On-line laser desorption/ionization mass spectrometry of matrix-coated aerosols

Matrix-assisted laser desorption/ionization (MALDI) was used for the on-line analysis of single particles. An aerosol was generated at atmospheric pressure and particles were introduced into a time-of-flight (TOF) mass spectrometer through a single-stage differentially pumped capillary inlet. Prior to entering the mass spectrometer, a matrix was added to the particles using a heated saturator and condenser. A liquid matrix, 3-nitrobenzyl alcohol (NBA), and a solid matrix, picolinic acid (PA), were used. Particles were ablated with a 351 nm excimer laser and the resulting ions were mass-separated in a two-stage reflectron TOF mass spectrometer. Aerosol particles containing the biomolecules erythromycin and gramicidin S were analyzed with and without the matrix addition step. The addition of NBA to the particles resulted in mass spectra that contained an intact molecular ion mass peak. In contrast, PA-coated particles did not yield molecular ion peaks from matrix-coated particles.     

Microhardness measurements of poly(methyl methacrylate) and poly(vinylidene fluoride) polyblends

The preparation of polymer blends of poly(methyl methacrylate) and poly(vinylidene fluoride) in different weight percentages is described. Vickers microhardness measurements have been made to study the effects of load and compositional ratio of the two polymers in polyblend. It is observed that poly(vinylidene fluoride) acts as a plasticizer for poly(methyl methacrylate). Evidence of increasing and decreasing strength of polyblends has been obtained for different compositional ratios of the two polymers.     

Extraction-spectrophotometric determination of uranium(VI) with PAR and N-octylacetamide

A new and simple method for selective spectrophotometric determination of uranium(VI) with 4-(2-pyridylazo)resorcinol (PAR) and N-octylacetamide into benzene over pH 7.0–9.0 is described. The molar absorptivity of the complex with 9 different amides is in the range of (0.40–3.2)·10⁴ 1·mol^–1·cm^–1 at the absorption maximum. Out of these, the most sensitive compound N-octylacetamide (OAA) was chosen for detailed studies in the present investigation. The detection limit of the method is 0.008 g U·ml^–1. The system obeys Beer's law in the range of 0–5 g U·ml^–1. The method is free from interferences of most of the common metal ions except vanadium(V) and copper(II), which are masked by proper masking agents. The composition of the complex is determined by curve-fitting method. The method has been applied for the recovery of the metal from rock samples and synthetic mixtures.     

Radiotracer technique in adsorption studies Part XVIII: Uptake of Ce(III) from aqueous solutions by hydrous manganese and stannic oxides

The removal of Ce(III) from aqueous solutions by hydrous manganese oxide (HMO) and hydrous stannic oxide (HSO) was studied as a function of concentrations (10⁻²−10⁻⁷ mol·dm⁻³) and pH (1.2–10.0) by using the radiotracer technique. The effects of co-ions and irradiation of HMO and HSO were also studied. The uptake of Ce(III) fitted well with the Freundlich adsorption isotherm. No significant desorption of pre-adsorbed Ce(III) in the studied temperature range (303–333 K) indicates that both the solids may be good adsorbents for the removal of Ce(III).     

A new method for determining the local environment and orientation of individual side chains of membrane-binding peptides

We studied here the binding of the mastoparan X peptide to a zwitterionic lipid bilayer (POPC) and demonstrated that nitrile-derivatized amino acids can be used to determine the hydration state (or change in hydration state) of specific sites of membrane-interactive peptides (upon binding). We have also shown that polarized ATR-FTIR measurements can further be used to uncover information regarding the spatial orientation of individual side chains as well as their conformational preference within the lipid bilayer.     

Mode of action and synergism of cellulases fromPenicillium funiculosum

A 1,4-β-d-glucan cellobiohydrolase (EC 3.2.1.91) and l,4-β-d-glucan glucanohydrolase (EC 3.2.1.4) were purified from the culture filtrates ofPenicillium funiculosum by using preparative isoelectric focusing. Both the enzymes were homogeneous on polyacrylamide gel with and without sodium dodecyl sulphate. The mol wt of the cellobiohydrolase and endoglucanase were 14,400 and 25,000 respectively. The purified enzymes were free of β-glucosidase activity. Acting in isolation, the cellobiohydrolase had little capacity for solubilizing Avicel or Walseth cellulose, but showed increased rates of hydrolysis when combined with endoglucanase. Cellobiose inhibition (50%) was observed in the initial rate of the hydrolysis of Walseth cellulose. It was also observed that cellobiohydrolase initiates the attack on crystalline cellulose. † NCL communication no. 3898.     

Site-selective C–H nitration of N-aryl-7-azaindoles under palladium(II) catalysis

The site-selective C–H nitration reaction of 7-azaindoles with t-butyl nitrite under palladium catalysis is described. This protocol provides an efficient method for the construction of ortho-nitrated N-aryl-7-azaindoles with excellent site-selectivity and functional group compatibility. The formed 7-azaindole derivatives can be readily transformed into 7-azaindoles containing an aniline functional group under palladium-catalyzed hydrogenation conditions.