Comparison of extraction techniques of robenidine from poultry feed samples

In this paper, effectiveness of six different commonly applied extraction techniques for the determination of robenidine in poultry feed has been compared. The sample preparation techniques included shaking, Soxhlet, Soxtec, ultrasonically assisted extraction, microwave – assisted extraction and accelerated solvent extraction. Comparison of these techniques was done with respect to the recovery extraction, temperature and time, reproducibility and solvent consumption. Every single extract was subjected to clean – up using aluminium oxide column (Pasteur pipette filled with 1 g of aluminium oxide), from which robenidine was eluted with 10 ml of methanol. The eluate from the clean-up column was collected in a volumetric flask, and finally it was analysed by HPLC–DAD–MS. In general, all extraction techniques were capable of isolating of robenidine from poultry feed, but the recovery obtained using modern extraction techniques was higher than that obtained using conventional techniques.

In particular, accelerated solvent extraction was more superior to other techniques, which highlights the advantages of this sample preparation technique. However, in routine analysis, shaking and ultrasonically assisted extraction is still the preferred method for the solution of robenidine and other coccidiostatics.     

A new calcium 2,5-dihydroxybenzoate: Synthesis,characterization and antioxidant studies and stress mediated cytotoxity in MCF-7 cells

The structure and composition of the calcium 2,5-dihydroxybenzoate (calcium gentisate) were studied by single-crystal and powder X-ray diffraction. Single-crystal X-ray analysis revealed that the compound crystallizes in the orthorhombic space group Pbcn. The Ca(II) cation is coordinated in a monodentate fashion by two symmetry-related gentisate anions and five water molecules. The metal ion and one of the water molecules are located on a 2-fold rotation axis. The adjacent monomeric units are assembled into a 3-D supramolecular framework via O–H…O hydrogen bonds. Comparison of the experimental powder pattern with that simulated from single-crystal X-ray data confirmed the purity and homogeneity of the sample. The FT-IR, UV/VIS, ¹H and ¹³C NMR spectra of the calcium 2,5-dihydroxybenzoic acid were registered and analysed. Moreover the effect of calcium complex and 2,5-dihydroxybenzoic acid on basic oxidative stress parameters, such as thiol group content and lipid peroxidation in the human breast cancer cells MCF-7 was studied. The antiradical and ferric reducing power of these compounds was measured by DPPH, CUPRAC and FRAP methods. The chemical reactivity parameters (e.g. HOMO and LUMO orbitals, ionization potential, electron affinity) for Ca 2,5-dHB and 2,5-dHB were calculated at B3LYP/6-311++G7 level of theory and discussed in relation to their antioxidant properties.     

Physical and Sensory Properties of Japanese Quince Chips Obtained by Osmotic Dehydration in Fruit Juice Concentrates and Hybrid Drying

Japanese quince has high health value, but due to its taste and texture, it is difficult to eat raw. The use of innovative drying methods to produce dried snack foods from these fruits may be of interest to producers and consumers. The physicochemical and sensory properties of 3 mm slices of Japanese quince fruit (with skin, without seeds) obtained by osmotic pre-treatment in chokeberry and apple juice concentrates, and with the use of convection (convective drying, C-D), freeze-drying (F-D), and convection-microwave-vacuum drying (hybrid) are assessed. The methods of drying osmo-dehydrated slices do not affect the dry matter content. In most dried quince, the water activity is 0.40 or lower. Pre-osmotic dehydration and drying have a significant impact on the mechanical and acoustic properties of quince chips. Sensory attractive chips emit loud acoustic emission (AE) during the breaking test. Chips that are osmo-dehydrated in a mixture of chokeberry juice concentrate and sucrose and dried by a hybrid method are attractive. They have a dark red color given by chokeberry concentrate and a slight sweet (with a slight sour-bitter) taste. The sensory evaluation was useful for determining the quality of the chips in terms of their texture (crispness) tested by mechanical methods. Their sensory ratings (overall desirability as weight of color, taste, crispness, and flavor) are high and similar (from 3.8 to 4.1). The use of innovative drying methods with pre-osmotic treatment allows obtaining dried material with properties comparable to those obtained by the F-D method, but in a much shorter time, i.e., with lower energy and using a simple method.     

Synthesis and spectroscopic characterisation of (E)-2-(2-(9-(4-(1H-1,2,4-triazol-1-yl)butyl)-9H-carbazol-3-yl)vinyl)-3-ethylbenzo[d]thiazol-3-ium, a new ligand and potential DNA intercalator

Three new compounds based on carbazole planar skeleton were synthesised. Among them there is a new ligand and a potential DNA intercalator which contains a benzothiazolium moiety connected to the carbazole ring by a vinyl bridge. The absorption and emission spectral properties of this new ligand have been studied by spectroscopic methods.     

LC and Principal Component Analysis in the Lipophilicity Study of Seven Angiotensin II-AT1 Receptor Antagonists (Sartans)

Seven sartans have been chromatographed with acetonitrile-buffer and methanol–buffer in different proportions as mobile phases. The retention values, log k or R _M were extrapolated to zero organic modifier content to obtain the log k _w or R _MW values. Calibration equations were obtained for standards of known lipophilicity. A simple method employing a gradient procedure of 10–100% acetonitrile or methanol in 60 min and standards of the extreme lipophilicity was also elaborated. Chromatographic log P values were compared to those calculated by use of different software products. Finally, principal component analysis was performed to explore and visualize similarities and differences among the drugs and among the methods.

     

Detection and Visualization Methods Used in Thin-Layer Chromatography

JPC – Journal of Planar Chromatography – Modern TLC - The use of thin-layer chromatography (TLC) for separation, identification and quantification of different organic and inorganic...     

Substantial Influence of Temperature on Anchoring of Gold‐Nanoparticle Monolayer for Performance of DNA Biosensors

This paper presents a way of modification of crystalline gold surface with a high quality layer of gold nanoparticles (Au NPs) via self‐assembled dithiol. The application of additional Au NPs monolayer prepared at various temperatures was tested with three types of biosensors previously described in the literature. The examined DNA biosensors differed by the detection method and the way of the immobilization of DNA probe at the modified gold electrode surface. For the immobilization of DNA probe in the sensing layer either the formation of SAM or the affinity binding (biotin – sterptavidin) or covalent attachment were used. The necessary condition of successful preparation of a perfect such monolayer is the preparation temperature of 4 °C. The preparation of Au NPs layers at higher than 4 °C temperatures leads to poor repeatability and unsatisfactory precision of the measurements. The application of the perfect Au monolayer lowers the detection limit (circa by 10 to 100 times) for all tested DNA biosensors.     

May thermal imaging be useful in the assessment of dental anaesthesia? Preliminary study

Journal of Thermal Analysis and Calorimetry - The main goal of this study was to find out if thermal imaging may be useful in the evaluation of two types of anaesthetic injections—with and...     

Surface‐enhanced resonance Raman spectroscopic characterization of cytochrome c immobilized on 2‐mercaptoethanesulfonate monolayers on silver

Single‐component self‐assembled monolayers (SAMs) of mercaptoethanesulfonate (MES) on Ag surfaces were studied with surface‐enhanced resonance Raman scattering (SERRS) spectroscopy with a view to their application to immobilize (ferro)cytochrome c (cyt c). SERS studies revealed that MES molecules adopt primarily trans (T) conformation even at early stages of the SAM growth and over wide range of pH values. High accessibility of the negatively charged groups for (bio)molecules in solution makes single‐component MES SAMs suitable linkage monolayers for electrostatic attachment of cyt c, which was verified with SERRS. Cyt c was successfully anchored to MES‐coated Ag at natural (∼5), neutral, and isoelectric point (10.6) pH. At pH = 7.0 and 10.6, SERRS bands characteristic of native six‐coordinated low‐spin (6cLS) heme iron configuration were detected. Lack of buffering resulted in additional appearance of five‐coordinated high‐spin (5cHS) SERRS markers and the presence of bands indicating ferric ion. An electrostatic attraction between protein and SAM was confirmed to exclude the hydrophobic interactions involved in cyt c binding. Cyt c attached to MES SAM on Ag was found to be electroactive at neutral pH, and protein oxidation was assisted with reversible conversion of 6cLS to the non‐native 5cHS state. Alteration of heme orientation deduced from SERRS spectra upon change of redox state allowed us to propose the protein dynamics as the electron transfer rate‐limiting step. Copyright © 2010 John Wiley & Sons, Ltd.