Determination of Flavonoid Markers in Honey with SPE and LC using Experimental Design

Determination of flavonoid markers quercetin, hesperetin, and chrysin, found in north Iranian citrus honey samples, was carried out by solid phase extraction (SPE) and isocratic liquid chromatographic separation using central composite design. Optimum conditions for SPE were achieved using 10 mL methanol/water (13:87, v/v, pH = 7) as the washing solvent and 4 mL methanol for elution. Good clean-up and high recovery >90% were observed for all analytes. The use of water/ACN/THF/AcOH (54:36:5:5, v/v) was found to serve as the optimum mobile phase composition and allowed for the separation of analytes from endogenous compounds present in honey. SPE parameters, such as maximum loading capacity and breakthrough volume, were also determined for each analyte. Limit of detection, linear range, recovery, repeatability of retention times, and peak heights were 3.11 × 10⁻⁸–4.44 × 10⁻⁸ g g⁻¹, 0.50–50.0 μg mL⁻¹ (R ² > 0.99), 90.7–96.9%, 3.0–3.6%, and 1.0–2.6%, respectively. Precision of the overall analytical procedure, estimated by five replicate measurements for quercetin, hesperetin and chrysin in citrus honey, as well as the relative standard deviations were 4.3%, 3.8%, and 5.5%, respectively.

     

Microwave Assisted Synthesis of 4-Substituted 1-Ethoxycarbonyl Semicarbazides from Ethyl Carbazate and Isocyanates

Summary.  A rapid and simple method for the preparation of 4-substituted 1-ethoxycarbonyl semicarbazide is reported. The reaction is carried out under microwave irradiation by the reaction of five different isocyanates with ethyl carbazate. Corresponding author. E-mail: mallak@cc.iut.ac.ir Previous name. Shadpour E. Mallakpour Received October 28, 2002; accepted October 31, 2002 Published online May 15, 2003     

Preparation of magnetic latexes functionalized with chloromethyl groups via emulsifier-free miniemulsion polymerization

Functionalized crosslinked polystyrene-co-divinylbenzene-co-chloromethylstyrene magnetic latex particles were prepared via emulsifier-free miniemulsion polymerization using 2, 2′ azobis (2-amidinopropane) dihydrochloride (V-50) as an initiator and in the presence of magnetite nanoparticles in the monomers. Transmission electron microscopy (TEM) proved the presence of magnetite nanoparticles in polymer particles. Differential scanning calorimetery (DSC) analysis of the product showed an exothermic signal due to crosslinking of chains through electrophilic aromatic substitution of phenyl groups with chloromethyl groups in the presence of the dispersed Fe₃O₄ as Lewis acid. This was proven by thermogravimetric analysis (TGA) via the loss of gaseous HCl. The results were also compared with those of magnetite-free miniemulsion polymerization using V-50.     

Sub-Second Accumulation and Stripping for Pico-Level Monitoring of Amikacin Sulphate by Fast Fourier Transform Cyclic Voltammetry at a Gold Microelectrode in Flow-Injection Systems

A novel chemiluminogenic reagent, refered to as spiro form fluorescein hydrazide, was synthesized, and its application to chemiluminescence (CL) determination of Co²⁺ is described. The method is based on the catalytic effect of Co²⁺ on the autoxidation of sulfite in basic solution to generate a series of powerful oxidative intermediates, which then oxidize colorless, nonfluoresent fluorescein hydrazide to generate strong CL emission. The CL signal is linearly related to the concentration of Co²⁺ in the range of 0.1–200nM with a detection limit of 0.04nM. The optimal conditions for the detection of Co²⁺ were evaluated, and the possible CL mechanism is discussed. The proposed method has been applied to the determination of Co²⁺ in pharmaceutical preparations and in soil samples.     

High-throughput capillary electrophoresis for the identification and differentiation of seven species of Eimeria from chickens

A capillary electrophoretic approach has been evaluated for the identification of seven currently recognised species of Eimeria infecting chickens. The second internal transcribed spacer of ribosomal DNA is PCR-amplified from any of the seven species using a single set of oligonucleotide primers (one of which is fluorescently labelled). The amplicons are heat-denatured and subjected to capillary electrophoresis in a MegaBACE 1000 (Amersham). The chromatograms captured are stored electronically and then analysed using MegaBACE Fragment Profiler software. Using control DNA samples representing monospecific lines of Eimeria, specific peaks in the chromatograms were defined for the unequivocal identification of each of the seven species and their differentiation. Electrophoretic reading and analysis are carried out automatically, thus making it a time- and cost-effective method. This procedure should find applicability as a tool for the quality control of Eimeria vaccines, the monitoring of coccidiosis outbreaks and the high-throughput analysis of oocyst samples for epidemiological surveys.     

Polarization-insensitive cross correlation using two-photon absorption in a silicon photodiode

We present experimental measurements of the polarization dependence of two-photon absorption in silicon photodiodes at 1550 nm, and we offer a simple theory that explains our observations. Based on this theory, we propose and demonstrate that it is possible to construct an optical cross-correlation system that is polarization insensitive, provided that one of the two input polarization states can be controlled.     

Kinetics study of a Diels‐Alder reaction in mixtures of an ionic liquid with molecular solvents

The second‐order rate constants for cycloaddition reaction of cyclopentadiene with naphthoquinone were determined spectrophotometrically in various compositions of 1‐(1‐butyl)‐3‐methylimidazolium terafluoroborate ([bmim]BF₄) with water and methanol at 25 °C. Rate constants of the reaction in pure solvents are in the order of water > [bmim]BF₄ > methanol. Rate constants of the reaction decrease sharply with mole fraction of the ionic liquid in aqueous solutions and increase slightly to a maximum in alcoholic mixtures. Multi‐parameter correlation of logk₂ versus solute–solvent interaction parameters demonstrated that solvophobicity parameter (Sp), hydrogen‐bond donor acidity (α) and hydrogen‐bond acceptor basicity (β) of media are the main factors influencing the reaction rate constant. The proposed three‐parameter model shows that the reaction rate constant increases with Sp, α and β parameters. Copyright © 2008 John Wiley & Sons, Ltd.     

Some Properties of Isologism of Groups and Baer-Invariants

Let be a variety of groups defined by the set of laws V. In this paper we study the concept of -isologism of groups in terms of -extensions and their connections with the Baer-invariant of groups are also discussed.AMS Subject Classification (2000): primary 20F14, 20F19, secondary 20E10     

Novel PVC-based copper(II) membrane sensor based on 2-(1'-(4'-(1'-hydroxy-2'-naphthyl)methyleneamino)butyl iminomethyl)-1-naphthol.

A copper(II) ion-selective PVC membrane sensor based on 2-(1'-(4'-(1'-hydroxy-2'-naphthyl)methyleneamino)butyl iminomethyl)-1-naphthol (BHNB) as a novel Schiff base containing a sensing material has been successfully developed. The sensor exhibits a good linear response of 29 mV per decade within the concentration range of 10(-1)-10(-6) M of Cu2+. The sensor shows good selectivity for copper(II) ion in comparison with alkali, alkaline earth, transition and heavy metal ions. The BHNB-based sensor is suitable for use with aqueous solutions of pH 3.5-7.0 and displays minimal interference by Sr(II), Cd(II), Hg(II), Zn(II) and Pb(II), which are known to interfere with other previously suggested electrodes. The proposed membrane electrode was used as a sensor for determining the Cu(II) content in black tea samples. It was also applied as an indicator electrode in the potentiometric titration of Cu2+ ions with EDTA.