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71.
Marie Kjærgaard Bjørk Kirsten Wiese Simonsen David Wederkinck Andersen Petur Weihe Dalsgaard Stella Rögn Sigurðardóttir Kristian Linnet Brian Schou Rasmussen 《Analytical and bioanalytical chemistry》2013,405(8):2607-2617
An efficient method for analyzing illegal and medicinal drugs in whole blood using fully automated sample preparation and short ultra-high-performance liquid chromatography–tandem mass spectrometry (MS/MS) run time is presented. A selection of 31 drugs, including amphetamines, cocaine, opioids, and benzodiazepines, was used. In order to increase the efficiency of routine analysis, a robotic system based on automated liquid handling and capable of handling all unit operation for sample preparation was built on a Freedom Evo 200 platform with several add-ons from Tecan and third-party vendors. Solid-phase extraction was performed using Strata X-C plates. Extraction time for 96 samples was less than 3 h. Chromatography was performed using an ACQUITY UPLC system (Waters Corporation, Milford, USA). Analytes were separated on a 100 mm?×?2.1 mm, 1.7 μm Acquity UPLC CSH C18 column using a 6.5 min 0.1 % ammonia (25 %) in water/0.1 % ammonia (25 %) in methanol gradient and quantified by MS/MS (Waters Quattro Premier XE) in multiple-reaction monitoring mode. Full validation, including linearity, precision and trueness, matrix effect, ion suppression/enhancement of co-eluting analytes, recovery, and specificity, was performed. The method was employed successfully in the laboratory and used for routine analysis of forensic material. In combination with tetrahydrocannabinol analysis, the method covered 96 % of cases involving driving under the influence of drugs. The manual labor involved in preparing blood samples, solvents, etc., was reduced to a half an hour per batch. The automated sample preparation setup also minimized human exposure to hazardous materials, provided highly improved ergonomics, and eliminated manual pipetting. Figure
Robotic setup for fully automated solid-phase extraction of whole blood 相似文献
72.
Pınar Talay Pınar Yavuz Yardım Zühre Şentürk 《Central European Journal of Chemistry》2013,11(10):1674-1681
This paper examined for the first time, the possibilities of the usage of a boron-doped diamond electrode for the redox behavior of rutin using cyclic and adsorptive stripping voltammetry. The cyclic voltammograms showed a pair of redox peaks at lower potentials followed by an irreversible oxidation peak at higher positive potential. Using square-wave adsorptive stripping voltammetry, the compound yielded a well-defined voltammetric response in Britton-Robinson buffer, pH 4.0 at +0.48 V (vs. Ag/AgCl) (after 60 s accumulations at a fixed potential of 0.2 V). The calibration curve was linear in the concentration range from 0.01 µg mL?1 to 0.1 µg mL?1 (1.64×10?8 M ? 1.64×10?7 M). A detection limit of 0.0017 µg mL?1 (2.78×10?9 M) was observed without any chemical modifications and electrochemical surface pretreatments. As an example, the practical applicability of boron-doped diamond electrode was tested with the measurement of rutin in dietary supplement products. 相似文献
73.
F. Ditrói F. Tárkányi S. Takács A. Hermanne H. Yamazaki M. Baba A. Mohammadi 《Journal of Radioanalytical and Nuclear Chemistry》2013,298(2):853-865
As a part of our series of studies on charged particle induced reactions on various target materials, proton induced excitation functions on natural cobalt have been determined by using the stacked-foil technique. In these measurements the radionuclides 55,56,57,58Co, 51Cr, 52,54,56Mn and 56,57Ni have been identified. For the above mentioned nuclides the cross-sections were derived from the measured activities and were compared with the literature data and with the results of EMPIRE code calculations and tabulated values in the TENDL 2011 library (based on TALYS code calculations). The agreement with previous measurements and with theoretical values was acceptable. 相似文献
74.
Pavel ?iler Josef Kr��tky Iva Kol��?ov�� Jarom��r Havlica Ji?�� Brand?tetr 《Chemical Papers》2013,67(2):213-220
Possibilities of a multicell isoperibolic-semiadiabatic calorimeter application for the measurement of hydration heat and maximum temperature reached in mixtures of various compositions during their setting and early stages of hardening are presented. Measurements were aimed to determine the impact of selected components?? content on the course of ordinary Portland cement (OPC) hydration. The following components were selected for the determination of the hydration behaviour in mixtures: very finely ground granulated blast furnace slag (GBFS), silica fume (microsilica, SF), finely ground quartz sand (FGQ), and calcined bauxite (CB). A commercial polycarboxylate type superplasticizer was also added to the selected mixtures. All maximum temperatures measured for selected mineral components were lower than that reached for cement. The maximum temperature increased with the decreasing amount of components in the mixture for all components except for silica fume. For all components, except for CB, the values of total released heat were higher than those for pure Portland cement samples. 相似文献
75.
Mehmet Burçin Pişkin Aysel Kantürk Figen Hatice Ergüven 《Research on Chemical Intermediates》2013,39(2):569-583
In this study, the solid-state reaction mechanism and kinetics were investigated for production of anhydrous sodium metaborate (NaBO2), an industrially and technologically important boron compound. To assess the kinetics of solid-state production of NaBO2, the chemical reaction between borax (Na2B4O7) and sodium hydroxide (NaOH) was investigated by use of the thermal analysis techniques thermogravimetry (TG) and differential thermal analysis (DTA). DTA curves obtained under non-isothermal conditions at different heating rates (5, 10 and 20 °C/min), revealed five endothermic peaks corresponding to five solid-state reactions occurring at 70, 130, 295, 463, and 595 °C. The stages of the solid-state reaction used for production NaBO2 were also analyzed by XRD, which showed that at 70 and 130 °C, Na2B4O7 and NaOH particles contacted between the grains, and diffusion was initiated at the interface. However, there was not yet any observable formation of NaBO2. Formation of NaBO2 was initiated and sustained from 295 to 463 °C, and then completed at 595 °C; the product was anhydrous NaBO2. Activation energies (E a) of the solid-state reactions were calculated from the weight loss based on the Arrhenius model; it was found that in the initial stages of the solid-state reaction E a values were lower than in the last three steps. 相似文献
76.
K. Gméling A. Simonits I. Sziklai László D. Párkányi 《Journal of Radioanalytical and Nuclear Chemistry》2014,300(2):507-516
Concentrations of major and trace elements in volcanic rock and soil samples, including geological standard reference materials, were determined by neutron activation analysis (NAA) and prompt gamma activation analysis (PGAA), both using the k 0-standardization method. The paper highlights the different experimental procedures, such as sample preparation, data collection and spectrum evaluation. In geological samples, PGAA gives precise results for major elements (Si, Ti, Al, Fe, Mn, Mg, Ca, Na, K and—as a unique method—for H), for some of the light trace elements as B and Cl, as well as for Sc, S, Cr, Co, Ni, Cd, Nd, Sm and Gd. NAA is sensitive for the rare earth elements, and for many major (Ti, Al, Fe, Mn, Mg, Ca, Na, K) and trace elements (e.g.: Sc, V, Cr, Co, Ni, Cu, Zn, As, Se, Rb, Sr, Zr, As, Sb, Ce, Ba, Hf, Ta, W). For most major elements the results obtained by the two methods show good agreement. The comparison of the results obtained for trace elements is not always possible, since PGAA is less sensitive and concentrations are often below its detection limits. Nevertheless, the complementarity of NAA and PGAA allows nearly panoramic analysis of geological materials. 相似文献
77.
A comparison of the analytical performances of four different (bio)sensor designs in H2O2 determination is discussed. The (bio)sensor designs developed were based on the use of (i) multiwalled carbon nanotubes (MWCNT), zinc oxide nanoparticles (ZnONP), prussian blue (PB); (ii) MWCNT, ZnONP, PB and ionic liquid (IL); (iii) MWCNT, ZnONP and horseradish peroxidase (HRP) and (iv) MWCNT, ZnONP, HRP and IL modified glassy carbon electrode (GCE). A performance comparison of (bio)sensors showed that the one based on HRP/IL-MWCNT-ZnONP/GCE showed the best analytical characteristics with a linear dynamic range of 9.99×10−8–7.55×10−4 M, detection limit of 1.37×10−8 M and sensitivity of 17.00 μA mM−1. 相似文献
78.
Cucer N Imamoglu N Tozak H Demirtas H Sarac F Tatlisen A Oztürk F 《Micron (Oxford, England : 1993)》2007,38(6):674-679
Traditional criterions are not sufficient to predict accurately the recurrence of transitional cell carcinoma of the urinary bladder. Therefore, we aimed to evaluate the AgNORs via total AgNOR area/nucleus area (TAA/NA) for each cell as a prognostic parameter, in TCC of urinary bladder. Tumor tissues of 20 consecutive cases of male bladder cancer patients were divided into two groups as middle differentiated (LG) and high grade (HG). The extra-tumoral tissue (ETT) samples of 10 males served as control group. A second control group (HC) consisted of five healthy and normal bladder tissue samples. The 3 microm of sections from each paraffin embedded tumoral, extra-tumoral and normal tissue samples served as patient and control groups. After deparaffinization and rehydratation steps, silver (AgNO(3)) staining of nucleolar organizer regions-associated proteins (AgNORs) was performed. Instead of Giemsa stain, we used Hematoxylin for contra staining. The images of the 100 analyzable nuclei from each tissue sample, transferred by means of a video camera and video capture card from microscope and recorded onto a computer. Software was prepared in Delphi language for analysis. Mean (E+02) TAA/NA values of HC, ETT, LG and HG groups were 6.97+2.80, 5.70+1.82, 7.80+3.22 and 9.24+3.88, respectively. Statistical comparisons have shown significant differences between all groups.In conclusion, mean TAA/NA per cell has a potential to be a prognostic parameter. Therefore, further evaluation of big patient series will be useful. 相似文献
79.
Aysel Kantürk Figen Pınar Yilmaz Atali Mehmet Burçin Pişkin 《Journal of Thermal Analysis and Calorimetry》2014,118(1):31-42
In this study, the thermal behavior in terms of glass transition (T g), degradation, and thermal stability of four commercial new-generation posterior bulk fill composites (Surefill SDR, Dentsply; Quixfill, Dentsply; Xtrabase, Voco; and Xtrafill, Voco) activated by light-emitting diodes (LEDs) was analyzed by thermogravimetric analysis (TG), differential scanning calorimetry (DSC), and dynamic mechanical analysis (DMA). The activation energies (E a) for the decomposition of the dental resins were calculated based on the Kissinger and Doyle kinetic models from the peaks of the endothermic curves obtained when the specimens were heated at four different temperatures (5, 10, 15, and 20 °C min?1) during DSC. The results show that the Xtrabase composite displayed the highest T g (120 °C at a 5 °C min?1 heating rate) and E a (157.64 kJ mol?1) values associated with thermal degradation from the main chain of the polymer. 相似文献
80.
Adsorption of Large Hydrocarbons on Coinage Metals: A van der Waals Density Functional Study
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The adsorption of organic molecules onto the close‐packed facets of coinage metals is studied, and how accurately adsorption heights can be described by using recent advances of the van der Waals density functional (vdWDF), with optPBE/vdWDF, optB86b/vdWDF, vdWDF2, and rev/vdWDF2 functionals is illustrated. The adsorption of two prototypical aromatic hydrocarbons is investigated, and the calculated adsorption heights are compared to experimental literature values from normal incident X‐ray standing wave absorption and a state‐of‐the‐art semi‐empirical method. It is shown that both the optB86b/vdWDF and rev/vdWDF2 functionals describe adsorption heights with an accuracy of 0.1 Å, compared to experimental values, and are concluded as reliable methods of choice for related systems. 相似文献