A Robust Transferable Method for the Determination of Glyphosate Residue in Liver After Derivatization by Ultra-high Pressure Liquid Chromatography–Tandem Mass Spectrometry

Glyphosate determination in liver is challenging due to this particular molecule/matrix combination. Glyphosate is a very polar molecule and liver composition is highly variable between individuals and species. Since 2014, the Multiannual Control Program (MACP) of the European Union (EU) demands to analyse glyphosate in food of animal origin on a voluntary basis. Moreover, this analysis will be mandatory in 2017. This paper describes a robust and easily transferable method for glyphosate quantification in liver of animal origin by means of liquid chromatography–tandem mass spectrometry (LC-MS/MS). An intensive clean-up was used to eliminate matrix interferences and was combined with a derivatization step which ensures good retention of glyphosate on a conventional reverse-phase LC column. This method allows to meet the MACP requirements without a time-consuming change in the set-up of the routinely used LC-MS/MS system. Furthermore, it allows the use of an LC column and mobile phases often used in multi-residue analysis. The analytical method was validated according to the SANCO/12571/2013 criteria. Isotopic dilution was used to quantify glyphosate, leading to mean apparent recoveries of 115 and 101 % for the low (0.025 mg kg^?1) and the high (0.250 mg kg^?1) fortification levels, respectively. At both levels, the relative standard deviation was below 10 %. The limit of quantification of 0.025 mg kg^?1 was found to be satisfactory as it was below the maximum residue level (MRL) value set at 0.050 mg kg^?1 for glyphosate in liver. It is also the lowest MRL for all commodity types.     

Enhanced O2 Flux of CaTi0.85Fe0.15O3−δ Based Membranes by Mn Doping

Dense symmetric membranes of CaTi_0.85?xFe_0.15Mn_xO_3?δ (x = 0.1, 0.15, 0.25, 0.4) are investigated in order to determine the optimal Mn dopant content with respect to highest O₂ flux. O₂ permeation measurements are performed as function of temperature between 700°C–1000°C and as function of the feed side ranging between 0.01 and 1 bar. X‐ray photoelectron spectroscopy is utilized to elucidate the charge state of Mn, and synchrotron radiation X‐ray powder diffraction (SR‐XPD) is employed to investigate the structure symmetry and cell volume of the perovskite phase at temperatures up to 800°C. The highest O₂ permeability is found for x = 0.25 over the whole temperature and ranges, followed by x = 0.4 above 850°C. The O₂ permeability for x = 0.25 reaches 0.01 mL(STP) min^?1 cm^?1 at 925°C with 0.21 bar feed side and Ar sweep gas. X‐ray photoelectron spectroscopy indicates that the charge state of Mn changes from approx. +3 to +4 when x > 0.1, which implies that Mn mainly improves electronic conductivity for x > 0.1. The cell volume is found to decrease linearly with Mn content, which coincides with an increase in the activation energy of O₂ permeability. These results are consistent with the interpretation of the temperature and dependency of O₂ permeation. The sintering behavior and thermal expansion properties are investigated by dilatometry, which show improved sinterability with increasing Mn content and that the thermal expansion coefficient decreases from 12.4 to 11.9 × 10^?6 K^?1 for x = 0 and x = 0.25, respectively.     

Properties of phyllosilicate-based porous ceramics shaped by conventional tape casting and freeze tape casting

Silicate ceramics were shaped using tape casting (TC) and freeze tape casting (FTC) processes from three clays labeled HCR, KORS, and KCR. These clays exhibited mass content of 77% halloysite–10 Å, 29% kaolinite, and 98% kaolinite minerals, respectively. After casting the slurries, the dried tapes were sintered at 1200°C. The microstructure changes were characterized before and after sintering using scanning electron microscopy. The apparent porosity of TC samples was lower (36–47 vol.%) compared to values obtained with FTC samples (67–79 vol.%). The latter samples exhibited a highly textured porosity, with micron-sized pores aligned perpendicular to the tape surfaces. Upon sintering, the porosity of TC samples tended to decrease conversely to the case of FTC samples. Such behavior seemed related to the simultaneous effect of organic additives and ice templating. Consequently, the FTC samples showed a relatively low mechanical strength of 3–7 MPa and thermal conductivity of .14– .22 W m⁻¹ K⁻¹. After sintering, the mullite crystallization contributed to strengthen the bulk materials, helping to compensate for the detrimental effect of porosity on the stress to rupture and on thermal conductivity values.     

The adsorption of an epoxy acrylate resin on aluminium alloy conversion coatings

A thermodynamic study of the adsorption of an epoxy acrylate resin used for UV-cured coatings on two different anticorrosion pretreatments on aluminium alloys relevant to aerospace industry has been undertaken. Aluminium alloy Al2219 specimens, treated with an inorganic chromate based conversion coating (Alodine 1200S) and an organic titanium based conversion coating (Nabutan STI/310), were immersed in solutions of different concentrations of the resin and adsorption isotherms were determined by assessing the uptake of the adsorbate, as a function of solution concentration, by time-of-flight secondary ion mass spectrometry (ToF-SIMS). The results show different behaviour for the two substrates, which can be attributed to the organic component of the titanium based coating. In the case of the inorganic conversion coating a clear plateau is achieved at relatively low concentrations and at a lower level of adsorption than for the hybrid coating. The data for both the coatings conform well to the Langmuir model, the organic coating, as well as showing a higher level of adsorption of the resin, also presents oscillatory behaviour at low concentration, which is shown to be complementary to the behaviour of the reactive diluent included with the epoxy acrylate to aid processing. A discussion of this competitive adsorption of the epoxy resin and the diluent on the different substrates is presented, based on considerations of the chemistry of the systems under investigation.     

Data quality awareness: a case study for cost optimal association rule mining

The quality of discovered association rules is commonly evaluated by interestingness measures (commonly support and confidence) with the purpose of supplying indicators to the user in the understanding and use of the new discovered knowledge. Low-quality datasets have a very bad impact over the quality of the discovered association rules, and one might legitimately wonder if a so-called “interesting” rule noted LHS→ RHS is meaningful when 30% of the LHS data are not up-to-date anymore, 20% of the RHS data are not accurate, and 15% of the LHS data come from a data source that is well-known for its bad credibility. This paper presents an overview of data quality characterization and management techniques that can be advantageously employed for improving the quality awareness of the knowledge discovery and data mining processes. We propose to integrate data quality indicators for quality aware association rule mining. We propose a cost-based probabilistic model for selecting legitimately interesting rules. Experiments on the challenging KDD-Cup-98 datasets show that variations on data quality have a great impact on the cost and quality of discovered association rules and confirm our approach for the integrated management of data quality indicators into the KDD process that ensure the quality of data mining results.     

Using Boolean factors for the construction of an artificial neural networks

ABSTRACT

We propose a novel approach to define Artificial Neural Network(ANN) architecture from Boolean factors. ANNs are a subfield of machine learning applicable to several areas of life. However, defining its architecture for solving a given problem is not formalized and remains an open research problem. Since it is difficult to look into the network and figure out exactly what it has learnt, the complexity of such a technique makes its interpretation more tedious. We propose in this paper to build feedforward ANNs using the optimal factors obtained from the Boolean context representing a data. Since optimal factors completely cover the data and therefore give an explanation to these data, We could give an interpretation to the neurons activation and justify the presence of a neuron in our proposed neural network. We show through experiments and comparisons on the use data sets that this approach provides relatively better results for some key performance measures.     

Hypoglycaemia‐free artificial pancreas project

Driving blood glycaemia from hyperglycaemia to euglycaemia as fast as possible while avoiding hypoglycaemia is a major problem for decades for type‐1 diabetes and is solved in this study. A control algorithm is designed that guaranties hypoglycaemia avoidance for the first time both from the theory of positive systems point of view and from the most pragmatic clinical practice. The solution consists of a state feedback control law that computes the required hyperglycaemia correction bolus in real‐time to safely steer glycaemia to the target. A rigorous proof is given that shows that the control‐law respects the positivity of the control and of the glucose concentration error: as a result, no hypoglycaemic episode occurs. The so‐called hypo‐free strategy control is tested with all the UVA/Padova T1DM simulator patients (i.e. ten adults, ten adolescents, and ten children) during a fasting‐night scenario and in a hybrid closed‐loop scenario including three meals. The theoretical results are assessed by the simulations on a large cohort of virtual patients and encourage clinical trials.Inspec keywords: biochemistry, medical control systems, blood, diseases, medical computing, closed loop systems, biomedical equipment, state feedback, patient treatment, patient monitoring, biomedical measurement, physiological models, sugarOther keywords: fasting‐night scenario, hybrid closed‐loop scenario, hypoglycaemia‐free artificial pancreas project, blood glycaemia, euglycaemia, type‐1 diabetes, control algorithm, guaranties hypoglycaemia avoidance, pragmatic clinical practice, state feedback control law, required hyperglycaemia correction bolus, rigorous proof, control‐law, glucose concentration error, hypo‐free strategy control     

Electro-precipitation of magnetite nanoparticles: An electrochemical study

Nanoparticles of magnetites (Fe₃O₄) are synthesized with a new process based on electro-precipitation in ethanol medium. A mechanism pathway is proposed consisting of a Fe(OH)₃ precipitation followed by the reduction of iron hydroxide to magnetite in the presence of hydroxyl ions which are generated at the cathode.     

Toward the first nonpeptidic molecular tong inhibitor of wild-type and mutated HIV-1 protease dimerization

Herein we describe the synthesis and HIV-1 protease (PR) inhibitory activity of 16 new peptidomimetic molecular tongs with a naphthalene scaffold. Their peptidic character was progressively decreased. Two of these molecules exhibited the best dimerization inhibition activity toward HIV-1 wild-type and multimutated ANAM-11 proteases obtained to date for this class of molecules (～40?nM for wild-type PR and 100?nM for ANAM-11 PR). Although the peptidic character of one molecular tong was completely suppressed, the mechanism of inhibition and inhibitory potency toward both proteases were maintained.     

Mechanisms of weight maintenance under high- and low-protein, low-glycaemic index diets

Scope: Weight maintenance after intended weight loss is a challenge in an obesogenic environment. In a large multicentre dietary intervention study (DiOGenes), it has recently been demonstrated that a high‐protein/low‐glycaemic index (HP/LGI) diet was slightly more efficient in maintaining weight loss than low‐protein/LGI or high‐GI (LP/LGI or HGI) diets. Here, we use a proteomic approach to assess the molecular mechanisms behind this positive effect. Methods and results: A subset of the most successful (weight loser, n=12) and unsuccessful (weight re‐gainer, n=12) individuals consuming the LGI diets with either high‐ or low‐protein content (HP or LP/LGI), following an initial calorie deficit run‐in weight loss phase, were analyzed at the plasma protein level. Proteomic analysis revealed 18 proteins regulated after 6 months of the dietary weight maintenance phase. Furthermore, 12 proteins were significantly regulated as a function of success rate under an HP diet, arising as candidate biomarkers of mechanisms of successful weight maintenance under an HP/LGI diet. Pregnancy‐zone protein (PZP) and protein S (PROS1) were revealed as novel biomarkers of weight maintenance showing opposite effects. Conclusion: Semantic network analysis of the 12 regulated proteins revealed that under an HP/LGI an anti‐atherogenic effect and alterations of fat metabolism were associated with the success of maintaining the initial weight loss.