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21.
22.
Souza MJ Kulmann RR Silva LM Nogueira DR Zimmermann ES Schmidt CA 《Journal of AOAC International》2006,89(5):1367-1372
Cefepime is a new parenteral cephalosporin that has been described as a fourth-generation, broad-spectrum antibiotic. This paper reports the development and in-house validation of an agar diffusion bioassay using a cylinder-plate method for the determination of cefepime in powder for injection. The validation performed yielded good results in terms of linearity, precision, accuracy, and robustness. The assay is based on the inhibitory effect of cefepime upon the strain of Micrococcus luteus ATCC 10240 used as the test microorganism. The results of assays were treated statistically by analysis of variance (ANOVA) and were found to be linear (r = 0.99993) in the selected range of 8.0-32.0 microg/mL; precise [repeatability: relative standard deviation (RSD) = 1.39%, intermediate precision: between-day RSD = 1.77%, and between-analyst RSD = 1.97%] and accurate. Comparison of bioassay and liquid chromatography by ANOVA showed no significant difference between methodologies. The results demonstrated the validity of the proposed bioassay, which is a simple and useful alternative methodology for cefepime determination in routine quality control. 相似文献
23.
Koichi Todoroki Maurizio Corradini Ryugo S. Hayano Takumi Kobayashi Marco Leali Evandro Lodi Rizzini Valerio Mascagna Anna Soter Luca Venturelli Nicola Zurlo Masaki Hori 《Hyperfine Interactions》2012,213(1-3):199-204
The ASACUSA (the Atomic Spectroscopy And Collisions Using Slow Antiprotons) collaboration is planning to measure the cross sections of antiproton annihilations at kinetic energy 100 keV on targets of various mass numbers (C,?Ni, Sn, and Pt) using the Antiproton Decelerator (AD) of CERN. No previous measurement exists in this region where the A-dependence of the cross section is expected to deviate from the A $^{\frac{2}{3}}$ (Batty et al, Nucl Phys A 689:721, 2001) as reported by the Obelix collaboration. A beam profile monitor based on secondary electron emission with a grid of electrode pads fabricated on an FR4-type glass-epoxy circuit board was developed for this measurement. The advantage of this kind of detector is that it is simple, lightweight, and low cost. It was used to measure the spatial profile of 100-ns-long beam pulses containing > 6 × 104 antiprotons with an active area of 40?mm?× 40 mm and a spatial resolution of 4 mm. 相似文献
24.
Schubert A Werle AL Schmidt CA Codevilla C Bajerski L Chiappa R Cardoso SG 《Journal of AOAC International》2003,86(3):501-504
An accurate, simple, reproducible, and sensitive liquid chromatographic method was developed and validated for the determination of omeprazole in powder for injection and in pellets. The analyses were performed at room temperature on a reversed-phase C18 column of 250 x 4.6 mm id, 5 microm particle size. The mobile phase, composed of methanol-water (90 + 10, v/v), was pumped at a constant flow rate of 1.5 mL/min. Detection was performed on a UV detector at 301 nm. The method was validated in terms of linearity, precision, accuracy, and ruggedness. The response was linear in the range 32-48 microg/mL (r2 = 0.9976). The relative standard deviation values for intra- and interday precision studies were 1.22 and 1.56% for injectable and 2.13 and 2.45% for pellets, respectively. Recoveries ranged between 95.81 and 100.48%. 相似文献
25.
A procedure for preconcentration and determination of lead in water is described. The method is based on the sorption of Pb(II) in a minicolumn packed with a functionalized sorbent and subsequent elution with acidic solution. The determination of lead content in the eluate was carried out using flame atomic absorption spectrometry. The sorbent was prepared by immobilization of the ligand 4-(5'-bromo-2'-thiazolylazo)orcinol on polystyrene-divinylbenzene through an azo spacer. Diazotization and coupling reactions were used for synthesis of the sorbent. Some variables affecting the preconcentration were optimized using a full factorial design. Under optimized conditions, the method presented a detection limit of 0.5 microg/L and enrichment factor of 36 for a sample volume of 25 mL. The accuracy of the method was tested by the determination of lead in a standard reference material (National Institute of Standards and Technology 1643d Fresh Water). The proposed procedure was applied to the determination of lead in samples of natural and drinking waters. 相似文献
26.
De Almeida MV De Assis JV Couri MR Anconi CP Guerreiro MC Dos Santos HF De Almeida WB 《Organic letters》2010,12(23):5458-5461
Two synthetic epoxide derivatives, important intermediates in organic synthesis, were obtained from L-quebrachitol, and their conformations were proposed based on spectroscopic analysis. Density functional theory (DFT) calculations of infrared and NMR spectra were shown to be reliable enough for organic chemistry applications. The observed structures were determined with the aid of the DFT spectroscopic data, stressing the relevance and utility of combined experimental/theoretical studies and also the usefulness of the (13)C NMR B3LYP/6-31G(d,p) calculations. 相似文献
27.
Cleber V. Ursini Fabrizio Mazzeo J. Augusto R. Rodrigues 《Tetrahedron: Asymmetry》2006,17(24):3335-3340
The asymmetric transfer hydrogenation (ATH) of ferrocenyl ketones, such as FcC(O)CH2Y [Fc = ferrocenyl, Y = H (1a), CH3 (1b), Cl (1c) or N3 (1d)] has been carried out using the Noyori/Ikariya catalysts [(−)-(1R,2S)-ephedrine] or N-tosyl-(1R,2R)-diphenylethylenediamine [(R,R)-TsDPEN] as chiral ligands combined with [RuCl2(η6-benzene)]2 and 2-PrOH or HCO2H–Et3N as the hydrogen sources, respectively. The best results were achieved with the [(R,R)-TsDPEN–RuIIHCO2H–Et3N] catalytic system, which produced the ferrocenylalcohols (R)-2a, (R)-2c, and (R)-2d in good yields and excellent enantiomeric excesses (>98% ee). 相似文献
28.
Oliveira CS Bastos EL Duarte EL Itri R Baptista MS 《Langmuir : the ACS journal of surfaces and colloids》2006,22(21):8718-8726
The interfacial localization and the ion pair formation of the positively charged dye crystal violet (CV) in sodium bis(2-ethylhexyl)sulfosuccinate reverse micelles (AOT RMs) were studied by several structural and spectroscopic techniques and by quantum chemical calculations. The size and shape of the AOT RMs in the presence of CV were investigated by small-angle X-ray scattering, showing that CV does not significantly change the RM structure. CV localization as a function of the water to surfactant molar ratio (w(0)) was characterized by H(1) and (13)C NMR, indicating the close proximity of CV to the sulfosuccinate group of AOT at small and large w(0) values. These results were confirmed by calculation of magnetic shielding constants using the gauge-independent atomic orbital method with the HF/6-31G(d) basis set. Two different types of ion pairs between AOT and CV, i.e., contact ion pair (CIPs) and solvent-separated ion pair (SSIPs), were characterized by UV-vis spectroscopy and quantum chemical calculations using the semiempirical ZINDO-CI method. In nonpolar isotropic solvents CIPs are formed with an association constant (K(ASSOC)) of 2 x 10(4) mol(-1) L in isooctane and 750 mol(-1) L in chloroform. In AOT RMs at low w(0), CV-AOT CIPs are also formed. By increasing w(0), there is a sharp decrease in the CIP association free energy, and SSIPs are formed. (CV(+))(H(2)O)(AOT(-)) SSIPs are stable in the AOT RM up to the largest w(0) tested (w(0) = 33). 相似文献
29.
Ruben Dario Fonseca Daniel Souza Correa Elaine Cristina Paris Vinicius Tribuzi Apurba Dev Tobias Voss Pedro Henrique Benites Aoki Carlos Jose Leopoldo Constantino Cleber Renato Mendonca 《Journal of Polymer Science.Polymer Physics》2014,52(4):333-337
We present an approach to fabricate ZnO nanowires/polymer composite into three‐dimensional microstructures, based on two‐photon polymerization direct laser writing, a fabrication method that allows submicrometric spatial resolution. The structural integrity of the structures was inferred by scanning electron microscopy, while the presence and distribution of ZnO nanowires was investigated by energy dispersive X‐ray, Raman spectroscopy, and X‐ray diffraction. The optical properties of the produced composite microstructures were verified by imaging the characteristic ZnO emission using a fluorescence microscope. Hence, such approach can be used to develop composite microstructures containing ZnO nanowires aiming at technological applications. © 2013 Wiley Periodicals, Inc. J. Polym. Sci. Part B: Polym. Phys. 2014 , 52, 333–337 相似文献
30.
Dalmora SL Júnior LB Schmidt CA Vaccari SF Oliveira PR Codevilla CF 《Journal of AOAC International》2004,87(6):1305-1308
Enoxaparin is a low-molecular weight heparin used clinically for the prevention and treatment of venous and arterial thrombosis. An anti-factor Xa assay was used to evaluate the potency of the final drug preparation. Method validation investigated parameters such as the range, linearity (r2 = 0.9971), precision, accuracy, and robustness; the biological assay incorporated a chromogenic endpoint and detection at 405 nm. The method yielded good results with a quantitation limit of 0.037 IU/mL and a detection limit of 0.011 IU/mL. The results demonstrated the validity of the anti-factor Xa assay for the determination of enoxaparin. 相似文献