Determination of quinocide as impurity in primaquine tablets by capillary zone electrophoresis

A capillary zone electrophoretic method has been developed and validated for the determination of the impurity quinocide (QC) in the antimalarial drug primaquine (PQ). Different buffer additives such as native cyclodextrins and crown ethers were evaluated. Promising results were obtained when either β‐cyclodextrin (β‐CD) or 18‐crown‐6 ether (18C6) were used. Their separation conditions such as type of buffer and its pH, buffer additive concentration, applied voltage capillary temperature and injection time were optimized. The use of 18C6 offers slight advantages over β‐CD such as faster elution times and improved resolution. Nevertheless, migration times of less than 5 min and resolution factors (R_s) in the range of 2–4 were obtained when both additives were used. The method was validated with respect to selectivity, linearity, limits of detection and quantitation, analytical precision (intra‐ and inter‐day variability) and repeatability. Concentrations of 2.12 and 2.71% (w/w) of QC were found in pharmaceutical preparations of PQ from two different manufacturers. A possible mechanism for the successful separation of the isomers is also discussed. Copyright © 2008 John Wiley & Sons, Ltd.     

Application of continual injection liquid‐phase microextraction method coupled with liquid chromatography to the analysis of organophosphorus pesticides

A liquid‐phase microextraction coupled with LC method has been developed for the determination of organophosphorus pesticides (methidation, quinalphos and profenofos) in drinking water samples. In this method, a small amount (3 μL) of isooctane as the acceptor phase was introduced continually to fill‐up the channel of a 1.5 cm polypropylene hollow fiber using a microsyringe while the hollow fiber was immersed in an aqueous donor solution. A portion of the acceptor phase (ca. 0.4 μL) was first introduced into the hollow fiber and additional amounts (ca. 0.2 μL) of the acceptor phase were introduced to replenish at intervals of 3 min until set end of extraction (40 min). After extraction, the acceptor phase was withdrawn and transferred into a 2 mL vial for a drying step prior to injection into a LC system. Parameters that affect the extraction efficiency were studied including the organic solvent, length of fiber, volume of acceptor and donor phase, stirring rate, extraction time, and effect of salting out. The proposed method provided good enrichment factors of up to 189.50, with RSD ranging from 0.10 to 0.29%, analyte recoveries of over 79.80% and good linearity ranging from 10.0 to 1.25 mg/L. The LOD ranged from 2.86 to 82.66 μg/L. This method was applied successfully to the determination of organophosphorus pesticides in selected drinking water samples.     

A mixed-valent ruthenium-oxo oxalato cluster Na7[Ru4(mu3-O)4(C2O4)6] with potent anti-HIV activities

A structurally characterized mixed-valent tetranuclear ruthenium-oxo oxalato cluster exhibits anti-viral activities toward R5- and X4-tropic HIV-1, and possesses cytoprotective activity toward HIV-1 infected cells.     

Directed self-assembly of gold-tipped CdSe nanorods

Gold-tipped CdSe rods (nanodumbbells) were solubilized in an aqueous phase and self-assembled in a head-to-tail manner using biotin disulfide and avidin. The disulfide end of the biotin molecule attaches to the gold tip of the nanodumbbell, and the biotin end of the molecule is able to conjugate to an avidin protein. The avidin can strongly conjugate up to four biotin molecules. Changing the ratios of biotin to nanodumbbells leads to the formation of dimers, trimers, and flowerlike structures. To further improve the distribution of chain lengths, a separation method based upon weight was applied using a concentration gradient. The gold tips provide effective anchor points for constructing complex nanorod structures by self-assembly.     

Sorption of azo dyes from aqueous solutions by tetradodecyloxybenzylcalix[4]resorcinarene derivatives

Four water-insoluble tetradodecyloxybenzylcalix[4]resorcinarenes with various functional groups at the upper macrocycle rim (unsubstituted calix[4]resorcinarene 1, carboxylic acid derivative 2, ethyl ester derivative 3 and aminoethylamide derivative 4) were synthesized and tested as sorbents for water-soluble azo dyes methyl orange (MO), acid orange 5 (AO 5) and congo red (CR) by solid–liquid extraction method without background electrolyte. It was observed that the sorption of azo dyes reaches 99% for sorbent 4, which is partial protonated in contact with water and becomes able to electrostatic interactions with the dyes. It was demonstrates that calixresorcinarene 4 has the excellent sorption capacity for AO5 (130.5?mg dye per g of sorbent) due to effective calixresorcinarene—dye association in equal molar ratio mode.     

Surface modification. I. Polyacrolein microspheres covalently bonded onto polyethylene

The synthesis and characterization of novel surfaces composed of polyacrolein microspheres covalently bonded onto polyethylene films are described. These surfaces were prepared through a sequence of reactions carried out onto polyethylene films in order to form primary amine groups at the w position. Polyacrolein microspheres in water were then covalently bonded to these modified polyethylene surfaces. The binding between the microspheres and the modified surfaces is due to the interaction between the aldehyde groups of the microspheres and the amine groups of the modified surfaces to form the polyvalent Schiff base bonds. Fourier transform-infrared/attenuated total reflection, electron spectroscopy for chemical analysis, contact angle measurements, and scanning electron microscopy have been used for the characterization of the modified polyethylene surfaces.     

Retinal fundus vasculature multilevel segmentation using whale optimization algorithm

The aim was to present a novel automated approach for extracting the vasculature of retinal fundus images. The proposed vasculature extraction method on retinal fundus images consists of two phases: preprocessing phase and segmentation phase. In the first phase, brightness enhancement is applied for the retinal fundus images. For the vessel segmentation phase, a hybrid model of multilevel thresholding along with whale optimization algorithm (WOA) is performed. WOA is used to improve the segmentation accuracy through finding the \(n{-}1\) optimal n-level threshold on the fundus image. To evaluate the accuracy, sensitivity, specificity, accuracy, receiver operating characteristic (ROC) curve analysis measurements are used. The proposed approach achieved an overall accuracy of 97.8%, sensitivity of 88.9%, and specificity of 98.7% for the identification of retinal blood vessels by using a dataset that was collected from Bostan diagnostic center in Fayoum city. The area under the ROC curve reached a value of 0.967. Automated identification of retinal blood vessels based on whale algorithm seems highly successful through a comprehensive optimization process of operational parameters.     

Eco-Friendly Colorimetric Nanofiber Design: Halochromic Sensors with Tunable pH-Sensing Regime Based on 2-Ethyl-2-Oxazoline and 2-n-Butyl-2-Oxazoline Statistical Copolymers Functionalized with Alizarin Yellow R

Colorimetric nanofibers provide visual, easy-to-interpret sensors for personal use as well as advanced applications. The potential of 2-n-butyl-2-oxazoline (B) and 2-ethyl-2-oxazoline (E) statistical copolymers as a universal, versatile support platform for nanofibrous halochromic sensor design is demonstrated. These polymers are electrospinnable from eco-friendly solvent systems, while wettability, moist adsorption capacity, and water-solubility of the membranes can be easily tuned by changing the B/E monomer ratio, ensuring wide applicability. The halochromic sensing functionality is introduced by incorporating the alizarin yellow R (AYR) chromophore, which is covalently modified with an ethyl ester-group or a short poly(2-n-butyl-2-oxazoline) chain, which is demonstrated to simultaneously prevent dye-leaching and allows tuning of the halochromic pH-sensing window. The colorimetric nanofibrous sensors reversibly respond toward aqueous solutions of different pH, (hydrochloric) acid and alkaline (ammonia) vapors, and several biogenic amines with detection limits as low as 5 ppb. Tunability of sensor responsivity, sensitivity, and pKa via manipulation of dye–polymer interactions, determined by support polymer structure and semi-crystallinity, as well as the chain length of the AYR-modified polymer, are discussed. Preliminary proof-of-principle studies indicate the potential of the developed sensors for sub-ppm biogenic amine vapor detection, which may serve as the basis for future applications in food packaging or breath analysis.