Search results for "Derivatization"
showing 10 items of 215 documents
Influence of the presence of surfactants and humic acid in waters on the indophenol-type reaction method for ammonium determination.
2005
Abstract This work has evaluated the influence of humic acid and/or surfactants in the quantification of ammonium in waters with the indophenol-type reaction method. Thymol has been employed with the colorimetric method for sample ammonium concentrations between 0.25 and 1 mg L −1 . In addition, SPE/diffuse reflectance method has been used for quantification of ammonium at low concentrations (between 0.025 and 0.25 mg L −1 ). Matrix effect owing to humic substances were observed with the colorimetric method when the concentration was equal or higher than 25 mg L −1 . Lower concentrations of humic compounds produced matrix effects with the more sensitive SPE/diffuse reflectance method. Gener…
Chromatographic Determination of Thiols After Pre‐column Derivatization witho‐Phthalaldehyde and Isoleucine
2004
Abstract The reaction of primary amines with excess o‐phthalaldehyde (OPA) and thiol yields unique isoindole derivatives that are readily separated by reversed‐phase liquid chromatography. In a previous work, a spectrophotometric procedure was proposed for the assay of N‐acetylcysteine by derivatization with OPA and isoleucine at pH 9.5, with satisfactory results. The chromatographic determination of this and other low molecular‐weight thiols, after isoindole formation with isoleucine, using mobile phases of acetonitrile–water at pH 3 and spectrophotometric detection, is now examined. From the assayed thiols (thioglycolic acid, 3‐mercaptopropionic acid, tiopronin, N‐acetylcysteine, N‐acetyl…
Chromatographic quantitation of the hydrophobicity of ionic compounds by the use of micellar mobile phases
1998
Abstract Many biologically active compounds of interest in structure–activity relationships are ionic at physiological pH. However, ionic organic compounds are only weakly or not retained in conventional RPLC which impedes the chromatographic estimation of their hydrophobicity and the development of quantitative retention–activity relationship studies. The use of micellar mobile phases allows the retention of ionic compounds. Hydrophobic and electrostatic forces govern the retention of ionic compounds in micellar liquid chromatography. In this paper three different retention models log k–log P for ionic compounds are tested (P=partition coefficient). The retention model (log k=a log P+bα+c)…
Single-pump bi-dimensional LC applied to the characterization of derivatized fatty alcohol ethoxylates.
2010
A column selection valve and a 6-port 2-position injection valve were combined to implement bi-dimensional LC in a system driven by a single pump. The system was applied to the separation of linear fatty alcohol ethoxylates with 12-18 carbon atoms in the hydrocarbon moiety, previous derivatization with diphenic anhydride. Separation on the first separation dimension (C(1)) was carried out with a propyl-diol column and an acetonitrile/aqueous ammonium acetate gradient. Fatty alcohol ethoxylate hydrocarbon series (oligomers with the same number of carbon atoms in the alkyl chain but differing in the number of ethylene oxide units) were resolved without distinguishing the oligomers within the …
Biocompatible polymeric micelles with polysorbate 80 for use in brain targeting.
2008
In this paper, the synthesis and characterization of novel amphiphilic graft copolymers based on an alpha,beta-poly(N-2-hydroxyethyl)-D, L-aspartamide (PHEA) backbone and D, L-polylactic acid (PLA) hydrophobic side chains are reported. These copolymers were obtained starting from PHEA-ethylenediamine (PHEA-EDA), which was functionalized with polysorbate 80 (PS(80)) and/or PLA in order to obtain the PHEA-EDA-PS(80)-PLA and PHEA-EDA-PLA samples, respectively. The degrees of derivatization, DD(PS80) and DD(PLA), of PHEA-EDA-PS80-PLA, calculated by (1)H-NMR, resulted in being 1.2 +/- 0.03 mol% and 0.54 +/- 0.05 mol%, respectively, while that of PHEA-EDA-PLA was found to be 0.60 +/- 0.05 mol%. S…
Separation of Proteic Primary Amino Acids under Several Reversed‐Phase Liquid Chromatographic Conditions
2006
Abstract The reversed‐phase liquid chromatographic (RPLC) analysis of proteic primary amino acids with acetonitrile‐water, using pre‐column derivatisation with o‐phthalaldehyde (OPA) and N‐acetylcysteine (NAC), was compared with RPLC modes using trifluoroacetic acid or pentadecafluorooctanoic acid and evaporative light‐scattering detection, or sodium dodecyl sulphate micelles with pre‐ and post‐column derivatisation. The importance of column lifetime, risk of potential damages in the instrumentation, retention and resolution, was considered. Among the assayed approaches, the best is still aqueous‐organic RPLC with pre‐column derivatisation. It not only yields the most reliable results, but …
Enzyme class identification in cleaning products by hydrolysis followed by derivatization with o-phthaldialdehyde, HPLC and linear discriminant analy…
2008
The enzymes present in raw materials of the cleaning industry (enzyme industrial concentrates) and in household cleaners were isolated by precipitation with acetone and hydrolyzed with HCl. The resulting amino acids were derivatized with o-phthaldialdehyde, and the derivatives were separated by HPLC. The peaks of 14 amino acids were observed using a C18 column and a multi-segmented gradient of acetonitrile-water in the presence of a 5 mM citric/citrate buffer of pH 6.5. Using either normalized peak areas (divided by the sum of the peak areas of the chromatogram) or ratios of pairs of peak areas as predictor variables, linear discriminant analysis models, capable of predicting the enzyme cla…
Method for determination of formaldehyde in air in the pptv-range by HPLC after extraction as 2,4-dinitrophenyl-hydrazone
1982
The derivatization of formaldehyde with 2,4-dinitrophenylhydrazine and the extraction of the product formalhydrazone is studied. The determination is carried out by HPLC. Applying a cryogenic sampling technique and a sampling volume of 300l of air the detection limit of formaldehyde in air is 30 pptv and this is suitable for measurements of formaldehyde in the atmosphere. (IFU)
Characterization of proteinaceous glues in old paintings by separation of the o-phtalaldehyde derivatives of their amino acids by liquid chromatograp…
2005
A HPLC-fluorescence method for characterization of proteinaceous glues from binding media used in pictorial works of art prior to conservation or restoration treatment is proposed. Fluorescence derivatization of amino acids released by acid hydrolysis of standard proteins is studied. The derivatization reagent was o-phtalaldehyde with 2-mercaptoethanol as catalyst. Mobile phase was a programmed gradient among two eluents (water buffered at pH 5.8 wit 5% THF, and methanol) and is able to satisfactorily resolve the amino acid derivatives in 45min. Peak area ratios among amino acid derivatives and the leucine derivative are useful to characterize the proteins. The method shows good sensitivity…
Infusion mass spectrometry as a fingerprint to characterize varnishes in oil pictorial artworks.
2007
Mass spectrometry methodology to characterize drying oil used as binding media and varnishes in pictorial artworks, prior to conservation or restoration treatment, is proposed. The analytical treatment requires prior basic hydrolysis of the samples to release the fatty acids : caprylic, pelargonic, capric, sebacic, azelaic, suberic, eicosanoic, lauric, mirystic, palmitic, linolenic, linoleic, oleic and stearic, followed by separation from the matrix by a hexane/water extraction. After removing the solvent, the remaining solid is dissolved in potassium hydroxide, propanol and methanol. The mixture is directly infused into a mass spectrometer without any previous derivatization or separation …