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101.
    
This paper reports the development of a simple electroanalytical method for imazethapyr (IMT) determination in rice samples based on molecularly imprinted polymer and functionalized carbon black paste electrode (MIP-fCBPE). Carbon black (CB) was functionalized by the insertion of oxygenated functional groups upon acid treatment with HNO3 and H2SO4. The functionalized carbon black (fCB) presented higher performance for IMT determination than the CB without functionalization. The insertion of molecularly imprinted polyvinylimidazole (MIP-VN) in the fCBPE promoted a significant increase in the cathodic peak current even at low proportions (7.5 % w/w) due to the specific binding sites for IMT recognition. For IMT determination, DPV parameters were optimized by the Doehlert matrix applying 0.1 V for 60 s as pre-treatment in acetate buffer solution (pH 3.0) as supporting electrolyte. The proposed method showed low limit of detection (0.03 μmol L−1), a wide linear range (0.10–70.00 μmol L−1), and good precision in terms of repeatability of intraday measures (RSD%=3.6). The method was applied in rice samples after microwave-assisted extraction of IMT and the accuracy of the method was evaluated by addition/recovery assays (96.3–105.7 %), being statistically attested using HPLC-DAD as reference technique.  相似文献   
102.
    
Different from works described in the literature, which use expansive analytical methods to separation of anthraquinones derivatives (AQs), this communication reported a simple and inexpensive methodology to get them. In this way, the expensive commercial AQs: Chrysophanol, physcione and emodine were extracted from plant material (Rhamnus frangula L.) and isolated by classical column chromatography technique under optimised binary mobile phase gradients (CHCl3 : AcOEt(a), a = 1 to 5%) in excellent yields.  相似文献   
103.
Silica nanoparticles attached to gallic acid were synthesized from 7-nm diameter fumed silica particles by different functionalization methods involving the condensation of hydroxyl or carboxyl groups. The particles were characterized by thermal analyses and UV–vis, FTIR, NMR, and EPR spectroscopies. In comparison to free gallic acid, enhanced stability and increased antimicrobial activity against Paenibacillus larvae were found for the functionalized nanoparticles. Thus, both derivatization strategies result in improved properties of the natural polyphenol as antimicrobial agent for the treatment of honeybee pathologies.  相似文献   
104.
Ceftazidime (CFZ) is a broad spectrum parenteral beta-lactam antibiotic of the cephalosporin family. This paper reports the development and validation of an agar diffusion microbiological assay using the cylinder-plate method for determination of CFZ in powder for injection. The validation carried out yielded good results in terms of linearity, precision, accuracy, selectivity, and robustness. The assay is based on the inhibitory effect of CFZ upon the strain of Pseudomonas aeruginosa ATCC 27853 used as the test microorganism. The results of the assays were treated statistically by analysis of variance and were found to be linear (correlation coefficient = 0.999998) in the selected range of 8.0-32.0 microg/mL; precise [repeatability: relative standard deviation (RSD) = 1.11%; intermediate precision: between-day RSD = 1.37% and between-analyst RSD = 1.41%]; and accurate. The selectivity of the bioassay was evaluated by analysis of degraded samples at 50 degrees C, and the results were compared with a pharmacopeial liquid chromatographic method at the time 0, 24, and 48 h. The results demonstrated the validity of the proposed bioassay, which allows reliable quantitation of CFZ in pharmaceutical samples and can be used as a useful alternative methodology for CFZ analysis in routine quality control.  相似文献   
105.
Multi-start methods for combinatorial optimization   总被引:1,自引:0,他引:1  
Multi-start methods strategically sample the solution space of an optimization problem. The most successful of these methods have two phases that are alternated for a certain number of global iterations. The first phase generates a solution and the second seeks to improve the outcome. Each global iteration produces a solution that is typically a local optimum, and the best overall solution is the output of the algorithm. The interaction between the two phases creates a balance between search diversification (structural variation) and search intensification (improvement), to yield an effective means for generating high-quality solutions. This survey briefly sketches historical developments that have motivated the field, and then focuses on modern contributions that define the current state-of-the-art. We consider two categories of multi-start methods: memory-based and memoryless procedures. The former are based on identifying and recording specific types of information (attributes) to exploit in future constructions. The latter are based on order statistics of sampling and generate unconnected solutions. An interplay between the features of these two categories provides an inviting area for future exploration.  相似文献   
106.
Journal of Inclusion Phenomena and Macrocyclic Chemistry - This research evaluated the chemical composition of Ocimum basilicum and Syzygium aromaticum and to characterize their complex with...  相似文献   
107.
A rapid, sensitive and specific LC‐MS/MS method was developed and validated for quantifying chlordesmethyldiazepam (CDDZ or delorazepam), the active metabolite of cloxazolam, in human plasma. In the analytical assay, bromazepam (internal standard) and CDDZ were extracted using a liquid‐liquid extraction (diethyl‐ether/hexane, 80/20, v/v) procedure. The LC‐MS/MS method on a RP‐C18 column had an overall run time of 5.0 min and was linear (1/x weighted) over the range 0.5–50 ng/mL (R > 0.999). The between‐run precision was 8.0% (1.5 ng/mL), 7.6% (9 ng/mL), 7.4% (40 ng/mL), and 10.9% at the low limit of quantification—LLOQ (0.500 ng/mL). The between‐run accuracies were 0.1, –1.5, –2.7 and 8.7% for the above mentioned concentrations, respectively. All current bioanalytical method validation requirements (FDA and ANVISA) were achieved and it was applied to the bioequivalence study (Cloxazolam—test, Eurofarma Lab. Ltda and Olcadil®— reference, Novartis Biociências S/A). The relative bioavailability between both formulations was assessed by calculating individual test/reference ratios for Cmax, AUClast and AUC0‐inf. The pharmacokinetic profiles indicated bioequivalence since all ratios were as proposed by FDA and ANVISA. Copyright © 2009 John Wiley & Sons, Ltd.  相似文献   
108.
The computation of penalties associated with the continuous relaxation of integer programming problems can be useful to derive conditional and relational tests which allow to fix some variables at their optimal value or to generate new constraints (cuts). We study in this paper the computation and the use of penalties as a tool to improve the efficiency of algorithms for solving set partitioning problems. This leads to a preprocessing scheme which can be embedded within any exact or approximate algorithm. The strength of these penalties is illustrated through computational results on some real-world set partitioning problems.This work was sponsored by FINEP (research contract number 4.3.86.0689-00), CNPq (research contract numbers 11.1592-84, 30.2281-85 and 40.2002-86.5), IBM Brazil and NSERC (grant # GP0036426).On leave from the Catholic University of Rio de Janeiro, Department of Electrical Engineering, Caixa Postal 38063, Gávea, Rio de Janeiro 22452, Brazil.  相似文献   
109.
The logical test of integrated VLSI circuits is one of the main phases of their design and fabrication. The pseudo-exhaustive approach for the logical test of integrated circults consists in partitioning the original circuits to be tested into non-overlapping subcircuits with a small, bounded number of subcircuits, which are then exhaustively tested in parallel. In this work, we present an approximate algorithm for the problem of partitioning integrated combinational circuits, based on the tabu search metaheuristic. The proposed algorithm presents several original features, such as: the use of a reduced neighborhood, obtained from moves involving only a subset of boundary nodes; complex moves which entail several resulting moves, although the variations in the cost function are easily computable; a bi-criteria cost function combining the number of subcircuits and the number of cuts, which simultaneously adds a diversification strategy to the search; and the use of a bin-packing heuristic as a post-optimization step. The behavior of the proposed algorithm was evaluated through its application to a set of benchmark circuits. The computational results have been compared with those obtained by the other algorithms in the literature, with significant improvements. The average reduction rates have been of the order of 30% in the number of subcircuits in the partition, and of the order of 40% in the number of cuts.  相似文献   
110.
The presence of fluorous tails in room-temperature ionic liquids imparts new properties to their already rich spectrum of appealing features. The interest towards this class of compounds that are of ionic nature with melting point less than 25 °C is accordingly growing; in particular, compounds bearing relatively long fluorous tails have begun to be considered. In this invited presentation, we show recent results arising from the systematic study of structural properties of a series of fluorinated room temperature ionic liquids, with growing fluorous chain length. At odd with the current understanding of this class of compounds, we show experimentally that they are characterized by the presence of segregated fluorous domains whose size depends on the fluorous chain length. This experimental finding, based on the synergic use of X-ray and neutron scattering, provides a structural scenario at the mesoscopic spatial scale that is in agreement with the recent state of the art molecular dynamic simulations. We speculate on the potential role of this significant compartmentalization of the bulk liquid phase into different nanoscale domains, as relevant in a series of applications including separation, solubility, catalysis, and so forth.  相似文献   
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