THE SEPARATION, DETERMINATION, AND CHARACTERIZATION OF 2-AMINO-2-DEOXY-D-GLUCOSE (D-GLUCOSAMINE) AND 2-AMINO-2-DEOXY-D-GALACTOSE (D-GALACTOSAMINE) IN BIOLOGICAL MATERIALS BY GAS–LIQUID PARTITION CHROMATOGRAPHY

1964 ◽  
Vol 42 (4) ◽  
pp. 451-460 ◽  
Author(s):  
M. B. Perry
Keyword(s):  
Hyaluronic Acid ◽  
Chondroitin Sulphate ◽  
Chromatographic Determination ◽  
Partition Chromatography ◽  
Quantitative Analyses ◽  
Optical Rotations ◽  
Trimethylsilyl Derivatives ◽  
Quantitative Procedure

A method for the separation, determination, and characterization of 2-amino-2-deoxy-D-glucose (D-glucosamine) and 2-amino-2-deoxy-D-galactose (D-galactosamine) is presented. Treatment of 2-acetamido-2-deoxy-α-D-glucose and 2-acetamido-2-deoxy-α-D-galactose in pyridine solution with trimethylchlorosilane and hexamethyldisilazane results in a rapid conversion of the glycoses to their respective trimethylsilyl 3,4,6-tri-O-trimethylsilyl-2-acetamido-2-deoxy-α-D-glycosides which are sufficiently stable and volatile to allow their separation and quantitative analysis to be made by gas–liquid partition chromatography. The two trimethylsilyl derivatives, collected by preparative gas–liquid partition chromatography, were crystalline compounds which had sharp melting points and characteristic infrared spectra and specific optical rotations. Quantitative analyses of mixtures of 2-amino-2-deoxy-D-glucose hydrochloride and 2-amino-2-deoxy-D-galactose hydrochloride were made by gas chromatographic analysis of their trimethylsilyl derivatives formed after prior conversion to their N-acetyl derivatives.The analytical procedure was applied to the characterization of 2-amino-2-deoxy-D-glucose in hyaluronic acid and 2-amino-2-deoxy-D-galactose in chondroitin sulphate. The quantitative procedure was also successfully applied to the analysis of mixtures of hyaluronic acid and chrondroitin sulphate by the gas–liquid partition chromatographic determination of the 2-amino-2-deoxy-D-glucose and 2-amino-2-deoxy-D-galactose in the hydrolyzates prepared from synthetic mixtures of the two mucopolysaccharides.

scholarly journals Gas-Chromatographic Determination of the Trimethylsilyl Derivatives of Polyhydric Alcohol Humectants in Tobacco and in Tobacco Smoke

1971 ◽  
Vol 6 (2) ◽  
Author(s):  
N. Carugno ◽  
S. Rossi ◽  
G. Lionetti
Keyword(s):  
Gas Chromatography ◽  
Mass Spectra ◽  
Triethylene Glycol ◽  
Chromatographic Determination ◽  
Flame Ionization ◽  
Trimethylsilyl Derivatives ◽  
Gas Chromatographic Method ◽  
Derivatives Of ◽  
Quantitative Procedure

AbstractA qualitative and quantitative procedure has been developed for the determination of humectants in manufactured tobacco by gas-chromatographic method with a flame ionization detector. It consists of extraction with methanol, concentration of the extract and treatment with Tri-Sil reagents. The operating gas-chromatographic conditions are set forth. Samples of tobacco containing glycerine, propylene glycol, diethylene glycol, triethylene glycol, 1-3 butylene glycol and sorbitol have been analysed with recoveries, for the first five ones, in the range of 95-104 %. In order to verify that each chromatographic peak corresponded to the relative glycol, with no interference by other silylated compounds, the mass spectra were obtained through the combination of gas-chromatography with mass spectrometry. The results achieved confirm, as far as tobacco is concerned, that the procedure is accurate and precise. The same method for the determination of humectants was extended to cigarette smoke. Even though this involves morecomplicated problems, as compared to tobacco, because of the presence of silylated compounds, it was found that, for certain glycols, the gas-chromatography of the trimethyl derivatives can be also used as a method of analysis. The mass spectra of some polyhydric alcohols are shown

Novel Cleanup Method for Quantitative Gas Chromatographic Determination of Trace Amounts of Di-2-Ethylhexyl Phthalate in Fish Lipid

1981 ◽  
Vol 64 (2) ◽  
pp. 282-286 ◽  
Author(s):  
B Garth Burns ◽  
Charles J Musial ◽  
John F Uthe
Keyword(s):  
Gel Permeation Chromatography ◽  
Chromatographic Determination ◽  
Confirmatory Test ◽  
Fish Lipid ◽  
Gel Permeation ◽  
Fish Lipids ◽  
Cleanup Procedure ◽  
Quantitative Analyses ◽  
Ethylhexyl Phthalate

Abstract A new, simple, and rapid cleanup procedure is described for di-2-ethylhexyl phthalate (DEHP) residues in fish lipids. Extracts are chromatographed on small alumina:sulfuric acid-impregnated alumina (layered) columns after gel permeation chromatography of the fish lipid extracts on BioBeads SX-3. Quantitative analyses were carried out by electron capture gas chromatography using 2 columns. Spiked DEHP recoveries varied from 79.3% in mackerel to 86.1% in herring. DEHP concentrations were determined in plaice, eel, redfish, herring, cod, and mackerel tissues and ranged from trace (<0.001 µ/g) to approximately 10 µ/g (wet wt basis). Ethanolic KOH saponification of the purified DEHP fraction, resulting in the disappearance of the DEHP peak, was used as a confirmatory test. Limited studies with dibutyl, di-n-heptyl, and diethyl phthalates suggest that the method can be made more versatile.

Column Chromatographic Determination of Certifiable Colors in Lipsticks

1963 ◽  
Vol 46 (6) ◽  
pp. 1013-1017
Author(s):  
Rachel Sclar Silk
Keyword(s):  
Binary Mixture ◽  
Ammonium Hydroxide ◽  
Chromatographic Determination ◽  
Aqueous Alcohol ◽  
Partition Chromatography ◽  
Immobile Phase ◽  
Column Chromatographic

Abstract Column partition chromatography on Celite is used to separate the colors present in lipsticks. In the proposed procedure the immobile phase is aqueous alcohol plus ammonium hydroxide. A small portion of lipstick is ground with a portion of Celite containing the aqueous immobile phase and packed on top of a prepared colrate umn. Solvents of increasing polarity are used to elute individual colors except for one binary mixture. D&C Red No. 19 and D&C Red No. 36 and/or D&C Orange No. 17 elute together.

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.

Characterization of Packing Columns For the Liquid Chromatographic Determination of Corticosteroids in Human Plasma

1986 ◽  
Vol 9 (12) ◽  
pp. 2601-2608 ◽  
Author(s):  
Tatsuhiko Ando ◽  
Shinri Koshika ◽  
Kazutaka Komura ◽  
Yoshiyuki Nakayama ◽  
Shoji Hara
Keyword(s):  
Human Plasma ◽  
Chromatographic Determination ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic
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