Composition and molar mass characterisation of bacterial extracellular polymeric substances by using chemical, spectroscopic and fractionation techniques

The chemical composition and molar-mass distribution of extracellular polymeric substances (EPS) produced by the bacterium Sinorhizobium meliloti have been characterised by combining asymmetrical flow field-flow fractionation (AFlFFF), chemical and spectroscopic techniques. The relationship between the EPS composition and molar-mass distribution has been studied by comparing the characteristics of EPS excreted by the wild type S. meliloti and by a mutant deficient in the production of high-molar-mass EPS, as well as by the analysis of total protein content in the collected AFlFFF fractions. Total organic carbon, protein and polysaccharide contents of the EPS were also determined. Obtained results demonstrate the existence of two major populations with weight-average molar masses of 1.40 x 10(5) and 4.57 x 10(5) g mol(-1) respectively. The lower molar-mass population contained predominantly protein-like substances, detectable by UV-VIS spectroscopy, whereas the higher molar-mass population was rich in exopolysaccharides and exoproteins. These findings are in general agreement with the size distributions and chemical heterogeneity observed by nanoparticle tracking analysis, and the characterisation of the composition of all the EPS by different analytical techniques

Assessment of metal–extracellular polymeric substances interactions by asymmetrical flow field-flow fractionation coupled to inductively coupled plasma mass spectrometry

Extracellular polymeric substances (EPSs) excreted by the bacterium Sinorhizobium meliloti and associated Ca, Cd and Pb were characterised by asymmetrical flow field-flow fractionation coupled with UV spectrophotometry and inductively coupled plasma mass spectrometry in terms of molar-mass distributions, number- and weight-average molar masses and polydispersity index. Two major populations with weight-average molar masses of 74 × 10^3 and 1.35 × 10^6 g mol^–1 were obtained for the EPS. Characterisation of the whole EPS–metal interactions evidenced the preferential binding of Ca and Cd to the low molar mass fraction, whereas Pb associated mainly with the high molar mass (HMM) fraction. Comparison with the EPS produced by exoY-mutant, deficient in HMM-EPS excretion, confirmed the preferential binding of Pb to the high molar mass fraction. Enrichment of the EPS with increasing metal concentrations induced the formation of aggregates, which was most pronounced in the presence of 10^–4 mol L^–1 Pb

Theoretical and experimental investigation of the focusing position in asymmetrical flow field-flow fractionation (AF4)

International audienceTo better understand the focusing process and to determine the focusing position (z(foc)) in Asymmetrical Flow Field-Flow Fractionation (AF4), theoretical and experimental studies were performed. A new theoretical expression that allows the calculation of z(foc) in AF4 channels of any shape having an axial plane of symmetry was established. The equation was then applied to the particular case of a trapezoidal AF4 channel with tapered ends. The applicability of this equation was verified by comparing the calculated results with the experimental measures of the focusing position obtained using blue dextran dye under different flow conditions. The calculated values and the experimental results were in good agreement. The total uncertainty associated with the calculated z(foc) was evaluated and was lower than 10%. A good repeatability and reproducibility of the focusing position was obtained.Moreover, the effects of the sample-injection position, the spacer thickness, the membrane aging, and the nature of the injected sample on the focusing position were investigated: z(foc) was not influenced by these parameters, proving the universal applicability of the equation given in this work for predicting the focusing position, when the assumption of constancy of the cross-flow velocity at the membrane, which underlies this equation, is fulfilled. Additionally, it is notable that this theoretical expression is suitable for different models of AF4 channel and not peculiar to specific supplier

Titanium nanoparticles fate in small-sized watersheds under different land-uses

International audienceSurface waters from three catchments having contrasting land-uses (forested, agricultural, and urban) were sampled monthly and analysed for nanoparticulate titanium dioxide (NPs-TiO2) by single particle ICPMS and electron microscopy. We report one-year of data for NPs-TiO2 having average number and mass concentrations of 9.1 x 108 NPs-TiO2 particles L-1 and 11 μg NPs-TiO2 L-1 respectively. An increase in concentration during warmer months is observed in the forested and agricultural catchments. Both concentrations of NPs-TiO2 are within the range of recently reported values using similar analytical approaches. The positive correlations for NPs-TiO2 mass concentration or particle number with the concentration of some trace elements and DOC in the forested and agricultural catchments suggest the detected NPs-TiO2 in these two systems are mostly from geogenic origin. Additionally, microscopy imaging confirmed the presence of NPs in the three catchments. Furthermore, the land-area normalized annual flux of NPs-TiO2 (1.65 kg TiO2 year-1 km-2) was highest for the agricultural catchment, suggesting that agricultural practices have a different impact on the NPs-TiO2 dynamics and exports than other land-uses (urban or forestry). A similar trend is also found by the reanalysis of recent literature data

Asymmetrical flow field flow fractionation - Multidetection system as a tool for studying metal-alginate interactions

The present study explores the potential use of asymmetrical flow field flow fractionation (aFlFFF) with a multidetection system for the study of metal-alginate interactions. aFlFFF, coupled on-line to a differential refractive index and seven angle laser light scattering detectors was used to provide information on the alginate size distributions. In parallel, the metal distributions of metal-alginate complexes were probed by aFlFFF-high resolution inductively coupled plasma-mass spectrometry. Average values and continuous distributions of molar masses, radiuses of gyration and hydrodynamic radiuses, which are critical for understanding the role of alginates as carriers of metal pollutants, were evaluated in presence of Pb or Cd and compared with those in metal-free solutions of alginate. The values of number average and weight average molar mass, weight average radius of gyration and shape factor for alginate were 150 and 188 kg mol(-1), 53 nm and 1.7, respectively. Alginate molar mass and radius of gyration distributions were slightly shifted to higher values by the addition of micromolar concentrations of Pb or Cd. The alginate size distribution in the presence of Cd was similar to the alginate-alone control, whereas in the presence of Pb the size distribution was broader with a shift of the maximum toward higher molar masses

Characterization of the colloidal organic matter from the Amazonian basin by asymmetrical flow field-flow fractionation and size exclusion chromatography

Colloidal organic matter (COM) collected in small and large watercourse tributaries of the Negro River (Brazil) were fractionated and characterized by an asymmetrical flow field-flow fractionation (AFlFFF) coupled to UV and seven angle laser light scattering (LS) detectors, and by size exclusion chromatography (SEC) coupled with a UV detection. Number and weight average molar masses, weight average gyration radiuses RGw and polydispersity indexes were obtained for each sample in two separate runs under conditions optimized for lower and larger size fractions. The results demonstrate the existence of a decrease of size of the colloidal matter when passing from first order streams to higher order rivers. No significant changes were found in size distributions of samples collected during the low and high flow stages at the same site. The influence of selected pre-treatments such as filtration and reverse osmosis pre-concentration on the size and molar mass distributions was also studied

Flow and fate of silver nanoparticles in small French catchments under different land-uses: The first one-year study

International audienc

Biotransformation of Food-Grade and Nanometric TiO2 in the Oral–Gastro–Intestinal Tract: Driving Forces and Effect on the Toxicity toward Intestinal Epithelial Cells

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An interlaboratory comparison on whole water samples

The European Water Framework Directive 2000/60/EC requires monitoring of organic priority pollutants in so called “whole water” samples, i.e. in aqueous non-filtered samples that contain natural colloidal and suspended particulate matter. Colloids and suspended particles in the liquid phase constitute a challenge for sample homogeneity and stability. Within the joint research project ENV08 “Traceable measurements for monitoring critical pollutants under the European Water Framework Directive 2000/60/EC” whole water test materials were developed by spiking defined amounts of aqueous slurries of ultra-finely milled contaminated soil or sediment and aqueous solutions of humic acid into a natural mineral water matrix. This paper presents the results of an European-wide interlaboratory comparison (ILC) using this type of test materials. Target analytes were tributyl tin, polybrominated diphenyl ethers and polycyclic aromatic hydrocarbons in the ng/L concentration range. Results of the ILC indicate that the produced materials are sufficiently homogeneous and stable to serve as samples for e.g. proficiency testing or method validation. To our knowledge, this is the first time that ready to use water materials with a defined amount of suspended particulate and colloidal matter have been applied as test samples in an interlaboratory exercise. These samples meet the requirements of the European Water Framework Directive. Previous proficiency testing schemes mainly employed filtered water samples fortified with a spike of the target analyte in a water-miscible organic solvent.JRC.D.2-Standards for Innovation and sustainable Developmen