Search results for "Derivatization"

Photo-induced fluorescence of magnesium derivatives of tetracycline antibiotics in wastewater samples

2009

Abstract An analytical strategy, for the determination of tetracyclines (TCs), based on a HPLC system coupled with a photo-reactor followed by post-column derivatization was developed. Higher fluorescence emission after coupling the resulting photo-fragments with magnesium ions was observed for the determination of minocycline (MC), epitetracycline (ETC), tetracycline (TC) and doxycycline (DC). The manifold included a HPLC system with a photo-reactor (PTFE tubing helically coiled around a low-pressure mercury lamp), a mixing T-piece and a fluorescence detector. The derivatization reagent was delivered at 0.5 mL min −1 by a pump. After HPLC separation using a gradient system with a mobile ph…

2018

Reactivity is an important parameter when considering the chemical modification or dissolution of cellulose. Different pretreatment methods affect cellulose reactivity by decreasing its degree of polymerization (DP) and crystallinity. In this study, the molar mass of cellulose was decreased via enzymatic pretreatment. Three commercial endoglucanase-rich products were tested. The target was to reduce the viscosity of the pulp to below 200 mL/g and, thus, increase the reactivity of the cellulose. For comparison, cellulose was also pretreated with ozone, and the effects of each pretreatment method on crystallinity and monosaccharide composition of the resulting pulps were investigated. Both en…

Analysis of Trace Pharmaceuticals and Related Compounds in Municipal Wastewaters by Preconcentration, Chromatography, Derivatization, and Separation …

2014

A significant portion of pharmaceuticals and other organic chemicals consumed by people and animals are released into municipal wastewater treatment plants. Most of them are degraded during the wastewater treatment processes, but some of them degrade only partially and may be widely transported and dispersed into the aquatic environment. This is why efficient and fast analytical methods are needed for detection of organic compounds in wastewaters at trace levels. Because wastewaters often consist of complex matrices and high-molecular mass materials, e.g., lignocellulosic biomass, which may bring challenges to the sample preparation procedures, efficient pre-concentration methods such as so…

Derivatization of ephedrine with o-phthaldialdehyde for liquid chromatography after treatment with sodium hypochlorite.

2000

The usefulness of the reaction with NaClO followed by derivatization with o-phthaldialdehyde (OPA) and N-acetyl-L-cysteine (NAC) has been investigated for the chromatographic analysis of ephedrine. The influence of parameters affecting the two-stage reaction has been evaluated, including concentration of NaClO, time of reaction, temperature and pH. On the basis of these studies, conditions for the pre-column and (automated) post-column determination of ephedrine are presented. The described conditions have been applied to the measurement of ephedrine in the concentration intervals 0.2-20.0 microg/ml and 2.0-50.0 microg/ml for the pre-column and post-column methods, respectively. The possibi…

Microwave-assisted synthesis of PHEA-oligoamine copolymers as potential gene delivery systems

2009

Aims - Copolymers bearing oligoamines and having buffering capacity in the endosomal pH range seems very promising as non viral vectors in gene delivery, due to the great importance of endosomal escaping for an efficient endocellular DNA release. Aim of this paper was to prepare new copolymers based on α,β-poly-(N-2-hydroxyethyl)-D,L-aspartamide (PHEA) as polymeric backbone and bearing an oligoamine, such as diethylentriamine (DETA) in the side chain and useful for gene delivery. Moreover in order to reduce solvent volume and to make faster the reaction, microwave-assisted has been used. Materials and methods - PHEA copolymers bearing different amount of DETA were prepared by using bis(4-ni…

Micellar electrokinetic chromatography of polyamines and monoacetylpolyamines

2001

A selective procedure for qualitative and quantitative analysis of ten polyamines by micellar electrokinetic chromatography (MEKC) was developed. Benzoylated polyamines and acetylpolyamines in micellar phase of SDS (10 mM) were separated at 25 degrees C by 20 mM borate buffer pH 8.5, containing 8% ethanol, with an applied voltage of 25 kV (5 microA) and then detected at 198 nm. The experimental factors and operational parameters were optimized by performing analysis at different surfactant concentrations, pH, voltage and temperature with and without ethanol. The repeatibility of migration times and peak heights is a peculiarity of the method here described.

Determination of N-acetyl-l-glutamine in urine by HPLC

1986

The determination of N-acetyl-l-glutamine (AC-GLN) in urine of rats after derivatization with xanthydrol by HPLC is described. The urine samples were collected from two groups of rats, one group fed normal nutrition, the other treated with AC-GLN. About 5 mM/l AC-GLN was detected in urine of untreated animals, whereas the excretion of the other group was in the range of 50 mM/l corresponding to about 50 wt.-% of the given AC-GLN.

An evaluation of solid phase microextraction for aliphatic amines using derivatization with 9-fluorenylmethyl chloroformate and liquid chromatography

2005

The reliability of SPME combined with a chemical reaction for the analysis of short-chain aliphatic amines by liquid chromatography has been investigated. Different options to couple SPME and derivatization have been tested and compared: (i) derivatization of the analytes in solution followed by the extraction of the derivatives, (ii) extraction of the analytes and subsequent derivatization by immersing the SPME fibre onto a solution of the reagent, and (iii) extraction/derivatization of the analytes using fibres previously coated with the reagent. Methylamine (MA), dimethylamine (DMA) and trimethylamine (TMA) have been selected as a model of primary, secondary and tertiary amines, respecti…

Derivatization of hydroxyl functional groups for liquid chromatography and capillary electroseparation

2013

The derivatization reactions commonly used to enhance the analytical signal in the HPLC and CE determination of compounds with hydroxyl functional groups are revised. Focus is placed on the determination of compounds having aliphatic alcohols and phenols while lacking other reactive functional groups. The derivatization with acyl chlorides, organic anhydrides, isocyanates and a variety of other approaches, including oxidation of primary and secondary alcohols, sulfonation, esterification with carboxylic acids, and the use of azides, sulfonyl chlorides and other reagents having miscellaneous leaving groups, is covered. Reactions mainly addressed to introduce a chromophore or a fluorophore in…

Liquid chromatographic determination of toxigenic secondary metabolites produced by Fusarium strains.

2002

Various liquid chromatographic methods used in the analysis of mycotoxins (zearalenone, trichothecenes and fumonisins) produced by Fusarium species were compared in this work. The results demonstrate the suitability of modern clean-up procedures employing multifunctional MycoSep and immunoaffinity columns although these methods are more expensive than conventional methodologies for clean-up. HPLC with both fluorescence and photodiode array detection is a suitable technique for the analysis of toxic secondary metabolites produced by Fusarium species; different derivatisation strategies have been studied to improve the sensitivity of the technique because of the low concentration of these met…