LC Method for Studies on the Stability of Sibutramine in Soft Gelatin Capsules

A sensitive and rapid liquid chromatographic method was successfully developed and validated for the determination of sibutramine hydrochloride in bulk and capsules. Sibutramine in the presence of its degradation products was analyzed using UV detection at 225 nm. Chromatography was performed on a reversed-phase C₈ (150 × 4.0 mm I.D., 5 μm) analytical column under isocratic conditions. The mobile phase was composed of acetonitrile:water (aqueous phase containing 0.3% triethylamine and pH adjusted to 7.0) (75:25, v/v) at a flow-rate of 1.1 mL min⁻¹. No chromatographic interference was found during the analysis. Light was the stress condition which most contributed to sibutramine degradation. The method showed a linear response (r > 0.999) from 30 to 90 μg mL⁻¹. The mean recovery for capsules was 101.2%. Inter-day assays showed relative standard deviations of 0.42 and 1.62% for bulk and capsules, respectively. The developed method is able to separate sibutramine from its major degradation products and it may be used in the quality control of this active pharmaceutical ingredient in both bulk and capsules.     

Silica-encapsulated CdTe/MPA quantum dots: microstructural,thermal, and chemical stability characterization

In this paper, we describe the synthesis of silica-encapsulated CdTe/MPA quantum dot (QD) nanocomposites (CdTe/MPA@SiO₂) at room temperature starting from water-soluble CdTe QDs capped with 3-mercaptopropionic acid (MPA) as surface ligand (CdTe/MPA), followed by their encapsulation with a thin layer of silica using the sol–gel process. The objective of this work was to evaluate the microstructural, thermal, and chemical properties of the encapsulated material as a way to evaluate these characteristics for possible applications in different technological areas. Transmission electron microscopy results proved that CdTe QDs (2.5 nm in size) were inside the SiO₂ nanoparticles, and the spherical CdTe/MPA@SiO₂ nanocomposite with a 69-nm thick shell. The photoluminescence intensity was evaluated as a function of pH in the range of 2–12. The CdTe/MPA@SiO₂ nanocomposite showed better chemical stability and greater intensity of photoluminescence in the pH 2–12 range than CdTe/MPA. In addition, the CdTe/MPA@SiO₂ nanocomposites showed good heat stability up to 125 °C. The changes in their optical properties were also evaluated by means of photoluminescence spectroscopy. The materials were also characterized by diffuse reflectance spectroscopy, X-ray diffraction, infrared spectroscopy, and thermogravimetric analysis.

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2,2′-Bipyridine-6,6′-bis(carbothioamide) metal complexes

Complexes of 2,2-bipyridine-6,6-bis(carbothioamide), obtained with a variety of metal cations, were characterised by microanalyses, molar conductivities and by i.r. and n.m.r. (for diamagnetic compounds) spectra. The iron(II) complex was also characterised by Mössbauer spectroscopy. The spectral data indicate that, in all cases, the ligand coordinates to the metal through one pyridine nitrogen and one sulphur.     

Development of low-cost planar electrodes and microfluidic channels for applications in capacitively coupled contactless conductivity detection (C4D)

Electrochemical techniques are commonly applied to micro total analysis system (μTAS) devices mainly due to its high sensitivity and miniaturization capacity. Among many electrochemical techniques, capacitively coupled contactless conductivity detection (C⁴D) stands out for not requiring direct electrode-solution contact, avoiding several problems such as electrolysis, bubble formation, and metal degradation. Furthermore, the instrumentation required for C⁴D measurements is compact, low cost, and easy to use, allowing in situ measurements to be performed even by nonspecialized personal. Contrarily, the production of metallic electrodes and microchannels adequate for C⁴D measurements commonly requires specialized facilities and workers, increasing the costs of applying these methods. We propose alternatives to batch manufacture metallic electrodes and polymeric microchannels for C⁴D analysis using more straightforward equipment and lower-cost materials. Three devices with different dielectric layer compositions and electrode sizes were tested and compared regarding their analytical performance. The constructed platforms have shown a reduction of more than 64% in cost when compared to traditional techniques and displayed good linearity (R² ≥ 0.994), reproducibility (RSD ≤ 4.07%, n = 3), and limits of detection (≤0.26 mmol/L) when measuring standard NaCl samples. Therefore, the proposed methods were successfully validated and are available for further C⁴D applications such as diagnosis of dry-eye syndrome.     

Verification of the selectivity of a liquid chromatography method for determination of stilbenes and flavonols in red wines by mass spectrometry

Quantification of bioactive phenols, like stilbenes and flavonols (SaF), has been conducted to evaluate the nutraceutical potential of red wines. However, there is still a lack of full validated, fast and accessible liquid chromatography methods offering high selectivity and a simple procedure. We present here the use of a high-resolution mass spectrometer to evaluate the selectivity of a feasible and traditional liquid chromatography technique (HPLC–DAD) to analyze markers of aglycone SaF in red wines. The SaF compounds were tested: trans-resveratrol, trans-ε-viniferin, quercetin, myricetin, and kaempferol, as well as trans-cinnamic acid, one of their precursors. System suitability and validation tests were employed for the selected conditions (octylsilane column, methanol mobile phase, and gradient elution). The validation process ensured the HPLC–DAD method was selective, linear, sensitive, precise, accurate and robust. The method was then applied to red wine samples from the Campanha Gaúcha region, Southern Brazil. The real samples contained different SaF levels, showing that the method is applicable to routine use. Furthermore, this was the first SaF characterization of red wines from the Campanha Gaúcha, contributing to regional and product development.     

Determination of tetrakis(hydroxymethyl)phosphonium sulfate in commercial formulations and cooling water by capillary electrophoresis with contactless conductivity detection

A novel capillary electrophoresis method using capacitively coupled contactless conductivity detection is proposed for the determination of the biocide tetrakis(hydroxymethyl)phosphonium sulfate. The feasibility of the electrophoretic separation of this biocide was attributed to the formation of an anionic complex between the biocide and borate ions in the background electrolyte. Evidence of this complex formation was provided by ¹¹B NMR spectroscopy. A linear relationship (R² = 0.9990) between the peak area of the complex and the biocide concentration (50–900 μmol/L) was found. The limit of detection and limit of quantification were 15.0 and 50.1 μmol/L, respectively. The proposed method was applied to the determination of tetrakis(hydroxymethyl)phosphonium sulfate in commercial formulations, and the results were in good agreement with those obtained by the standard iodometric titration method. The method was also evaluated for the analysis of tap water and cooling water samples treated with the biocide. The results of the recovery tests at three concentration levels (300, 400, and 600 μmol/L) varied from 75 to 99%, with a relative standard deviation no higher than 9%.     

电子光学系统质量的模糊二级综合评判

采用模糊二级综合评判来比较不同屏面位置时的电子光学系统的质量,从而找到一个最佳的屏面位置。     

Different approaches for fabrication of low-cost electrochemical sensors

Electrochemistry combined with economical and sustainable platforms (such as paper) provides portable, affordable, robust, and user-friendly devices. In general, techniques, such as photolithography and sputtering, are excellent alternatives for producing these platforms. However, owing to the requirement of expensive and sophisticated instrumentation, as well as cleanroom facilities, these techniques have limited access. Thus, the search for easy to use and produce approaches have been reported, using consumables, including adhesives, carbon ink, graphite, pencil, office paper, paperboard, among others. In this sense, in this mini-review, we discuss various strategies explored to fabricate low-cost electrochemical sensors, including its main applications. Different manufacturing methods, such as screen and stencil printing, laser-scribing, and pencil drawing, will be discussed here, emphasizing the performance of the obtained devices, in addition to their advantages and disadvantages.     

Ruthenium(II) complexes of 2-benzoylpyridine-derived thiosemicarbazones with cytotoxic activity against human tumor cell lines

Reaction of [RuCl(3)(dppb)H(2)O] (dppb=1,4 bis(diphenylphospine)butane) with 2-benzoylpyridine thiosemicarbazone (H2Bz4DH) and its N(4)-methyl (H2Bz4M) and N(4)-phehyl (H2Bz4Ph) derivatives gave [RuCl(dppb)(H2Bz4DH)]Cl (1), [RuCl(dppb)(H2Bz4M)]Cl (2) and [RuCl(dppb)(H2Bz4Ph)]Cl (3). The cytotoxic activity of the studied compounds was tested against the MCF-7, TK-10 and UACC-62 human tumor cell lines. The precursor [RuCl(3)(dppb)H(2)O] exhibits cytocidal activity against the tree cell lines. H2BzDH, H2Bz4M, and [RuCl(dppb)(H2Bz4M)]Cl (2) show a selective cytocidal effect against the UACC-62 cell line which makes them the most promising compounds.