Synthesis and Properties of Mixed Ligand Complexes of Diorganotin(IV): Part(VII) – Synthesis and Characterisation of Some Antibacterial Dibenzoylmethane Diorganotin(IV)‐O‐alkyl Trithiophosphates

A series of some new mixed ligand complexes have been synthesized with an objective for evaluation as antimicrobials. Reactions of diorganotin(IV) dichloride with dibenzoyl methane and O‐alkyl trithiophosphates in a 1:1:1 molar ratio in refluxing benzene yield products of the type [PhCOCHCOPh]R₂Sn‐[SSH(S)POR'] [where R = Me, Bu, Ph; R' = Me, Et, Prⁱ, Buⁱ, Ph]. The newly synthesized complexes are light yellow colored crystalline solids, non‐volatile, soluble in common organic solvents, monomeric in nature and highly sensitive towards atmospheric moisture. These complexes are characterized by elemental analysis, IR and multinuclear NMR (¹H, ³¹P and ¹¹⁹Sn) spectral studies. Spectral studies of these complexes indicate that dibenzoyl methane and O‐alkyl trithiophosphate moieties are bidentate and the central tin atom is hexacoordinated in nature. A few of these compounds were tested for their antibacterial activity using standard drugs.     

Recent advances of capillary electrophoresis in pharmaceutical analysis

This review covers recent advances of capillary electrophoresis (CE) in pharmaceutical analysis. The principle, instrumentation, and conventional modes of CE are briefly discussed. Advances in the different CE techniques (non-aqueous CE, microemulsion electrokinetic chromatography, capillary isotachophoresis, capillary electrochromatography, and immunoaffinity CE), detection techniques (mass spectrometry, light-emitting diode, fluorescence, chemiluminescence, and contactless conductivity), on-line sample pretreatment (flow injection) and chiral separation are described. Applications of CE to assay of active pharmaceutical ingredients (APIs), drug impurity testing, chiral drug separation, and determination of APIs in biological fluids published from 2008 to 2009 are tabulated.     

Versatile bio-ink for covalent immobilization of chimeric avidin on sol-gel substrates

A bio-ink for covalent deposition of thermostable, high affinity biotin-binding chimeric avidin onto sol-gel substrates was developed. The bio-ink was prepared from heterobifunctional crosslinker 6-maleimidohexanoic acid N-hydroxysuccinimide which was first reacted either with 3-aminopropyltriethoxysilane or 3-aminopropyldimethylethoxysilane to form silane linkers 6-maleimide-N-(3-(triethoxysilyl)propyl)hexanamide or -(ethoxydimethylsilyl)propyl)-hexanamide. C-terminal cysteine genetically engineered to chimeric avidin was reacted with the maleimide group of silane linker in methanol/PBS solution to form a suspension, which was printed on sol-gel modified PMMA film. Different concentrations of chimeric avidin and ratios between silane linkers were tested to find the best properties for the bio-ink to enable gravure or inkjet printing. Bio-ink prepared from 3-aminopropyltriethoxysilane was found to provide the highest amount of active immobilized chimeric avidin. The developed bio-ink was shown to be valuable for automated fabrication of avidin-functionalized polymer films.     

Effect of pH on growth and fatty acid composition ofLactobacillus büchneri andLactobacillus fermentum

Growth and fatty acid composition of two lactobacilli,Lactobacillus büchneri andLactobacillus fermentum, were studied at different pHs of the media in a small-scale fermenter with particular interest in lactobacillic acid production of the cultures. Generally, the total fatty acid content of the bacterial cells increased with increasing culture age. The production of lactobacillic acid was affected in the two lactobacilli by both culture age and pH of the media, but in a very different manner. In L.büchneri cultures, the relative proportion of lactobacillic acid was highest when the pH was lowest (pH 4.5), whereas inL. fermentum cultures, the proportion of lactobacillic acid was highest at pH 7.0. The pH of the medium affected not only the relative proportion of lactobacillic acid, but also biomass production and total fatty acid accumulation of the cultures. Thus, by controlling the pH of the cultures, the volumetric yield of lactobacillic acid could be improved considerably compared to cultures without pH control.     

Acetylated derivatives of C-methylated analogues of spermidine: synthesis and interaction with N1-acetylpolyamine oxidase

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Europium(III)-chelates embedded in nanoparticles are protected from interfering compounds present in assay media

Lanthanide chelates are excellent labels in ligand binding assays due to their long lifetime fluorescence, which enables efficient background reduction using time-resolved measurement. In separation-free homogeneous assays, however, some compounds in the sample may cause quenching of the lanthanide fluorescence and extra steps are required before these samples can be measured. In this study we have evaluated whether europium chelates packed inside a polystyrene nanoparticle are better protected from the environment than individual Eu(III)-chelates, and do these particles have higher tolerance against known interfering compounds (bivalent metal ions and variation of pH). We also tested whether metal ions had any effect on a fluorescence resonance energy transfer (FRET) based detection of a bioaffinity binding reaction. The presence of metal ions or variation of pH did not affect the fluorescence of the Eu(III)-chelate dyed nanoparticles, while significant decrease of the fluorescence was detected with a 9-dentate Eu(III)-chelate. Metal ions also decreased the fluorescence lifetime of the 9-dentate Eu(III)-chelate from 0.960 to 0.050 ms. Coloured metal ions caused a minor decrease in sensitised emission generated by FRET when Eu(III)-chelate dyed nanoparticles were used as donor labels. The decreased signal was due to the absorption of the sensitised emission by the coloured metal ions, since the metal ions had no effect on the lifetime of the sensitised emission. Thus the Eu(III)-chelate dyed nanoparticles are preferred labels in homogeneous bioaffinity assays, when interfering compounds are known to be present.     

Mass spectrometric and tandem mass spectrometric behavior of nitrocatechol glucuronides: A comparison of atmospheric pressure chemical ionization and electrospray ionization

The mass spectrometric (MS) and tandem mass spectrometric (MS/MS) behavior of six nitrocatechol-type glucuronides using atmospheric pressure chemical ionization (APCI) and electrospray ionization (ESI) was systematically studied, and the effect of operation parameters on the fragmentations are presented. The positive ion APCI- and ESI-MS spectra showed an intense protonated molecule and the respective negative ion spectra a deprotonated molecule with minimal fragmentation. The main fragment ions in the MS/MS spectra of the protonated and deprotonated molecules were [M + H - Glu]+ and [M - H - Glu]-, respectively, formed by the loss of the glucuronide moiety. The measured limits of detection indicated that ESI is a significantly more efficient ionization method than APCI in the negative and positive ion modes for the compounds studied. MS/MS was found to be less sensitive, but more reliable and simple than MS due to the absence of chemical noise.     

Clean-up method for determination of established and emerging brominated flame retardants in dust

A clean-up method was developed to enable the determination of tri-decabrominated diphenyl ethers, isomer-specific hexabromocyclododecanes (HBCDs), 1,2-bis(2,4,6-tribromophenoxy)ethane (BTBPE), decabromodiphenyl ethane (DBDPE), (2-ethylhexyl)tetrabromobenzoate (TBB), and bis(2-ethylhexyl)tetrabromophthalate (TBPH) in the same dust sample extract using reasonable amounts of solvents and without dividing the sample. After extraction, the sample was separated on a silica column into three fractions that were subsequently cleaned up individually. The polybrominated diphenyl ethers (PBDEs) and DBDPE were eluted in Fraction I, TBB, TBPH, and BTBPE in Fraction II, and HBCDs in Fraction III. Fractions I and II were analyzed using gas chromatography/mass spectrometry and Fraction III using liquid chromatography/mass spectrometry. The method gave good recoveries (60-120%), precise results using (13)?C-labelled internal standards and was accurate when comparing results to certified values (PBDEs in NIST SRM 2585). The method was applied to dust samples from the Stockholm (Sweden) area. All the emerging brominated flame retardants (BFRs) studied, except BTBPE, were present in all the samples in quantifiable concentrations, often higher than the PBDEs. BTBPE was quantified in only one sample. It is evident that emerging BFRs are present in Swedish homes, and these compounds should be included in the BFR analyses of indoor environments.