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The performance of commercially available microtiter plate enzyme-linked immunosorbent assays (ELISA) kits specific for the determination of triazines (atrazine), chlorpyrifos, and diazinon was evaluated for sensitivity, intra-assay repeatability, and accuracy using samples of known concentration in aqueous solution. Mean percent recovery values were not significantly different among concentrations...
The European research project DIFFERENCE is focussed on the development, optimisation and validation of screening methods for dioxin analysis, including bio-analytical and chemical techniques (CALUX, GC-LRMS/MS, GCxGC-ECD) and on the optimisation and validation of new extraction and clean-up procedures. The performance of these techniques is assessed in an international validation study and the results...
Accuracy profiles of chemical assays are introduced and derived from the uncertainty of the analytical result. The calculation of accuracy profiles is based on the estimation of the measurement uncertainty of the analytical assay from validation data. For the sake of illustration, a case study dealing with the spectrofluorimetric determination of quinine in tonic water is explained in detail.
Certified reference materials (CRMs) of different origin were used to validate the direct determination of total mercury by solid sampling Zeeman atomic absorption spectrometry (SS-ZAAS) and a specially designed furnace. The temperature program provides only for one step. Atomisation of mercury and pyrolysis of the matrix is performed at a constant temperature in the range of 900–1000°C. Calibration...
4-Aminophenol (4-AP) is the primary degradation product of paracetamol (PARA). According to the European Pharmacopoeia, 50ppm 4-AP/PARA is the specification limit of 4-aminophenol in paracetamol drug substance. For drug products, often higher specification limits, such as 1000ppm 4-AP/PARA are applied. This paper describes a fluorimetric method to quantify the low amount of this degradant (50ppm)...
Miniaturized electrochemical graphite based sensor for the analysis of colchicine, along with its detailed construction was described.The electrochemical behavior of colchicine, both by cyclic and differential pulse voltammetry was investigated, showing an irreversible reduction and oxidation mechanism. The effect of several different electrochemical mediators was studied in order to decrease the...
A new method was developed and validated for the quantification of strictosamide in the extract of the stem bark of Nauclea pobeguinii. This plant belongs to the Rubiaceae family and is widely used in the African traditional medicine against malaria and malaria-like symptoms. Alkaloids are suspected to be responsible for the antimalarial activity. One of these alkaloids is strictosamide, already reported...
In this study, a conventional TEKNOKROMA, Tr-015605 TRACER EXTRASIL ODS2 (25cm×0.4cm, i.d. 5μm) column and a new stationary phase TEKNOKROMA, Tr-010065 Mediterranea sea 18 (15cm×0.4cm, i.d. 3μm) were compared for the separation of five phenolic compounds.Sensitivity, performance characteristics, analysis time and method validation were reported for both columns. A better sensitivity and performance...
Quantification of polycyclic aromatic hydrocarbons (PAHs) in smoked fish products often requires multiple clean-up steps to remove fat and other compounds that may interfere with the chemical analysis. We present a novel pressurized liquid extraction (PLE) method that integrates exhaustive extraction with fat retention in one single analytical step. The PLE parameters: type of fat retainer, flush...
Simultaneous and multi-elemental method was optimized to determine 35 elements in 274 coarse and fine aerosol samples by using HR-ICP-MS. The procedures were validated. Measurement uncertainties of all elements including sampling uncertainties were calculated by applying bottom-up approach. The average recoveries obtained for each element ranged between 79% and 129% using NIST SRM 1648, urban dust...
A sensitive and efficient method was developed for determination of metoprolol in human plasma by gas chromatography–mass spectrometry (GC–MS). Metoprolol and atenolol (internal standard, IS) were extracted from human plasma with a mixture of ethylacetate and diethylether at basic pH with liquid–liquid extraction. Calibration curves were linear over the concentration range 15–500ng/ml. Intra- and...
Roots of Pelargonium sidoides D.C. are used for the production of phytomedicines. Current quality control of phytopreparations containing P. sidoides extracts has been made in terms of total phenolics content. In this work we describe the development and validation of an HPLC method for the analysis of P. sidoides tincture and commercial syrup phytopreparations using umckalin (7-hydroxy-5,6-dimethoxycoumarin)...
In this work we compared the results of the GSNO determination in human plasma by two independent methods. The first method is based on the pre-column derivatization of GSNO thiolic part by p-hydroxymercury benzoate (PHMB) and followed by the determination of GS-PHMB product by reversed phase chromatography coupled to chemical vapour generation atomic fluorescence spectrometry (RPC-CVGAFS). The second...
A sensitive and specific liquid chromatography tandem mass spectrometry method with electrospray ionization for the determination of endothelin-1 in rat plasma and lung effluents has been developed and validated. Detection was achieved by an Applied Biosystems MDS Sciex API 2000 triple quadrupole mass spectrometer coupled to an Agilent 1100 LC system. The limit of detection and the limit of the quantification...
A pressurised liquid extraction (PLE) method for extraction and quantification of total fat and oil in bread and derivatives products has been proposed. Parameters implied in the extraction process; such us temperature, static time, number of extraction cycles, purge time and flush volume; have been optimised using a formal methodology based on statistical experimental design in order to obtain the...
Galanthamine, an acetylcholinesterase inhibitor marketed as a hydrobromide salt for the treatment of Alzheimer's disease, is obtained from some Amaryllidaceae plants. A new method was developed and validated for its quantification by GC–MS in different plant sources: bulbs and leaves from Narcissus confusus; bulbs from N. pseudonarcissus cv. Carlton; and leaves and in vitro cultures from L. aestivum...
The incidence of malignant melanona has increased over the past decades, particularly in Caucasian population. This disease presents defavourable prognosis in terms of survey, especially when detection occurs at the metastatic phase. Reliable analytical methods for biomarker determination are thus an interesting tool in pathology detection and follow-up. In this context, a method using SPE-LC–ESI–MS–MS...
This article aims to expose a new global strategy for the validation of analytical methods and the estimation of measurement uncertainty. Our purpose is to allow to researchers in the field of analytical chemistry get access to a powerful tool for the evaluation of quantitative analytical procedures. Indeed, the proposed strategy facilitates analytical validation by providing a decision tool based...
This work reports a sequential-injection analysis (SIA) method with chemiluminescence (CL) detection for the rapid assay of the total antioxidant capacity (TAC) in wines. The method exploited the Co(II)-catalysed CL reaction of luminol with hydrogen peroxide in alkaline medium. Zones of sample, hydrogen peroxide, catalyst (Co(II) solution) and alkaline luminol were sequentially aspirated into the...
A strategy for the accurate determination in foodstuffs of seven elements liable to be interfered with (V, Cr, Fe, Co, Ni, As and Se), was successfully applied. Firstly, to reduce spectroscopic interferences, four influential factors (hexapole and quadrupole bias, helium and hydrogen flows) of the collision/reaction cell device were optimised through the experimental design methodology. Secondly,...
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