Search results for "Derivatization"
showing 10 items of 215 documents
A denuder-impinger system with in situ derivatization followed by gas chromatography-mass spectrometry for the determination of gaseous iodine-contai…
2008
Reactive iodine species have been suggested to play an important role in the atmosphere (e.g. tropospheric ozone depletion, coastal new particle formation). However, there still exist major uncertainties about their atmospheric chemistry, mostly due to the lack of analytical approaches for the accurate speciation of certain key compounds. In this study, 1,3,5-trimethoxybenzene (1,3,5-TMB)-coated denuder proved to be suitable for the differentiation between gaseous interhalogens (iodine monochloride (ICl), iodine monobromide (IBr)) and molecular iodine (I2) based on a selective collection/derivatization method. The results of the denuder sampling were compared with the results of impinger sa…
Application of the 6-aminoquinolyl-N-hydroxysccinimidyl carbamate (AQC) reagent to the RP-HPLC determination of amino acids in infant foods.
2005
The validation of a pre-column derivatization procedure with 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate (AQC) to the determination of the amino acid content by RP-HPLC with fluorescence detection (lambda excitation 250 nm, lambda emission 395 nm) in milk-cereal based infant foods was carried out. The analytical parameters: linearity (0.0025-0.2mM), precision of the method (0.2-3.5% variation coefficients), accuracy (derivatization: 86-106% average recovery and method: 88.3-118.2% average recovery) and the limits of detection (0.016-0.367 microM) and quantification (0.044-1.073 microM) were determined. Glutamic acid, proline and leucine were the most abundant amino acid whereas the lowe…
Highly efficient separation of amines by electrokinetic chromatography using resorcarene-octacarboxylic acids as pseudo-stationary phases
1998
Abstract Resorcarene-octacarboxylic acids, macrocyclic molecules built up by four alkylidene-bridged resorcinol units, were synthesized and used as pseudostationary phases in electrokinetic chromatography (EKC). Resorcarenes provide a stable structure and good solubility in electrolytes even with organic modifiers. The high electrophoretic mobility of the resorcarene-octacarboxylic acids introduced here as pseudostationary phases is based on the eight partly deprotonated carboxylic groups. This offers a broad migration time window, which is the main parameter for the resolution of peaks. From three compounds with different alkyl chain lengths (C 1 , C 5 , C 11 ), the C 11 -resorcarene-octa-…
Solid-Phase Extraction and Clean-Up Procedures in Pharmaceutical Analysis
2012
Solid-phase extraction (SPE) using small cartridges filled with sorbents of a small particle size has rapidly established itself as an important sample clean-up technique. It has prospered at the expense of liquid-liquid extraction (LLE), which is considered labor intensive and frequently plagued by problems, such as emulsion formation and use of large volumes of hazardous solvents. A remarkable characteristic of SPE is its easy adaptation to on-line mode by column-switching techniques; switching can be effected manually or by automated controllers. The same analyte/sorbent interactions that are exploited in liquid chromatography (LC) are of use in SPE, but particle sizes employed are great…
HPLC: a tool for the analysis of T-2 toxin and HT-2 toxin in cereals.
1984
An analytical procedure for the determination of trichothecenes in various cereals is described. HPLC was performed with a reversed-phase (C18) column eluted with methanol:water (60:40, v/v). Compounds were detected with a refractive index detector. The elution patterns of free and contaminated samples were compared. The recovery of added T-2 toxin (2 and 5 micrograms/g) in rye and wheat was approximately 80%. The application of this method allows for combined use with other sensitive methods such as mass spectrometry and gas chromatography. The described method is operationally simple, relatively inexpensive, and requires no derivatization.
Chiral determination of amphetamine and related compounds using chloroformates for derivatization and high-performance liquid chromatography
1999
The enantiomeric determination of amphetamine and various amphetamine-type compounds by liquid chromatography after chiral derivatization with 9-fluorenylmethyl chloroformate-L-proline (FMOC-L-Pro) is reported. The results obtained were compared with those achieved after achiral derivatization with 9-fluorenylmethyl chloroformate and subsequent separation of the derivatives on a beta-cyclodextrin chiral stationary phase. Conditions for the derivatization of amphetamines with FMOC-L-Pro were investigated, including the effect of the derivatization reagent concentration, pH and reaction time, using amphetamine, ephedrine and pseudoephedrine as model compounds. On the basis of these studies, p…
Photochemical Derivatization and Fluorimetric Determination of Promethazine in a FIA Assembly
1992
Abstract The flow injection fluorimetric determination of promethazine is carried out by on-line photoderivatization. The PTFE tubing is helically coiled around the lamp. An analytical procedure is proposed by using aqueous solution as carrier stream: the calibration graph is linear over the range 0.05 - 20 ppm. The influence of foreign compounds is studied and the method is applied to promethazine determination in pharmaceutical formulations.
Characterization of bile acids and fatty acids from ox bile in oil paintings by gas chromatography?mass spectrometry*1
2004
Characterization of ox bile, traditionally used in painting, is of interest in the fields of archaeometry and conservation and restoration of works of art. Bile acids, fatty acids (F), and cholesterol found in ox bile have been identified using a derivatization method that combines the formation of ethyl esters from the carboxylic groups and the trimethylsilyl ethers from hydroxyl groups. This method of analysis is consistent with these others proposed by the authors to analyze drying oils, proteins, and diterpenic resins usually used as binders and varnishes by the painters. Bile acids from binary samples such as animal glue/ox bile, casein/ox bile and Arabic gum/ox bile have been successf…
On the Derivatization of Drugs Using 1-Nitroso-2-naphthol, 4-aminoantipyrine and 2,6-Dihaloquinone Chlorimides
1992
Coupling of 1-nitroso-2-naphthol (1N2N), 4-aminoantipyrine (4-AAP), 2,6-dichloroquinone chlorimide (DCQC) and 2,6-dibromoquinone chlorimide (DBQC) with several bioactive substances, including adren...
Simple high-performance liquid chromatographic assay for polyamines and their monoacetyl derivatives.
1993
A rapid reversed-phase high-performance liquid chromatographic method, using pre-column derivatization with benzoyl chloride and ultraviolet detection at 254 nm, was developed for the simultaneous measurement of polyamines and their monoacetyl derivatives. Calibration curves were linear for concentrations from 1.25 to 25 nmol/ml. The method was employed to assay these compounds in chick embryo retina explants using organic solvent extraction and 1,7-diaminoheptane as an internal standard. This simple and sensitive method can be applied to routine determinations of these compounds in various biological samples.