scholarly journals Alkylresorcinols in rye (Secale cereale L.) grains. I. Micromethod for determination of alkyl derivatives of resorcinol in rye grain

2015 ◽  
Vol 44 (4) ◽  
pp. 479-489 ◽  
Author(s):  
W. Mejbaum-Katzenellenbogen ◽  
F. Tłuścik ◽  
A. Kozubek ◽  
A. Sikorski
Keyword(s):  
Preparative Thin Layer Chromatography ◽  
Uv Spectrum ◽  
Selective Determination ◽  
Alkyl Derivatives ◽  
Secale Cereale L ◽  
Spectrum Characteristic ◽  
Acetone Extracts ◽  
Layer Chromatography ◽  
Derivatives Of

A pure preparation of alkylresorcinol from rye grains was obtained by preparative thin-layer chromatography, which gave a UV spectrum characteristic for 5-n-alkylresorcinols and orcinol. This preparation served as standard in the elaboration of a micro method (for alkylresorcinols determination in acetone extract from rye grain. It was found that this method is suitable for selective determination of 5-n-alkylrezorcinols in acetone extracts from rye grains.

scholarly journals Alkylresorcinols of rye (Secale cereale L.) caryopses IV. Three-step preparation of 5-n-alkylresorcinols

2015 ◽  
Vol 47 (4) ◽  
pp. 379-389 ◽  
Author(s):  
W. Mejbaum-Katzenellenbogen ◽  
F. Tłuścik ◽  
A. Kozubek
Keyword(s):  
Thin Layer ◽  
Secale Cereale ◽  
Room Temperature ◽  
Uv Spectrum ◽  
Wheat Grains ◽  
Alkyl Derivatives ◽  
Secale Cereale L ◽  
Spectrum Characteristic ◽  
Layer Chromatography ◽  
Derivatives Of

Whole rye or wheat grains were extracted with acetone at room temperature. The extracts were pooled and acetone was evaporated. The remaining acetone oil was washed out with n-pentane until a colourless filtrate was obtained. The residue was dried, then dissolved in chloroform-acetone (95:5) mixture and separated by column chromatography on silica gel. The fractions containing 5-n-alkylresorcinols were pooled, condensed and crystallised from n-hexane. The preparation obtained was homogeneous in thin-layer chromatography and gave the UV spectrum characteristic for 5-n-alkyl derivatives of resorcinol.

scholarly journals Alkylresorcinols in rye (Secale cereale L.) grains. VI. Colorimetric micromethod for the determination of alkylresorcinols with the use of diazonium salt, Fast Blue B

2014 ◽  
Vol 50 (4) ◽  
pp. 645-651 ◽  
Author(s):  
Franciszek Tłuścik ◽  
Arkadiusz Kazubek ◽  
Wanda Mejbaum-Katzenellenbogen
Keyword(s):  
Secale Cereale ◽  
Diazonium Salt ◽  
Precise Method ◽  
Fast Blue ◽  
Alkyl Derivatives ◽  
Secale Cereale L ◽  
Derivatives Of

A simple and precise method for alkylresorcinols determination was elaborated. The method a based on coupling of alkylresorcinals with diazotized Fast Blue B, in acidified propaaiol. The method is highly specific for 5-n-alkyl derivatives of resorcinols. In case of rye and wheat 98.1% and 96.2% respectively of total extinction value were due to 5-n-alkylresorcinols.

Determination of Biphenyl in Citrus Fruits by Thin Layer Chromatography and Ultraviolet Spectrophotometry

1967 ◽  
Vol 50 (4) ◽  
pp. 934-938
Author(s):  
Paul E Corneliussen
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Uv Light ◽  
Preparative Thin Layer Chromatography ◽  
Mean Deviation ◽  
Citrus Fruits ◽  
Ultraviolet Spectrophotometry ◽  
Spectrophotometric Measurement ◽  
Layer Chromatography

Abstract A rapid method for determining biphenyl in citrus fruits has been developed and was studied collaboratively. Biphenyl is separated from fruit tissue by steam liquidliquid extraction. The ra-heptane extract is subjected to preparative thin layer chromatography (TLC) on plates coated with silica gel containing phosphors for ready visibility of the biphenyl spots under UV light. The spots are removed from the plate and extracted with alcohol for spectrophotometric measurement at 248 mμ. The TLC cleanup adds specificity to the method; o-phenylphenol, if present, does not interfere and crop blanks are insignificant. The average of 36 recoveries (12 each at abovit 100, 50, and 10 ppm) was 96.7% with a mean deviation of 10.7%. It is recommended that the method be adopted as official, first action.

The synthesis, separation, and identification of the methyl ethers of arabinose and their derivatives

1967 ◽  
Vol 45 (3) ◽  
pp. 275-290 ◽  
Author(s):  
S. C. Williams ◽  
J. K. N. Jones
Keyword(s):  
Reducing Sugars ◽  
Reducing Sugar ◽  
The Other ◽  
Partition Chromatography ◽  
Ring Form ◽  
Optical Rotations ◽  
Layer Chromatography ◽  
Derivatives Of ◽  
Spray Reagents

A study has been made of various methods available for the identification and separation of the methyl ethers of arabinose. Gas–liquid partition chromatography has been used to separate the acetylated glycosides and the acetylated alditols of the methyl ethers of arabinose. All of the methyl ethers of arabinopyranose and arabinofuranose have been separated by paper chromatography. Several spray reagents have been used to distinguish between those methyl ethers with similar rates of movement. Thin-layer chromatography has been used to separate the methyl glycosides, acetylated methyl glycosides, and glycitols of the methyl ethers of arabinose, as well as the methyl ethers of the reducing sugar. The optical rotations of the reducing sugars and of the methyl glycosides of the methyl ethers of arabinose provide information about the ring form and, in the case of the glycosides, about the anomer present. The rotations of the acetylated and unacetylated O-methyl arabinitols aid in the determination of the position of the methyl substitutents. In connection with this study, all of the mono-O-methyl and tri-O-methyl, and most of the di-O-methyl ethers of arabinose have been synthesized. New syntheses have been devised for 4-O-methyl and 2,3-di-O-methyl arabinose, and the other sugars have been synthesized by known or partially revised syntheses. During this work, previously unreported derivatives of these sugars have been prepared.

Selective Determination of Pentafluorobenzyl Ester Derivatives of Carboxylic Acids by GC Using Microwave Plasma and Mass Selective Detection

1991 ◽  
Vol 45 (10) ◽  
pp. 1617-1620 ◽  
Author(s):  
Jeffrey H. Brill ◽  
Bikshandarkoil A. Narayanan ◽  
John P. McCormick
Keyword(s):  
Carboxylic Acids ◽  
Microwave Plasma ◽  
Selective Detection ◽  
Capillary Gc ◽  
Selective Determination ◽  
Fragmentation Behavior ◽  
Microwave Induced Plasma ◽  
Characteristic Fragmentation ◽  
Derivatives Of

A highly selective, sensitive method for determination of carboxylic acids in water has been developed that is based on fluorine-selective gas chromatography (GC) detection of pentafluorobenzyl ester derivatives. The atmospheric-pressure helium microwave-induced plasma detector is well suited for fluorine-specific detection of these derivatives, which were well resolved by capillary GC and displayed a characteristic fragmentation behavior when examined by GC-mass selective detection. For demonstration purposes, a number of carboxylic acids, ranging from C1 to C20, were examined and found to be derivatized with yields greater than 90%, and a sample of creek water was examined for its carboxylic acid content.

Determination of Oxidative Metabolites of Dimethoate and Thimet in Soil by Emission Spectroscopic Gas Chromatography

1966 ◽  
Vol 49 (3) ◽  
pp. 647-650
Author(s):  
C A Bache ◽  
D J Lisk
Keyword(s):  
Gas Chromatography ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Preparative Thin Layer Chromatography ◽  
Oxidation Products ◽  
Oxygen Analog ◽  
Oxidative Metabolites ◽  
Layer Chromatography

Abstract The conversion of dimethoate to its oxygen analog and the production of oxidative metabolites of Thimet in soil has been shown by using emission spectroscopic gas chromatography for their determination. Preparative thin layer chromatography was vised for prior separation of Thimet oxidation products. The sulfoxide and sulfone of Thimet were the major determinable products.

Determination of Matacil and Zectran by Fluorigenic Labeling, Thin Layer Chromatography, and In Situ Fluorimetry

1972 ◽  
Vol 55 (6) ◽  
pp. 1259-1264
Author(s):  
R W Frei ◽  
J F Lawrence
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Sulfonyl Chloride ◽  
Relative Standard ◽  
Dansyl Derivatives ◽  
Layer Chromatography ◽  
Derivatives Of ◽  
Fluorescent Derivatives

Abstract The fluorigenic labeling of Matacil (4-dimethylamino- m-tolyl N-methylcarbamate) and Zectran (4-dimethylamino-3,5-xylyl Wmethylcarbamate) with dansyl chloride (1-dimethylamino- naphthalene-5-sulfonyl chloride) results in 3 fluorescent derivatives, and labeling with NBD-Cl (4-chloro-7-nitrobenzo- 2,1,3-oxadiazole) produces 2 fluorescent derivatives for each carbamate, all of which can be separated by thin layer chromatography (TLC). These derivatives are identified by nuclear magnetic resonance, infrared, and fluorescence spectroscopy, aided by TLC data. The carbamates are hydrolyzed in dilute base and the resulting amine or phenol hydrolysis products react with the labeling reagents. The derivatives are analyzed by TLC and in situ fluorimetry with a spectrophotometer in the fluorescence mode and a spectrophotofluorometer with the thin layer scanning accessory. Reactions, fluorescence phenomena, and chromatographic properties of the derivatives are investigated for evaluation of the method as a quantitative technique. A reproducibility of 3–5% relative standard deviation can be expected in the concentration range from 15 to 300 ng/spot for derivatives of the 2 labeling procedures. The dansyl derivatives are instrumentally detectable as low as 1 ng/spot while the NBD derivatives may be detected at concentrations of less than 0.5 mg/spot.

Sign in / Sign up

Export Citation Format

Share Document