Soluble manganese (IV); a new chemiluminescence reagent

The oxidations of twenty five organic and inorganic species, with solublised manganese(IV), were found to elicit analytically useful chemiluminescence with detection limits (3 × S/N) for Mn(II), Fe(II), morphine and codeine of 5 × 10^–8 M, 2.5 × 10^–7 M, 7.5 × 10^–8 M and 5 × 10^–8 M, respectively. Additionally, the corrected spectra from four different analytes gave wavelengths of maximum emission in the range from 733 nm up to 740 nm suggesting that all these chemiluminescence reactions shared a common emitting species.

Comparison of soluble manganese(IV) and acidic potassium permanganate chemiluminescence detection using flow injection and sequential injection analysis for the determination of ascorbic acid in vitamin C tablets

The limits of detection (3s) for ascorbic acid were 5×10⁻⁸ M with acidic potassium permanganate using both flow injection analysis (FIA) and sequential injection analysis (SIA) whereas the soluble manganese(IV) afforded 1×10⁻⁸ M and 5×10⁻⁹ M for FIA and SIA, respectively. Determinations of ascorbic acid in Vitamin C tablets were achieved with minimal sample pretreatment using a standard additions calibration and gave good agreement with those of iodimetric titration.

Soluble poly-3-alkylpyrrole polymers on films and fabrics

Conductive textiles with specific properties can be produced by the chemical polymerisation of a range of 3-alkylpyrroles in the presence of textiles. The morphologies of these coatings are altered from the traditional conductive coatings. Comparison using a SEM reveals substantial differences.

Application of soluble poly (3-alkylpyrrole) polymers on textiles

Soluble conducting poly(3-decanylpyrrole) was directly applied to textiles as a nanoparticle emulsion, using a variety of techniques including hand-brushing, dipping and spray painting. These coatings were compared to those formed by chemical polymerization of 3-decanylpyrrole on the surface of the textile by solution, using vapor and spray polymerization methods. The coating formed using chemical polymerization methods had lower surface resistivity than that formed by direct application of a soluble polymer.

It was observed that applied coatings of poly(3-decanylpyrrole) showed a smoother surface morphology with a more even dispersion compared to those formed by chemical methods.

Soluble manganese(IV) as a chemiluminescence reagent for the determination of opiate alkaloids, indoles and analytes of forensic Interest

We present the results of our investigations into the use of soluble manganese(IV) as a chemiluminescence reagent, which include a significantly faster method of preparation and a study on the effect of formaldehyde and orthophosphoric acid concentration on signal intensity. Chemiluminescence detection was applied to the determination of 16 analytes, including opiate alkaloids, indoles and analytes of forensic interest, using flow injection analysis methodology. The soluble manganese(IV) reagent was less selective than either acidic potassium permanganate or tris(2,2′-bipyridyl)ruthenium(III) and therefore provided a more universal chemiluminescence detection system for HPLC. A broad spectral distribution with a maximum at 730 ± 5 nm was observed for the reaction between the soluble manganese(IV) and a range of analytes, as well as the background emission from the reaction with the formaldehyde enhancer. This spectral distribution matches that reported for chemiluminescence reactions with acidic potassium permanganate, where a manganese(II) emitting species was elucidated. This provides further evidence that the emission evoked in reactions with soluble manganese(IV) also emanates from a manganese(II) species, and not bimolecular singlet oxygen as suggested by previous authors.

Bioassay detects soluble MAdCAM-1 in body fluids

Mucosal addressin cell adhesion molecule (MAdCAM-1) is a key player in mediating the infiltration of leucocytes into chronically inflamed tissues. Five anti-MAdCAM-1 monoclonal antibodies (mAb), designated 17F5, 201F7, 314G8, 377D10 and 355G8, were generated by fusion of P3 × 63Ag8.653 myeloma cells with spleen cells from BALB/c mice immunized with recombinant human MAdCAM-1-Fc. The latter four mAb recognize the ligand-binding first Ig domain, and block T -cell adhesion to MAdCAM-1. The non-blocking mAb 17F5 recognizes the mucin domain. Extensive analysis of a large panel of paraffin-embedded human tissues revealed that the 314G8 mAb detected MAdCAM-1 on venules in the spleen and small intestine. MAdCAM-1 was strongly expressed in the synovium of osteoarthritis patients, predominantly on the endothelial lining of blood vessels, but also within the vessel lumen. An ELISA, based on mAb 377D10 and 355G8, was developed to determine whether soluble MAdCAM-1 was present in body fluids, and to measure the levels present. The assay detected soluble MAdCAM-1 in the serum and urine of healthy donors, at levels similar to those of soluble forms of the related CAM, ICAM-1 and VCAM-1. The anti-MAdCAM-1 antibodies and assay developed here may be useful therapeutically in the treatment of inflammation in humans. Similarly, they may be useful diagnostically to monitor the presence and levels of MAdCAM-1.

Design, synthesis and preliminary analytical evaluation of water soluble reagents for peroxyoxalate chemiluminescence

Describes the investigation into a number of facets of the peroxyoxalate chemiluminescence reaction, and the application of this chemistry to the detection of certain analytes under purely aqueous conditions.

Synthesis and characterization of soluble conducting polymers

Although conducting polymers have various potential applications, lack of solubility is an impediment in their direct application to material surfaces. Synthesis of alkyl pyrrole monomers and subsequent polymerization into soluble conducting polymers are aimed as alternatives to conventional methods of application of conducting polymers on substrates. Alkyl chains are attached to a pyrrole ring to produce solubility in the resulting conducting polypyrroles, which allow direct application of conductive polymer emulsions to any desired surface. Friedel-Crafts acylation of the tosyl-protected pyrrole provides high yields of the 3-acylated product. The conductivity values of poly-3- and 3, 4-substituted pyrroles are generally less than the unmodified polypyrrole. Increasingly bulkier groups attached to the pyrrole means lower conductivity of the resultant polymer. As the carbon chain length attached to the 3-position of pyrrole increases, the solubility also increases. However, the magnitude of change in conductivity of films and pellets of soluble conducting polypyrroles over the alkyl range is not significant.

Cellular localization of water soluble, allergenic proteins in rye-grass (Lolium perenne) pollen using monoclonal and specific IgE antibodies with immunogold probes

A postembedding method has been developed for localizing water soluble allergens in rye-grass pollen. This uses dry fixation in glutaraldehyde vapour, followed by 2,2-dimethoxypropane, prior to a 100% ethanol series leading into embedment in LR Gold. This has allowed the attachment of specific monoclonal antibodies to the allergen, which are themselves probed with specific immunogold labels to the antibodies. Wall and cytoplasmic sites have been identified, representing an improvement of fixation and localization of allergens over previous studies employing polyclonal, broad spectrum antibodies.

Rye-grass allergens are labelled in mature pollen grains in the exine (tectum, nexine and central chamber), and in the electron opaque areas of the cytoplasm, especially mitochondria. The allergens are absent from the intine, polysaccharide (P) particles, amyloplasts, Golgi bodies and endoplasmic reticulum. IgE antibodies derived from humans allergic to rye-grass pollen, bind to similar sites in the cytoplasm but only to the outer surface of the pollen grain wall. This method now provides a valuable tool for further developmental studies on the pollen grains, in order to establish the site/s of synthesis of the allergens.

Methods of coating textiles with soluble conducting polymers

Soluble conducting alkyl polypyrrole polymers have been applied by either chemical polymerization of the 3-alkyl monomers or direct application of polymer emulsion to the surface. Solution, vapor and spray polymerization methods of coating poly(3-alkylpyrroles) to the surface of woven wool fabrics are explored. Conductive textile samples have also been prepared by applying emulsions of soluble prepolymerized 3-alkylpyrrole to the fabric surface. Direct applications of a conductive paint to the textile surface eliminate the exposure of the substrate to damaging oxidizing agents which allow the coating of more sensitive and delicate substrates. All textiles produced are tested for abrasion resistance and conductivity. For alkyl polypyrrole coated fabrics, the optimum carbon chain lengths are between n=10 and n=14, which result in optimum values of conductivity and solubility. The darkness of the tone is inversely related to the surface resistivity of the resulting conductive fabric. Therefore, deep black coatings have low resistivity whereas light gray coatings on a white fabric surface have higher surface resistivity. Longer alkyl chains result in higher surface resistivity in fabrics. The conductive coating of poly(3-decanylpyrrole) on the textile surface has a better abrasion resistance compared to that of an unsubstituted polypyrrole coating.

Boron carbon nitride nanostructures from salt melts : tunable water-soluble phosphors

A simple, high yield, chemical process is developed to fabricate layered h-BN nanosheets and BCNO nanoparticles with a diameter of ca. 5 nm at 700 °C. The use of the eutectic LiCl/KCl salt melt medium enhances the kinetics of the reaction between sodium borohydride and urea or guanidine as well as the dispersion of the nanoparticles in water. The carbon content can be tuned from 0 to 50 mol % by adjusting the reactant ratio, thus providing precise control of the light emission of the particles in the range 440–528 nm while reaching a quantum yield of 26%. Because of their green synthesis, low toxicity, small size, and stability against aggregation in water, the as-obtained photoluminescent BCNO nanoparticles show promise for diagnostics and optoelectronics.

Chemiluminescence detection with water-soluble iridium(III) complexes containing a sulfonate-functionalised ancillary ligand

The chemiluminescence from four cyclometalated iridium(III) complexes containing an ancillary bathophenanthroline-disulfonate ligand exhibited a wide range of emission colours (green to red), and in some cases intensities that are far greater than the commonly employed benchmark reagent, [Ru(bpy)3](2+). A similar complex incorporating a sulfonated triazolylpyridine-based ligand enabled the emission to be shifted into the blue region of the spectrum, but the responses with this complex were relatively poor. DFT calculations of electronic structure and emission spectra support the experimental findings.