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Synthetic Samples (synthetic + sample)
Selected AbstractsEvaluation and use of a synthetic quality control material, included in the European external quality assessment scheme for cystic fibrosis,HUMAN MUTATION, Issue 8 2008Sarah Berwouts Abstract Assuring high quality within the field of genetic testing is fundamental, as the results can have considerable impact on the patient and his or her family. The use of appropriate quality control (QC) samples is therefore essential. Diagnostic laboratories mainly use patient samples as QC material, which of course include a maximum of two mutations per sample. Bearing in mind that some assays (such as for cystic fibrosis [CF] testing) can test for more than 100 mutations, multiplex QC materials including more than two mutations could save valuable time and reagents. Based on this need, synthetic multiplex controls have been developed by Maine Molecular Quality Controls, Inc. (MMQCI) for CF. A synthetic control, containing six homozygous mutations and one polymorphism for CF transmembrane conductance regulator (CFTR), was evaluated by distributing it through the CF external quality assessment (EQA) scheme, along with the EQA samples in 2005. A total of 197 participants returned results of the yearly EQA scheme and 133 laboratories participated in the evaluation of the synthetic sample. Respectively, 76% and 73% of the participants were assigned as successful. This evaluation study revealed that the multiplex QC material performed well in the majority of assays and could be useful in method validation, as a tool to challenge interpretation skills, and as potential proficiency testing (PT) material. Hum Mutat 0, 1,8, 2008. © 2008 Wiley-Liss, Inc. [source] High-performance liquid chromatography with electrospray ionisation mass spectrometry and diode array detection in the identification and quantification of the degradation products of calix[4]arene crown-6 under radiolysisRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 13 2004C. Lamouroux The extraction of 135Cs from high-activity liquid waste, arising from reprocessing of spent nuclear fuel, can be achieved by using calix[4]arene crown-6 compounds. The radiolytic degradation of di(n-octyloxy)calix[4]arene crown-6 (octMC6), in aliphatic or aromatic solvent in contact with 3 M nitric acid, was studied by high-performance liquid chromatography directly coupled to electrospray ionisation mass spectrometry (LC/ESI-MS). More than 50 distinct degradation products were observed, and about 30 of these were identified. These compounds can be assigned to three categories, namely, products of reactions involving radical cleavage or addition, of oxidation reactions, or of aromatic substitution reactions. The major product, corresponding to substitution by an NO2 group, was quantified by external standard calibration using a purified synthetic sample. Despite the observation of all these degradation compounds, octMC6 appears to be remarkably stable under these drastic conditions, combining hydrolysis (HNO3 3,M) and an extreme exposure to radiolysis (106,Gy). Less than 35% degradation of octMC6 was observed in aromatic solvent under these conditions. Copyright © 2004 John Wiley & Sons, Ltd. [source] Simultaneous Quantification of Heavy Metals Using a Solid State Potentiometric Sensor ArrayELECTROANALYSIS, Issue 8 2009Jesús Gismera Abstract A potentiometric sensor array of four nonspecific electrodes with solid-state membranes is developed and tested for simultaneous analysis of copper(II), mercury(II), and silver(I) ions. The cross-sensitivity responses of the sensors for these ions are evaluated. The array potentiometric signals are processed by partial least-squares regression (PLS) and back propagation artificial neural networks (ANN) to determinate analyte concentrations. The ANN configuration is optimized and two different training algorithms of the ANN are also evaluated. Best results are obtained when the potentiometric sensors are activated and the data are processed using ANN and the gradient descent adaptive algorithm. The system is used to quantify these heavy metals in synthetic samples and in dental amalgams with successful results. [source] Electrochemical Detection of Arsenic(III) in the Presence of Dissolved Organic Matter (DOM) by Adsorptive Square-Wave Cathodic Stripping Voltammetry (Ad-SWCSV)ELECTROANALYSIS, Issue 4 2008Tsanangurayi Tongesayi Abstract This study has demonstrated that As(III) can be electrochemically detected and quantified in the presence of fulvic acid (FA) and dissolved organic matter (DOM). This eliminates the need to remove DOM prior to measurement of As(III) in environmental samples. Apart from reducing analysis time and the cost of the analysis, this could be potentially useful for the development of electrochemical methods for the detection and measurement of As(III) onsite. Both synthetic samples in which FA was added and a real sample with 22.16,mg/L total organic carbon (TOC) were analyzed. [source] Minerals as Model Compounds for Cu/ZnO Catalyst Precursors: Structural and Thermal Properties and IR Spectra of Mineral and Synthetic (Zincian) Malachite, Rosasite and Aurichalcite and a Catalyst Precursor MixtureEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 10 2009Malte Behrens Abstract The Cu/ZnO system is a model for Cu/ZnO/Al2O3 catalysts, which are employed industrially for the synthesis of methanol. These catalysts are usually prepared from mixed basic carbonate precursors. A complex phase mixture, with constituents structurally related to the minerals rosasite andaurichalcite, is present at the industrially applied composition (Cu/Zn , 70:30). Using minerals and phase-pure synthetic samples as references, a comprehensive characterisation of such a phase mixture, including the determination of the individual compositions of the different phases, has been attempted by complementary analytical laboratory techniques (XRD, TGA, IR). The results are critically discussed in light of the complexity of the system. A thermally very stable carbonate species , well-known for mixed synthetic systems , is also detected for the mineral reference samples. Significant amounts of amorphous phases are found to be present in the synthetic zincian malachite sample but not in synthetic aurichalcite or the catalyst precursor. A simplified explanation for the shift of the characteristic 20 reflection of the malachite structure as a function of Zn incorporation based on the varying average Jahn,Teller distortion of the MO6 octahedra is proposed. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2009) [source] Determination of Selenium Concentration in Sixty Five Reference Materials for Geochemical Analysis by GFAAS after Separation with Thiol CottonGEOSTANDARDS & GEOANALYTICAL RESEARCH, Issue 2-3 2001Luc Marin sélénium; SAA four graphite; séparation; matériaux géologiques de référence; coton thiol Selenium has been determined in sixty five geological reference materials of different origins by graphite furnace atomic absorption spectrometry. Samples were decomposed with a mixture of nitric and hydrofluoric acids. Selenium was reduced to SeIV with hydrochloric acid, and then fixed and separated from the matrix on thiol cotton. After digestion of the thiol cotton in hot nitric acid, the Se concentration was measured using palladium and magnesium nitrates as a matrix modifier. The limit of determination was 0.02 ,g g,1, the precision of the results (relative standard deviation of 3 to 8 replicates) varied from 2.6 to 17.7% with an average of 7.9% in the range 0.02-42.7 ,g g,1 and was similar to the value obtained for synthetic samples. Our results are in good agreement with available literature values. Le sélénium a été dosé sur 65 standards géochimiques de référence de différentes provenances par spectrométrie d'absorption atomique avec four graphite. Les échantillons ont été mis en solution par une attaque acide HNO3 -HF. Le sélénium a été réduit en SeIV avec de l'acide chlorhydrique, fixé et séparé de la matrice sur du coton thiol. Après décomposition du coton thiol par chauffage avec de l'acide nitrique, les concentrations en sélénium ont été mesurées en utilisant du nitrate de palladium et de magnésium comme modificateur de matrice. La limite de détermination est de 0.02 ,g g,1, la précision des résultats (écart type relatif sur 3 à 8 mesures) pour les standards géochimiques varie de 2.6 à 17.7% avec une moyenne de 7.9% dans la game 0.02-42.7 ,g g,1et est comparable à celle obtenue pour des échantillons synthétiques. Nos résultats sont en bonne concordance avec les résultats déjà publiés dans la littérature. [source] The differentiation of biodegradable and non-biodegradable dissolved organic matter in wastewaters using fluorescence spectroscopyJOURNAL OF CHEMICAL TECHNOLOGY & BIOTECHNOLOGY, Issue 8 2002M Reynolds Abstract The chemical and biochemical oxygen demand values of a number of synthetic and wastewater samples were determined using fluorescence spectroscopy. Treated and untreated sewage samples were obtained from a local sewage treatment works while synthetic samples were analysed before, during, and after treatment via a rotating biodisc contactor. Fluorescence intensities were normalised using the water Raman signal as an internal standard and corrections applied to take into account the attenuation effects caused by the sample matrix. The fluorescence emission spectra (,exc,=,280,nm) of synthetic and sewage samples were very similar in that two main fluorescence bands centred around 350,nm and 440,nm were observed in all samples. Normalised fluorescence data, centred at 350,nm, correlate well with corresponding BOD, COD and TOC values (R2 values ranging between 0.93 and 0.98). Using BOD, COD and TOC data the fluorescence at 350,nm and 440,nm can be apportioned to biodegradable and non-biodegradable dissolved organic matter respectively. The findings of this research show that fluorescence data can be used to quantify oxygen demand values (chemical and biochemical) and total organic carbon values. Furthermore, the fluorescence spectral response can be apportioned to biodegradable (BOD) and non-biodegradable (COD,,,BOD) dissolved organic matter. The potential of using fluorescence spectroscopy as a possible tool for real-time monitoring of sewage wastes is discussed. © 2002 Society of Chemical Industry [source] A fluorimetric method for the determination of trace pentachlorophenol, based on its inhibitory effect on the redox reaction between the improved Fenton reagent and rhodamine BLUMINESCENCE: THE JOURNAL OF BIOLOGICAL AND CHEMICAL LUMINESCENCE, Issue 5 2007Huiqin Guo Abstract A sensitive fluorimetric method is presented and discussed for the determination of pentachlorophenol in aqueous solutions. This method is based on the inhibitory effect of pentachlorophenol on the reaction of conventional Fenton [Fe(III) + H2O2] reagent with rhodamine B in the medium of perchloric acid, which results in the fluorescence quenching of rhodamine B. It was further found that the sensitivity for the determination was improved significantly when the molecular ligand EDTA was added. This improved system was therefore presented for the determination of pentachlorophenol. The characteristics of the excitation and emission spectra, optimization of the experimental conditions, the stability of the system and the influence of foreign matter have all been investigated. Under optimal conditions, the linear range for the determination of pentachlorophenol is 12,480 ng/mL with a 3, limit of detection of 0.96 ng/mL. Compared with the conventional Fenton system, the improved system shows obvious advantages in both sensitivity and selectivity. By combination with the pretreatment of samples using ion exchange resins and XDA-1 absorption resin, the improved Fenton method was used for the first time for the determination of pentachlorophenol in synthetic samples and natural water samples, and satisfactory results, in agreement with those of the HPLC method, were achieved. The possible mechanism of the reactions has also been discussed. Copyright © 2007 John Wiley & Sons, Ltd. [source] Wavelength-dispersive X-ray fluorescence analysis of ancient glasses,ARCHAEOMETRY, Issue 4 2002R. Falcone The application of X-ray fluorescence to the study of the composition of ancient glasses has been limited by the large amount of material required for samples. In this paper the setting of a reduced sampling XRF method for the analysis of ancient glasses is described. The method involves the preparation of glass beads by melting the sample with lithium tetraborate flux. By means of reference and synthetic samples, the method allows regression curves to be set, covering broad ranges from ppm to high concentrations. By means of a single program, up to 31 elements of interest in the study of ancient glass are analysed. The reproducibility, sensitivity and reliability of the method are discussed. The results demonstrate that 0.2 g of glass is sufficient to obtain accurate and sensitive analyses for most of the elements of interest. [source] Metabolism of a Highly Selective Gelatinase Inhibitor Generates Active MetaboliteCHEMICAL BIOLOGY & DRUG DESIGN, Issue 5 2007Mijoon Lee (4-Phenoxyphenylsulfonyl)methylthiirane (inhibitor 1) is a highly selective inhibitor of gelatinases (matrix metalloproteinases 2 and 9), which is showing considerable promise in animal models for cancer and stroke. Despite demonstrated potent, selective, and effective inhibition of gelatinases both in vitro and in vivo, the compound is rapidly metabolized, implying that the likely activity in vivo is due to a metabolite rather than the compound itself. To this end, metabolism of inhibitor 1 was investigated in in vitro systems. Four metabolites were identified by LC/MS-MS and the structures of three of them were further validated by comparison with authentic synthetic samples. One metabolite, 4-(4-thiiranylmethanesulfonylphenoxy)phenol (compound 21), was generated by hydroxylation of the terminal phenyl group of 1. This compound was investigated in kinetics of inhibition of several matrix metalloproteinases. This metabolite was a more potent slow-binding inhibitor of gelatinases (matrix metalloproteinase-2 and matrix metalloproteinase-9) than the parent compound 1, but it also served as a slow-binding inhibitor of matrix metalloproteinase-14, the upstream activator of matrix metalloproteinase-2. [source] Resonance Light Scattering Imaging Detection of Single Suprahelical Species of DNA Induced by Porphine-5,10,15,20-tetrakis(p -phenyltrimethylaminium)CHINESE JOURNAL OF CHEMISTRY, Issue 1 2006Xi-Dong Liu Abstract A resonance light scattering (RLS) imaging method was proposed based on imaging and measuring the RLS features of single suprahelical species of DNA, and its application to DNA assay was also investigated. In acidic medium, porphine-5,10,15,20-tetrakis(p -phenyltrimethylaminium) (PTPTMA), could stack along the molecular surface of DNA with the mode of long-range assembly to induce the formation of suprahelical species of DNA, resulting in strong RLS signals in the range of 450,510 nm. Under the excitation of 488 nm light beam of argon ion laser source, single suprahelical species could be observed with the aid of a common microscope due to the strong scattered light emitted by the suprahelical species. By capturing the RLS images of the single suprahelical species with a cooled charge coupled device (CCD) camera, and analyzing the RLS data, herein an RLS imaging method of DNA was proposed based on the linear relationship between the counts of suprahelical species in the detection focus plane and the concentration of DNA in nanograms. When 1.8??µmol/L PTPTMA was employed, both calf thymus DNA (ct DNA) and fish sperm DNA (fs DNA) in the range of 25,1100 ng/mL could be detected with the limits of detection lower than 25 ng/mL (3,). Four synthetic samples were detected satisfactorily with relative standard deviations less than 5.1%. [source] Analysis of optical purity and impurity of synthetic d -phenylalanine products using sulfated ,-cyclodextrin as chiral selector by reversed-polarity capillary electrophoresisCHIRALITY, Issue 2 2006Yan Zhao Abstract A new capillary electrophoresis (CE) method has been achieved for simultaneous separation and quantification of phenylalanine, N -acetylphenylalanine enantiomers, and prochiral N -acetylaminocinnamic acid, possibly co-existent in reaction systems or synthesized products of d -phenylalanine. The separation was carried out in an uncoated capillary under reversed-electrophoretic mode. Among the diverse charged cyclodextrins (CDs) examined, highly sulfated (HS)-,-CD as the chiral selector exhibited the best enantioselectivity. The complete separation of the analytes was obtained under the optimum conditions of pH 2.5, 35 mM Tris buffer containing 4% HS-,-CD, applied voltage ,15 kV, and capillary temperature 25°C. Furthermore, the proposed method was applied to the determination of optical purity and trace impurities in three batches of the asymmetric synthetic samples of d -phenylalanine, and satisfactory results were obtained. The determination recoveries of the samples were in the range of 97.8,103.8%, and precisions fell within 2.3,5.0% (RSD). The results demonstrate that this CE method is a useful, simple technique and is applicable to purity assays of d -phenylalanine. © 2005 Wiley-Liss, Inc. Chirality 18:84,90, 2006. [source] | |||||||||||||