Search results for "Derivatization"

Asymmetrically substituted calix[4]arenes; A two-dimensional 1H NMR study of a tetraester derivative in the cone-conformation

1991

Abstract Several new chiral calix[4]arenes with three or four different substituents in the p-position have been prepared by fragment condensation. Standard derivatization procedures always led to the formation of mixtures of various conformational isomers from which the derivative in the cone-conformation could be isolated only by preparative HPLC. For a tetraester derivative it was shown by two-dimensional 1H NMR spectroscopy, that due to the different substituents the cone-conformation is strongly distorted. The sodium complex of this tetraester, however, assumes a regular cone-conformation again.

Reliable and simple analytical methods for determination of citrulline and metabolically related amino acids by liquid chromatography after derivatiz…

2014

We describe the development of a high-performance liquid chromatography (HPLC) method for the determination of citrulline and other amino acids relevant to intestinal diseases. The amino acids were derivatized with 9-fluorenylmethylchloroformate (FMOC-Cl) and their derivatives were separated on two different columns, a core-shell column (Halo C18) and a silica-based monolith (Chromolith Performance RP-18). The derivatization reaction was optimized with respect to pH, buffer concentration and reproducibility. The optimal derivatization conditions were achieved with 0.4 M borate buffer at pH 9.20, a constant ratio of FMOC-Cl/total amino acids (10 : 1) and 75 mM tyramine after 1 min (quenching…

ChemInform Abstract: A New Route to Chiral Calix(4)arenes via 1,3-Derivatization.

2010

New Glass Capillary Gas-Chromatographic Methods for Metabolites in Urine and Serum

1981

The analytical system suggested in this paper is a further development of pre-chromatographic methods and of column switching techniques described in previous papers1,2,3.In order to use modern gas-chromatographic techniques for the determination of metabolites in urine and serum quick and reliable pre-chromatographic methods for extraction, concentration and derivatization must be developed which give final (dosage) volumes of 5 to 10 μl with starting sample volumes of 0.1 ml of urine or 5 ml of serum as described by Dunges4.

Validation of Methylmercury Determinations in Aquatic Systems by Alkyl Derivatization Methods for GC Analysis Using ICP-IDMS

2001

Isotope dilution mass spectrometry (IDMS), using an inductively coupled plasma quadrupole mass spectrometer (ICPMS) and a species-specific methylmercury spike was applied to validate the commonly used GC method for methylmercury (MeHg+) determination, which is based on the formation of volatile methylethylmercury by derivatization with NaBEt4. The spike compound, Me201Hg+, was synthesized by reaction of 201Hg-enriched mercury chloride with methylcobalamin. By analyzing different environmental aquatic samples, it was found that in most cases, transformation of MeHg+ into elemental mercury (Hg0) took place. From investigations of synthetic solutions, it could be followed that halide ions are …

Amphetamine and Methamphetamine Determinations in Biological Samples by High Performance Liquid Chromatography. A Review

1994

Abstract This critical review shows the different high performance liquid chromatography methods proposed for amphetamine and methamphetamine determinations. It is directed mainly towards sample clean up and derivatizations steps, because of their significance in such determinations.

Comparative assessment of solid-phase extraction clean-up procedures, GC columns and perfluoroacylation reagents for determination of type B trichoth…

2005

Abstract Various solid-phase extraction (SPE) procedures for clean-up, two perfluoroacylation reagents (pentafluoropropionic anhydride (PFPA) and heptafluorobutyric anhydride (HFBA)) and two chromatographic columns (HP-1701 and HP-5) have been assessed comparatively to achieve the determination of type B trichothecenes (deoxynivalenol (DON), nivalenol (NIV), 3- and 15-acetyldeoxynivalenol (3- and 15-ADON)) in wheat grain by gas chromatography (GC)–electron-capture detection (ECD). Spiked wheat samples were extracted with acetonitrile–water (84:16, v/v). Tested SPE procedures were MycoSep 225 column, Florisil and different cartridges prepared in the laboratory with mixtures of various sorben…

Identification of drying oils used in pictorial works of art by liquid chromatography of the 2-nitrophenylhydrazides derivatives of fatty acids.

2004

A new HPLC-UV-Vis method for identification of drying oils from binding media or protective film used in pictorial works of art prior to conservation or restoration is proposed. Chromophore derivatization of fatty acids released by hydrolysis of structural drying oils is studied. The derivatization reagent selected was 2-nitrophenylhydrazine with 1-ethyl-3-(3-dimethyl animopropyl)carbodiimide hydrochloride/pyridine as catalyst. This reaction was carried out using microwave heating. Mobile phase was methanol/water/n-propanol/acetic acid (80:14:5:1) running in isocratic mode. Absorbance was measured at 400nm. In these conditions, hydrazides of myristic, palmitic, oleic, and stearic acids were…

Rapid fluorimetric assay for primary amine groups in water samples

2003

Bond Elut C(18) solid-phase extraction cartridges were used for pre-concentration followed by derivatization with o-phthaldialdehyde-N-acetylcysteine (OPA-NAC) of primary amines in water. Optimal conditions were: conditioning the cartridges with borate buffer pH 10.4, retention of the primary amines, addition of the OPA-NAC(3.7 mmol L(-1)) 1:1 molar ratio and borate buffer pH 8, elution of the isoindol with MeOH-borate buffer (9:1) pH 10.2 and fluorescence measurement. The equations of the calibration graphs for methylamine, ethylamine, propylamine, butylamine, pentylamine, and beta-phenylethylamine at lambda(excitation)=330 nm and lambda(emission)=440 nm, in the optimal conditions are pres…

HPLC Method for Cyst(e)ine and Methionine in Infant Formulas

1996

Cyst(e)ine and methionine were converted into cysteic acid and methionine sulfone by oxidizing with performic acid. The oxidized samples were then subjected to acid hydrolysis (6N HCl, 105-110°C/24 hr). After derivatization with phenylisothiocyanate, reverse phase HPLC separation was carried out at 48°C and with UV detection. Different gradients and pH values in the eluent were assayed to determine the best resolution. Analytical parameters, detection and quantification limits, linearity, precision and accuracy, were determined. The method was reliable and accurate for measuring cyst(e)ine and methionine in infant formulae.