Determination of glucosamine in raw materials and dietary supplements containing glucosamine sulfate and/or glucosamine hydrochloride by high-performance liquid chromatography with FMOC-Su derivatization: collaborative study

A collaborative study was conducted for determination of glucosamine in raw materials and dietary supplements containing glucosamine sulfate and/or glucosamine hydrochloride by high-performance liquid chromatography (HPLC) with N-(9-fluorenyl-methoxycarbonyloxy) succinimide (FMOC-Su) derivatization. Thirteen blind materials, one pair of which were duplicates, were tested by 12 collaborating laboratories. The test samples consisted of various commercial products, including tablets, capsules, drink mix, and liquids as well as raw materials, blanks, and those for spike recovery analyses. The tests with blank products and products spiked with glucosamine showed good specificity of the method. The average recoveries at spike levels of 100 and 150% of the declared amount were 99.0% with a relative standard deviation (RSD) of 2.1%, and 101% with an RSD of 2.3%, respectively. The test results between laboratories on each commercial product were reproducible with RSD values of no more than 4.0%, and the results were repeatable in the same laboratory with an average RSD of 0.7%. HorRat values ranged from 0.5 to 1.7 on both tests of spike recovery and reproducibility between laboratories on commercial products. The average determination coefficient of the calibration curves from the laboratories was 0.9995 with an RSD of 0.03%. All of the 12 collaborating laboratories succeeded in the study and none of their reported test results were outliers, partly indicating the robustness of the method. It is recommended that the method be accepted by AOAC INTERNATIONAL as Official First Action.     

Synthesis and Visible Spectral Behaviour of Some New N‐Bridgehead Heterocyclic Cyanine Dyes Incorporating Pyrazolo (4,5‐b) Indolizine (Benzoindolizine)

The new unsymmetrical N‐bridgehead, apo (zeromethine), mono‐methine, dimethine, meso substituted tetramethine and styryl cyanine dyes incorporating pyrazolo (4,5‐b) indolizine (benzoindolizine) nuclei were prepared. Structural confirmation was carried out by elemental analyses, IR, H‐NMR, mass spectra and ¹³C‐NMR with the aid of carbon DEPT spectral data. The visible absorption spectra for the newly synthesized cyanines were examined in 95% ethanol.     

Synthesis and Structure Determination of Some New N‐Glycosides of 4,5‐Disubstituted‐1,2,4‐Triazole‐3‐Thiones

Some new N‐glycosides of 4‐(2‐phenylethyl)‐5‐pyridyl‐1,2,4‐triazole‐3‐thiones were synthesised by the coupling reaction of halo sugar with 4,5‐disubstituted 3H‐1,2,4‐triazole‐3‐thiones in the presence of mercuric cyanide and dry nitromethane as solvent, followed by deprotection using dry ammonia in methanol. All of the above compounds were fully characterized by means of infrared, ¹H NMR spectroscopy, mass spectroscopy and elemental analysis.     

Effect of Phosphorus Content on Thermal Behaviour of Diglycidyl Ether of Bisphenol-A/phosphorus Containing Amines

Curing of diglycidyl ether of bisphenol-A (DGEBA) with phosphorus containing amide amines i.e. bis[3(3’-aminobenzamido phenyl)]methyl phosphine oxide (MB),bis[3(4’-aminobenzamido phenyl)]methyl phosphine oxide (PB), tris[3(3’-aminobenzamidophenyl)] phosphine oxide (MT) and tris[3(4’-aminobenzamido phenyl)] phosphine oxide (PT)and conventionally used curing agent 4,4’-diaminodiphenyl sulfone (D) was studied by DSC. The amines MB, PB, MT and PT were synthesised in the laboratory and were characterized by determining elemental composition, melting point, and amine equivalent. Structural characterization was done by ¹H-NMR and FTIR. The onset temperature of curing depended on the nucleophilicity of the amines and was in the orderMT≈MB<PT<PB<D. The exothermic peak temperatures were in the orderD>PB>PT>MT≈MB. The char residue of cured epoxy resin was significantly higher when phosphorus was incorporated in the cured network. Using mixed amine formulations based on amine D and P-containing amines and the molar ratio of these amines could easily control the curing characteristics. A linear relationship between char yield and P-content was observed in such formulations. This revised version was published online in August 2006 with corrections to the Cover Date.     

Method for Visible Light‐Induced Photocatalytic Degradation of Methylparaben in Water Using Nanostructured Ag/AgBr@m‐WO3

An efficient method of photocatalytic degradation of methylparaben in water using Ag nanoparticles (NPs) loaded AgBr‐mesoporous‐WO₃ composite photocatalyst (Ag/AgBr@m‐WO₃), under visible light is presented. In this process, quantification of methylparaben in water was carried out by high‐performance liquid chromatography (HPLC) and the HPLC results showed a significant reduction of methylparaben in water due to the enhanced of photocatalytic degradation efficiency of Ag/AgBr@m‐WO₃. For the material synthesis, highly ordered mesoporous‐WO₃ (m‐WO₃) was initially synthesized by sol–gel method and AgBr nanoparticles (NPs) were subsequently introduced in the pores of m‐WO₃, and finally, the Ag nanoparticles were introduced by light irradiation. The enhanced photocatalytic degradation of methylparaben in water is attributed to the formation of surface plasmonic resonance (SPR) due to the introduction of Ag NPs on the surface of the catalyst. Also, the formation of heterojunction between AgBr and mesoporous‐WO₃ in Ag/AgBr@m‐WO₃ significantly inhibited the recombination of light‐induced electron‐hole pairs in the semiconductor composite. The morphological and optical characterizations of the synthesized photocatalysts (Ag/AgBr@m‐WO₃) were carried out using SEM, TEM, XDR, N₂ adsorption–desorption, UV‐VIS diffuse reflectance spectroscopy (DRS). Also, the photocatalytic studies using radical scavengers were carried out and the results indicated that ${\text{O}}_2^{·-}$ is the main reactive species.     

Mixed ligand palladium(II) and platinum(II) complexes of tertiary diphosphines and benz-1,3-imidazoline-2-thione,benz-1,3-oxazoline-2-thione or benz-1,3-thiazoline-2-thione

Palladium(II) and platinum(II) complexes containing the mixed ligands tertiary diphosphines Ph₂P(CH₂) _n PPh₂, (n = 1–4) and benz-1,3-imidazoline-2-thione, benz-1,3-oxazoline-2-thione or benz-1,3-thiazoline-2-thione have been prepared and characterized by elemental analysis, magnetic susceptibility, molar conductance and i.r. spectral data. ³¹P–{¹H}-n.m.r. data have been applied to characterize the produced linkage isomers.     

Rapid analysis of intact phospholipids from whole bacterial cells by matrix-assisted laser desorption/ionization mass spectrometry combined with on-probe sample pretreatment

Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOFMS), utilizing an on-probe sample pretreatment, was applied to the rapid and direct detection of intact phospholipids from whole bacterial cells. The sample preparation procedure involved depositing growing bacterial colonies from culture dishes directly onto the MALDI probe followed by treatment of the sample spot with a 3 micro L aliquot of an aqueous 0.05 M solution of sodium iodide prior to the addition of a 2,5-dihydroxybenzoic acid (DHB) matrix solution (ca. 8 mg dissolved in 70% acetonitrile/30% H(2)O containing 0.1% of trifluoroacetic acid). The MALDI spectra obtained from whole bacteria cells showed a series of ions generated from bacterial phospholipids, such as phosphatidylethanol-amines (PEs) and phosphatidylglycerols (PGs), which were clearly observed as well-resolved peaks. The ranges of the observed total carbon numbers in two acyl groups for PEs and PGs (30-36 and 33-36, respectively) were in good agreement with those reported previously. Furthermore, the distinct discrimination of four species of the Enterobacteriaceae family cultured identically was achieved by using principal components analysis (PCA) conducted on the relative peak intensities of phospholipids observed from the MALDI spectra.     

Phosphodiesterase‐Inhibiting Glycosides from Symplocos racemosa

Phytochemical investigation of Symplocos racemosa resulted in the isolation of two new glycosides, symploracemoside ( 1 ) and symplomoside ( 2 ), which are structurally related to the reported benzoylsalireposide ( 3 ) and salireposide ( 4 ). The structure elucidation of the isolated compounds was based primarily on 1D‐ and 2D‐NMR analysis, including COSY, NOESY, HMQC, and HMBC correlations. These glycosides showed inhibitory activity against snake‐venom phosphodiesterase I.     

Additives for the reduction of sulfur in FCC gasoline

Sulfur reduction ability of alumina supported zinc, gallium and zinc-gallium additives for fluid catalytic cracking catalysts was evaluated in a micro-activity test unit (MAT). Gallium/alumina showed the highest sulfur reduction of 31%, but the cracking activity of the catalyst was decreased. Zinc-gallium/alumina reduced sulfur in 24 wt.% without decreasing the base catalyst activity.