Search results for "SOLID-PHASE"
showing 10 items of 178 documents
A Classical Synthesis of the Collagen-like Peptides with the Sequence Z(GlyProPro)nOBut and their characterization with circular dichroism and ultrac…
1975
Oligopeptides with the sequence Z(GlyProPro)nOBut (n = 3–7) were synthesized along a clasical pathway. Generally long fragments were condensed in order to allow an easy separation of the products from the reactants. It is established by molecular weight determination and measurements of circular dichroism that the peptides form the collagen-like triple helix in methanol and that they assume the random coil conformation in dilute acetic acid. The circular dichroism spectra agree reasonably well with the corresponding spectra for (ProProGly)10 which was obtained by solid phase synthesis in another laboratory.
In situ generation of Co(II) by use of a solid-phase reactor in an FIA assembly for the spectrophotometric determination of penicillamine
2005
[EN] A flow injection analysis (FIA) manifold for the determination of penicillamine in pharmaceutical preparations is proposed. The manifold includes a solid-phase reactor for the in situ production of the derivatizing reagent, Co(II) ion, which forms a coloured complex with penicillamine in an alkaline medium. The reactor is prepared by natural immobilization of cobalt carbonate on a polymer matrix, which endows it with a high mechanical and microbiological stability. The cobalt released by passage of a 5 x 10(-4) Mol l(-1) sulphuric acid stream at a flow-rate of 2.3 ml min(-1) is merged with a volume of 314 mu l of sample containing penicillamine in ammonium-ammonia buffer at pH 9.5 to m…
Miniaturized solid-phase extraction techniques
2015
More than 80% of analysis time is spent on sample collection and sample preparation, so sample preparation is a critical part of the analytical process. Traditionally, liquid-liquid extraction was developed and employed to screen for general unknowns. However, solid-phase extraction (SPE) is becoming highly popular as an alternative, due to its simplicity and economy in terms of time and solvent. This review summarizes the current state of the art and the future prospects for green analytical chemistry with special emphasis on environment-friendly sample-preparation techniques based on the solid phase. We discuss in detail miniaturized SPE techniques, based on the most relevant, most repres…
Sample Preparation to Determine Pharmaceutical and Personal Care Products in an All-Water Matrix: Solid Phase Extraction
2020
© 2020 by the authors.
On-line analysis of carbonyl compounds with derivatization in aqueous extracts of atmospheric particulate PM10 by in-tube solid-phase microextraction…
2011
Abstract A new device for carbonyl compounds based on coupling on-line and miniaturizing both, sample pretreatment and chromatographic separation, is reported. Two capillary columns, a GC capillary column (95% methyl–5% phenyl substituted backbone, 70 cm × 0.32 mm i.d., 3 μm film thickness) in the injection valve for in-tube solid-phase microextraction (IT-SPME) and a Zorbax SB C18 (150 mm × 0.5 mm i.d., 5 μm particle diameter) LC capillary column were employed. Different combinations of IT-SPME and derivatization using 2,4-dinitrophenylhydrazine (DNPH) were examined for mixtures containing 15 carbonyl compounds (aliphatic, aromatic and unsaturated aldehydes and ketones). A screening analys…
Analysis of methylamine by solid-phase microextraction and HPLC after on-fibre derivatization with 9-fluorenylmethyl chloroformate
2004
Abstract A method for the determination of methylamine (MA) in aqueous matrices is reported which uses solid-phase microextraction (SPME) for enrichment and derivatization of the analyte, and high performance liquid chromatography (HPLC). The fluorogenic reagent 9-fluorenylmethyl chloroformate (FMOC) has been used for derivatization. The SPME fibres were successively immersed in the samples and in the derivatization solutions to extract MA and FMOC, respectively. After a defined time of reaction, the derivatized analyte was desorbed into the chromatographic system, and chromatographed in a LiChrosphere 100 RP18, 125 mm ×4 mm i.d., 5 μm, column under gradient elution. In order to improve the…
Recent developments and future trends in solid phase microextraction techniques towards green analytical chemistry.
2013
Solid phase microextraction find increasing applications in the sample preparation step before chromatographic determination of analytes in samples with a complex composition. These techniques allow for integrating several operations, such as sample collection, extraction, analyte enrichment above the detection limit of a given measuring instrument and the isolation of analytes from sample matrix. In this work the information about novel methodological and instrumental solutions in relation to different variants of solid phase extraction techniques, solid-phase microextraction (SPME), stir bar sorptive extraction (SBSE) and magnetic solid phase extraction (MSPE) is presented, including prac…
New micromethod combining miniaturized matrix solid-phase dispersion and in-tube in-valve solid-phase microextraction for estimating polycyclic aroma…
2008
Abstract Miniaturized matrix solid-phase dispersion (MSPD) was developed for the extraction of common polycyclic aromatic hydrocarbons (PAHs) from bivalve samples (100 mg, dry weight). Additional clean-up and analyte enrichment was accomplished by in-tube solid-phase microextraction (SPME). For this purpose the extracts collected after MSPD were diluted with water and injected into a capillary column coated with the extractive phase. This capillary column was connected to the analytical column by means of a switching valve. Separation and quantification of the PAHs were carried out using a monolithic LC column and fluorescence detection. Since the in-tube SPME device allowed the processing …
Advantages of monolithic over particulate columns for multiresidue analysis of organic pollutants by in-tube solid-phase microextraction coupled to c…
2011
Abstract The performance of a monolithic C 18 column (150 mm × 0.2 mm i.d.) for multiresidue organic pollutants analysis by in-tube solid-phase microextraction (IT-SPME)-capillary liquid chromatography has been studied, and the results have been compared with those obtained using a particulate C 18 column (150 mm × 0.5 mm i.d., 5 μm). Chromatographic separation has been carried out under isocratic elution conditions, and for detection and identification of the analytes a UV-diode array detector has been employed. Several compounds of different chemical structure and hydrophobicity have been used as model compounds: simazine, atrazine and terbutylazine (triazines), chlorfenvinphos and chlorp…
Improving analysis of apolar organic compounds by the use of a capillary titania-based column: Application to the direct determination of faecal ster…
2010
This article reports a new procedure for the direct determination of faecal sterols coprostanol and cholesterol in wastewater samples as tracers of human sewage contamination. The method combines in-tube solid-phase microextraction (IT-SPME) for analyte enrichment and capillary liquid chromatography (LC) for separation with diode array detection for identification and quantification. A titania-based polymeric capillary column and a conventional octadecyl silica (ODS) capillary column were evaluated and compared for their ability to separate the analytes. The titania-based column allowed the separation of the analytes in much shorter chromatographic times and with better chromatographic prof…