Polymorphism and stability of norfloxacin, (1-ethyl-6-fluoro-1,4-dihydro-4-oxo-7-(1-piperazinil)-3-quinolinocarboxylic acid

Norfloxacin was studied by thermal methods (TG and DSC), X-ray powder diffraction, and by FT-IR, UV-VIS and NMR spectroscopy. The drug substance can be prepared in two different crystalline forms and in amorphous state, depending on the experimental conditions of preparation. DSC examinations were carried out at various heating rates and by cycling the samples in the temperature range 50°–250°C. The unstable crystalline form undergoes two irreversible solid-solid phase transitions at 176.5° and 197.6°C. The polymorph melts in the temperature range 218.5°–220.0°C.

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Zusammenfassung Norfloxacin wurde mittels thermischer Methoden (TG und DSC), weiterhin mittels der Debye-Scherrer-Methode und FTIR-, UV-VIS-und NMR-Spektroskopie untersucht. Je nach den experimentellen Bedingungen bei der Herstellung kann die Wirkstoffsubstanz in zwei verschiedenen kristallinen und in einer amorphen Form hergestellt werden. Die DSC-Untersuchungen wurden bei zahlreichen Aufheizgeschwindigkeiten und durch abwechselnden Temperaturwechsel zwischen Raum- und Schmelztemperatur durchgeführt. Die unstabile kristalline Form unterliegt zwei irreversiblen Feststoff-Feststoff-Umwandlungen bei 176.5° und bei 195.6°C. Das polymorphe Material schmilzt im Temperaturbereich 218.5°–220.0°C.

     

Spectrofluorimetric determination of terbium as its ternary complex with edta and tiron Compositional studies,optimization of fluorescence output and conversion to a flow system

The spectrofluorimetric determination of terbium(III) as its ternary complex with EDTA and Tiron was studied further with regard to composition of the complex and the procedure was optimized by a simplex method. The results suggest a 1:1 molar ratio of terbium to Tiron for the ternary complex. The optimization study indicated that the three chosen variables (pH, and EDTA and Tiron concentration) are not interactive. The method was converted for use in a segmented-flow system with basic Technicon units and a spectrophotofluorimeter as detector. This procedure is satisfactory for the determination of terbium(III) in the range 0.03–0.24 μg ml^?1 at a sampling rate of 30 h^?1. Results were satisfactory for the determination of terbium in lanthanide oxides, mixed oxides, the mineral bastnasite and a green phosphor (Gd_0.96 Ce_0.02 Tb_0.02 F₃).     

A front-tracking/ghost-fluid method for fluid interfaces in compressible flows

A front-tracking/ghost-fluid method is introduced for simulations of fluid interfaces in compressible flows. The new method captures fluid interfaces using explicit front-tracking and defines interface conditions with the ghost-fluid method. Several examples of multiphase flow simulations, including a shock–bubble interaction, the Richtmyer–Meshkov instability, the Rayleigh–Taylor instability, the collapse of an air bubble in water and the breakup of a water drop in air, using the Euler or the Navier–Stokes equations, are performed in order to demonstrate the accuracy and capability of the new method. The computational results are compared with experiments and earlier computational studies. The results show that the new method can simulate interface dynamics accurately, including the effect of surface tension. Results for compressible gas–water systems show that the new method can be used for simulations of fluid interface with large density differences.     

Automatic spectrolfluorimetric method for the determination of dysprosium as its ternary complex with EDTA and Tiron

The automatic method is based on the ternary complex formed with EDTA and Tiron. The method is satisfactory or quantifying 0.1–1.2 μg ml^?1 dysprosium under conditions similar to those used for terbium. The effect of other lanthanides, yttrium, thorium, and dioxouranium(VI) on the fluorescence intensity is described; the main interference is from terbium(III).     

Optimization of MAE for the Separation of Nicotine and Phenolics from Tobacco Waste by Using the Response Surface Methodology Approach

This study intends to valorize by-products of the industrial processing of tobacco to obtain nicotine and phenolics as value-added compounds. Three influential parameters of the microwave-assisted extraction-MAE (temperature, treatment time, and solvent/solid ratio) were studied for the optimization of the extraction protocol for tobacco leaves and three types of waste—scrap, dust, and midrib, respectively. Nicotine was the dominant bioactive compound in all extracts, ranging from 1.512 to 5.480% in leaves, 1.886 to 3.709% in scrap, 2.628 to 4.840% dust, and 0.867 to 1.783% in midrib extracts. Five phenolic compounds were identified and quantified, predominated by chlorogenic acid and rutin. Additionally, total phenol content and antioxidant activity were determined using spectrophotometric assays. Optimization was performed in two aspects: to obtain a maximum extraction yield with minimum nicotine content and to obtain a maximum extraction yield with maximum nicotine content. These findings demonstrate that tobacco waste is a valuable source of bioactive compounds and MAE can be a promising alternative technique to obtain extracts rich in targeted bioactive compounds, especially nicotine.     

Interaction between protoporphyrin IX and tryptophan silver nanoparticles

Silver nanoparticles (AgNPs) have been intensively studied for several purposes including therapeutic applications in cancer. When prepared with tryptophan and photoreduction, silver nanoparticles (TrpAgNPs) become an alternative to conventional anticancer drugs. In this study, the anticancer activity of synthesized TrpAgNPs against MCF-7 breast cancer cells was evaluated, and the inhibitory concentration (IC50) was found to be ~3.4 mg/mL. Since the protoporphyrin IX (PPIX) concentrations in tumor cells are elevate compared to normal cells, the PPIX-TrpAgNP interaction was studied to investigate if it could contribute for cell apoptosis. The investigation was performed using PPIX solution (0.9 μg/mL) with different TrpAgNP concentrations (from 0 to 13 mg/mL). PPIX was characterized by UV-Vis spectroscopy, steady-state and time-resolved fluorescence spectroscopy. The results have shown that the presence of spherical TrpAgNps with 16-nm diameter quench the PPIX fluorescence intensity. This quenching is strongly dependent on the concentration of the TrpAgNPs, and it is caused by a combination of a static and a dynamic process. The chemical binding leads to oxidation of tryptophan and formation of kynurenine, observed in the emission spectra around 470 nm. The strong reduction of the PPIX fluorescence decay lifetime with nanoparticle increasing concentration confirms the quenching processes due to charge transfer from the excited PPIX states to the resonant silver states. The present study confirms the anticancer activity of TrpAgNPs on the human breast cancer cell line (MCF-7) in vitro and indicates that PPIX-AgNP interaction could contribute with MCF-7 apoptosis.

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Graphical abstract Interaction between TrpAgNPs and PPIX

     

On log-hyponormal operators

LetTB(H) be a bounded linear operator on a complex Hilbert spaceH.TB(H) is called a log-hyponormal operator itT is invertible and log (TT ^*)log (T ^* T). Since log: (0, )(–,) is operator monotone, for 0<p1, every invertiblep-hyponormal operatorT, i.e., (TT ^*) ^p (T ^* T) ^p , is log-hyponormal. LetT be a log-hyponormal operator with a polar decompositionT=U|T|. In this paper, we show that the Aluthge transform is . Moreover, ifmeas ((T))=0, thenT is normal. Also, we make a log-hyponormal operator which is notp-hyponormal for any 0<p.This research was supported by Grant-in-Aid Research No. 10640185