Identification of four cornua by ultra‐performance liquid chromatography with time‐of‐flight mass spectrometry coupled with principal component analysis

An ultra‐high performance liquid chromatography with quadrupole time‐of‐flight mass spectrometry method coupled with principal component analysis was developed and applied to the identification of Cornu Antelopis, Cornu Bubali, Cornu Naemorhedi, and Cornu Bovis. The data obtained from the trypsin‐digested samples were subjected to principal component analysis to classify these four cornua. Additionally, marker peptides of the cornua were determined by orthogonal partial least‐squares discriminant analysis, and fragmentation tandem mass spectra of these marker peptides were evaluated. The results from this study indicate that the proposed method is reliable, and it has been successfully applied to the identification of variants of cornua commonly used in traditional Chinese medicine.     

Synthesis and mesomorphism of 2,5-bis(3,4-bis(n-alkoxy)phenyl)thiazolo[5,4-d]thiazole tetracatenar liquid crystals

A series of new symmetrical 2,5-bis(3,4-bis(n-alkoxy)phenyl)thiazolo[5,4-d]thiazoles (TTn) prepared via condensation of dithiooxamide with six different 3,4-di-n-alkoxybenzaldehydes were characterized by ¹H NMR, FTIR, UV-Vis, and photoluminescence spectroscopy. Moreover, one compound lack of aliphatic chains, i.e., 2,5-diphenylthiazolo[5,4-d]thiazole (TT) was synthesized and characterized. The investigated TTn compounds emitted blue light. The effect of length of n-alkoxy (i.e., OC _n H_{2 n +1}, n?=?8, 10, 12, 14, 16, and 18) peripheral groups on thermal and mesomorphic behavior was investigated by means of differential scanning calorimetry, polarizing optical microscopy, and X-ray diffraction. Variable heating and cooling rates were used to study the liquid-crystalline properties of TTn. All compounds exhibited liquid-crystalline properties which self-organize into one or two smectic mesophases (SmB and SmE).     

Synthesis and mesomorphism of ionic self-assembled complexes of anthraquinones

Anthraquinones are known to exhibit mesomorphism upon appropriate substitutions. In this report, the concept of ionic self-assembly has been applied to design and synthesise new anthraquinone-based liquid crystals. Four different anthraquinones were used as polyelectrolytes which form ionic complexes with double-tail ammonium surfactants. The chemical structures were characterised by spectral techniques and elemental analysis. The thermal behaviour of the complexes was investigated by polarising optical microscopy, differential scanning calorimetry, thermogravimetric analysis and X-ray diffraction studies. All these complexes display lamellar mesomorphism. The amphotropic nature of the complexes has also been studied.     

Oxide reduced silicon nanowires

Core crystalline silicon nanowires with a heavily reduced amorphous shell have been successfully synthesised using palladium as a metal catalyst. We present two approaches to reduce the oxidation of the nanowires during the thermal annealing growth. The ratios of the amorphous shell to crystalline core of the nanowires produced, from the two methods, are compared and show a remarkable drop (hence thinner oxide) compared to wires fabricated using currently available techniques. In addition, a focused ion beam was utilised to contact the oxide-reduced nanowires for transport measurements, without first removing the thin oxide shell. The oxygen-reduced core-shell silicon nanowires showed a very low electrical resistivity (4 × 10⁻¹ Ω cm). Our novel approach presents a new alternative to the production of low cost, high yield, highly conducting silicon nanowires offering a wide range of opportunities for semiconductor based technology.     

Simultaneous determination of residues of metalaxyl,cyazofamid and a cyazofamid metabolite in tobacco leaves and soil by liquid chromatography with tandem mass spectrometry

A simple method was developed and validated for the simultaneous determination of metalaxyl, cyazofamid and the cyazofamid metabolite 4‐chloro‐5‐p‐tolylimidazole‐2‐carbonitrile (CCIM) by liquid chromatography with tandem mass spectrometry. The three target compounds were extracted from tobacco and soil with acetonitrile containing 0.1% acetic acid, and the extracts were purified using octadecylsilane. The proposed method showed satisfactory linearity (R² ≥ 0.9985) for the target compounds. The limits of detection for metalaxyl, cyazofamid and CCIM were 0.006, 0.06 and 0.06 mg/kg in soil and green tobacco leaves and 0.03, 0.3 and 0.3 mg/kg in cured tobacco leaves, respectively. The limits of quantification for metalaxyl, cyazofamid and CCIM were 0.02, 0.2 and 0.2 mg/kg in soil and green tobacco leaves and 0.1, 1 and 1 mg/kg in cured tobacco leaves, respectively. The average recoveries from soil and tobacco were 72.91–98.40% for metalaxyl, 76.73–105.80% for cyazofamid and 74.48–106.45% for CCIM. The relative standard deviation range was 1.23–6.99%. The developed method was successfully applied to analysis of residues of metalaxyl, cyazofamid and CCIM in real soil and tobacco samples. The results indicated that the established method could meet the requirement for the analysis of trace amounts of all three analytes in soil and tobacco.     

Simultaneous quantification of atenolol and chlorthalidone in human plasma by ultra‐performance liquid chromatography–tandem mass spectrometry

A simple, sensitive and reproducible ultra‐performance liquid chromatography–tandem mass spectrometry method has been developed for the simultaneous determination of atenolol, a β‐adrenergic receptor‐blocker and chlorthalidone, a monosulfonamyl diuretic in human plasma, using atenolol‐d7 and chlorthalidone‐d4 as the internal standards (ISs). Following solid‐phase extraction on Phenomenex Strata‐X cartridges using 100 μL human plasma sample, the analytes and ISs were separated on an Acquity UPLC BEH C₁₈ (50 mm × 2.1 mm, 1.7 µm) column using a mobile phase consisting of 0.1% formic acid–acetonitrile (25:75, v/v). A tandem mass spectrometer equipped with electrospray ionization was used as a detector in the positive ionization mode for both analytes. The linear concentration range was established as 0.50–500 ng/mL for atenolol and 0.25–150 ng/mL for chlorthalidone. Extraction recoveries were within 95–103% and ion suppression/enhancement, expressed as IS‐normalized matrix factors, ranged from 0.95 to 1.06 for both the analytes. Intra‐batch and inter‐batch precision (CV) and accuracy values were 2.37–5.91 and 96.1–103.2%, respectively. Stability of analytes in plasma was evaluated under different conditions, such as bench‐top, freeze–thaw, dry and wet extract and long‐term. The developed method was superior to the existing methods for the simultaneous determination of atenolol and chlorthalidone in human plasma with respect to the sensitivity, chromatographic analysis time and plasma volume for processing. Further, it was successfully applied to support a bioequivalence study of 50 mg atenolol + 12.5 mg chlorthalidone in 28 healthy Indian subjects. Copyright © 2015 John Wiley & Sons, Ltd.     

Bixin extraction from defatted annatto seeds

Bixin is the major carotenoid in the seed of the Annatto plant (Bixa orellana L.). The aim of this study was to obtain extracts containing bixin from seeds that had been partially defatted by supercritical fluid extraction. Pressurized liquid extraction (PLE) and low-pressure solvent extraction (LPSE) methods were used, and the effects of the solvent, temperature, pressure, solvent mass to feed mass (S/F) ratio and ultrasonication were evaluated for the global yield (X₀(%)) and the bixin yield (BY(%)). Extraction conditions producing high yields of bixin were established for both the PLE and LPSE methods. Analysis of variance was used to examine the influence of the individual extraction variables in LPSE and PLE. For LPSE; significant effects were found for solvent, temperature, and the interactions of temperature with solvent and temperature with S/F. Solvent was the only variable that significantly affected X₀(%) and BY(%), for PLE. While ultrasonication did not significantly affect X₀(%) or BY(%), scanning electron microscopy analysis revealed structural changes in the vegetal matrix following this treatment.     

Simultaneous analysis of bisphenol A based compounds and other monomers leaching from resin‐based dental materials by UHPLC–MS/MS

Resin‐based dental materials have raised debates concerning their safety and biocompatibility, resulting in a growing necessity of profound knowledge on the quantity of released compounds into the oral cavity. In this context, the aim of this study was to develop a comprehensive and reliable procedure based on liquid chromatography with mass spectrometry for the simultaneous analysis of various leached compounds (including bisphenol A based compounds) in samples from in vitro experiments. Different experiments were performed to determine the optimal analytical parameters, comprising mass spectrometry parameters, chromatographic separation conditions, and sample preparation. Four internal standards were used as follows: deuterated diethyl phthalate and bisphenol A (commercially available), and deuterated analogues of triethylene glycol dimethacrylate and urethane dimethacrylate (custom‐made). The optimized method was validated for linearity of the calibration curves and the associated correlation coefficient, lower limit of quantification, higher limit of quantification, and intra‐ and interassay accuracy and precision. Additionally, the developed liquid chromatography with tandem mass spectrometry method was applied to the analysis of leaching compounds from four resin‐based dental materials. The results indicated that this method is suitable for the analysis of different target compounds leaching from dental materials. This method might serve as a valuable basis for quick and accurate quantification of leached compounds from resin‐based dental materials in biological samples.     

An anti‐diffusive volume of fluid method for interfacial fluid flows

A volume of fluid (VOF) method is developed combining a first‐order limited downwind scheme with higher order accurate schemes. The method is characterized by retaining a sharp fluid interface and a reduction in numerical diffusion near the interface, but avoids complicated geometrical reconstruction as occurs in most volume tracing algorithms. To demonstrate the accuracy and robustness of the method, a selection of numerical experiments are presented involving a pure advection problem, a water wave impact caused by a dam breaking and liquid sloshing in a partially filled tank. Copyright © 2011 John Wiley & Sons, Ltd.