Gas-chromatographic determination of acetyl and trimethylsilyl derivatives of alkyl carbamates and their N-hydroxy derivatives

The Analyst ◽  
1969 ◽  
Vol 94 (1115) ◽  
pp. 130 ◽  
Author(s):  
R. Nery
Keyword(s):  
Chromatographic Determination ◽  
Trimethylsilyl Derivatives ◽  
Derivatives Of

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

Liquid Chromatographic Determination of Primary and Secondary Amines as 8-Quinolinesulfonyl Chloride Derivatives

1984 ◽  
Vol 67 (4) ◽  
pp. 687-691
Author(s):  
F Taylor Noggle ◽  
C Randall Clark
Keyword(s):  
Chromatographic Determination ◽  
Secondary Amines ◽  
Absorption Bands ◽  
Reverse Phase ◽  
Primary And Secondary Amines ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Liquid Chromatographic ◽  
Derivatives Of

Abstract The normal phase and reverse phase liquid chromatographic properties of seven 8-quinolinesulfonyl derivatives of primary and secondary amines are examined using dual wavelength ultraviolet detection. The amines are further identified by infrared spectrophotometry with emphasis on structural elucidation based on absorption bands at characteristic wavelengths.

Gas-chromatographic determination of nanogram amounts of enantiomers of nortilidine, a main metabolite of tilidine, in biological specimens.

1978 ◽  
Vol 24 (4) ◽  
pp. 692-697 ◽  
Author(s):  
H Hengy ◽  
K O Vollmer ◽  
V Gladigau
Keyword(s):  
Intravenous Administration ◽  
Chromatographic Determination ◽  
Optical Isomers ◽  
Sensitive Detector ◽  
Main Metabolite ◽  
Chiral Reagent ◽  
The Individual ◽  
Derivatives Of ◽  
Sensitive Method

Abstract We report a specific and sensitive method for determination of the individual optical isomers of nortilidine, a main metabolite of tilidine, with the aid of a nitrogen-sensitive detector. With N-trifluoroacetyl-L-leucyl chloride as chiral reagent, the diastereomeric derivatives of the nortilidine enantiomers could be separated and quantified in the nanogram range. Under these conditions, the enantiomers of bisnortilidine, another main metabolite of tilidine, were also separated. Investigations in rats with the enantiomers of tilidine and nortilidine indicated that no racemization occurs during N-demethylation in the organism. After oral and intravenous administration of 50 mg of tilidine.HCI to a human volunteer, identical concentrations of nortilidine enantiomers were found in the plasma.

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.

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