorimetric methods.

An improved rapid thin-layer chromatographic—gas—liquid chromatographic procedure for the determination of free fatty acids in plasma

1989 ◽  
Vol 183 (2) ◽  
pp. 207-215 ◽  
Author(s):  
Hendrik Y. Tichelaar ◽  
A.J.Spinnler Benadé ◽  
Annette K. Daubitzer ◽  
Theunis J.v.W. Kotze
Keyword(s):  
Fatty Acids ◽  
Thin Layer ◽  
Free Fatty Acids ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic

Simple Derivatization Procedure for Gas-Liquid Chromatographic Analysis of Diflubenzuron in Pond Water and for Analysis of Its Trifluoromethyl Analog Penfluron in Boll Weevils

1978 ◽  
Vol 61 (3) ◽  
pp. 629-635
Author(s):  
Albert B DeMilo ◽  
Paul H Terry ◽  
Diane M Rains
Keyword(s):  
Thin Layer ◽  
Chromatographic Analysis ◽  
Boll Weevil ◽  
Pond Water ◽  
Electron Capture Detection ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Analysis ◽  
Natural Pond ◽  
Liquid Chromatographic

Abstract A simple and convenient gas-liquid chromatographic procedure involving electron capture detection is described for determining diflubenzuron (N- [[(4-chlorophenyl) amino] carbonyl] - 2,6-difluorobenzamide) in pond water and for determining the uptake of penfluron (trifluoromethyl analog of diflubenzuron) by boll weevils sexually sterilized by this compound. Both compounds were quantitatively converted to their respective N-(trifluoroacetyl) anilines by treatment with trifluoroacetic anhydride and pyridine in benzene at 50–60 °C. In boll weevil analyses, the procedure was quantitative for penfluron at concentrations involving microgram quantities (10–35 ≧g/weevil) without the necessity of a cleanup step. However, at submicrogram quantities, background interference necessitated a thin layer chromatographic cleanup prior to derivatization. This modification enabled the determination of 100 ng/ weevil. Analysis for diflubenzuron in natural pond water gave excellent results. For example, diflubenzuron at 2, 0.2, and 0.02 ppm in pond water was recovered at 95, 82, and 98%, respectively. A mechanism describing the reaction is proposed.

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.

Thin Layer Chromatographic Detection and Liquid Chromatographic Determination of Stevioside and Rebaudioside A in Beverages and Foods Following Reverse Phase Column Chromatography

1986 ◽  
Vol 69 (5) ◽  
pp. 799-802
Author(s):  
Kenji Fujinuma ◽  
Kazuo Saito ◽  
Mitsuo Nakazato ◽  
Yoko Kikuchi ◽  
Akihiro Ibe ◽  
...  
Keyword(s):  
Thin Layer ◽  
Chromatographic Determination ◽  
Rebaudioside A ◽  
Reverse Phase ◽  
Reverse Phase Column ◽  
Chromatographic Procedure ◽  
Acid Reagent ◽  
Liquid Chromatographic ◽  
Phase Column

Abstract A method for the detection and determination of stevioside and rebaudioside A in beverages and foods by thin layer chromatography (TLC) and liquid chromatography (LC) is presented. Stevioside and rebaudioside A are extracted with water from a sample and purified by a reverse phase column chromatographic procedure using a silica gel 60 silanized column. The eluate from the column is concentrated to dryness, and the resulting residue is dissolved in 80% ethanol. For the detection, TLC is used, and spots of stevioside and rebaudioside A are visualized with anisaldehyde sulfuric acid reagent. Stevioside and rebaudioside A detected in samples are determined by LC with a Finepak SIL NH2 column and a mobile phase of acetonitrile-water (200 + 45) containing tetrabutylammonium phosphate, which is added to achieve the separation from some interfering compounds. Recoveries from samples spiked at 10 and 100 ppm ranged from 97.8 to 100.3% (stevioside) and 96.3 to 99.7% (rebaudioside A).

OPTIMIZATION OF THIN LAYER CHROMATOGRAPHY METHODS FOR SEPARATION AND IDENTIFICATION OF ANTIDEPRESSANTS IN THEIR MIXTURE

2014 ◽  
Vol 21 (1) ◽  
pp. 11-15
Author(s):  
Daiva Kazlauskienė ◽  
Guoda Kiliuvienė ◽  
Palma Nenortienė ◽  
Giedrė Kasparavičienė ◽  
Ieva Matukaitytė
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Solvent System ◽  
Ammonia Solution ◽  
Relative Standard ◽  
Rf Values ◽  
Solvent Systems ◽  
Paroxetine Hydrochloride ◽  
Fluvoxamine Maleate ◽  
Layer Chromatography

By conducting the toxicological analysis it is meaningful to determine the analytical system that could identify simultaneously several medicinal preparations quickly and precisely. The purpose of this work was to create and validate the method of thin-layer chromatography that would be suitable to separate the components of antidepressant mixture (amitriptyline hydrochloride, paroxetine hydrochloride, sertraline hydrochloride, fluvoxamine maleate and buspirone hydrochloride) and to identify them. The system was validated with regard to the sensitivity, repetition of data, resistance and particularity. The solvent systems with potential of high separation of components in their mixture were created: acetonitrile, methanol, ammonia solution 25 percent (85:10:5); acetonitrile, methanol, ammonia solution 25 percent (75:20:5); dichlormethane, 1,4-dioxane, ammonia solution 25 percent (50:45:5); dichlormethane, 1,4-dioxane, ammonia solution 25 percent (42:55:3); trichlormethane, 1,4-dioxane, ammonia solution 25 percent (25:70:5); trichlormethane, 1,4-dioxane, ammonia solution 25 percent (60:36:4). One of the most suitable solvent systems for separation of the analyzed mixture (sertraline, amitriptyline, paroxetine, buspirone, fluvoxamine) was determined – acetonitrile, methanol, ammonia solution 25 percent (85:10:5). When this solvent system was used, the average Rf values of the analyzed compounds differed the most. Validation was conducted – the relative standard deviation (RSD, percent) of the average Rf value of the analyzed compounds varied from 0,6 to 1,8 percent and did not exceed the permissible error of 5 percent. The sensitivity of methodology was determined by assessing the intensity of the mixture’s spots on the chromatographic plate. The detection limit of buspirone was 0,0012 µg; sertraline – 0,0008 µg; amitriptyline – 0,0004 µg; fluvoxamine – 0,0004 µg; paroxetine – 0,0008 µg. The resistance of results to the changed conditions – it was determined that when the amounts of the solvents acetonitrile and methanol were increased or decreased to two milliliters, the average Rf values of the analyzed compounds did not change statistically significantly

Simultaneous liquid-chromatographic determination of vitamin K1 and vitamin E in serum.

1989 ◽  
Vol 35 (12) ◽  
pp. 2285-2289 ◽  
Author(s):  
B E Cham ◽  
H P Roeser ◽  
T W Kamst
Keyword(s):  
Vitamin E ◽  
Human Serum ◽  
High Performance ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Tocopheryl Acetate ◽  
Vitamin K1 ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract We describe a high-performance liquid chromatographic procedure for the simultaneous measurement of vitamins K1 and E in human serum. Delipidated human serum (free of vitamins K1 and E) was used to make standard solutions of these vitamins, and cetyl naphthoate and alpha-tocopheryl acetate were the internal standards for vitamin K1 and vitamin E, respectively. A simple, novel separation method utilizing liquid-liquid partition chromatography was used as a preparative "clean-up" procedure. Cetyl naphthoate and vitamin K1 (after post-column reduction) were detected by fluorescence, alpha-tocopheryl acetate and vitamin E by ultraviolet absorption. Sensitivity (detection limit) of the assay was 30 pg for vitamin K1 and 5 ng for vitamin E per injection. The method is specific, precise, and more rapid than previously described procedures. Within- and between-assay CVs were 8.1% and 12.9%, respectively, for vitamin K1; 3.5% and 6.0%, respectively, for vitamin E. Analytical recoveries of vitamins K1 and E were 80% and 93%, respectively, from serum and from delipidated serum (standards). The average neonatal serum concentration of vitamin K1 was 83 ng/L, 2.5 mg/L for vitamin E; for normolipidemic adults, the values were 343 ng/L and 7.9 mg/L, respectively, and for hyperlipidemic adults, 541 ng/L and 11.1 mg/L, respectively.

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