Determining adulteration of canned products using SNIF-NMR and IRMS: detection of undeclared addition of synthetic acetic acid

Possible adulteration of canned products containing spirit vinegar pickle by adding synthetic acetic acid is a significant problem of the food industry. Isotope analyses, which determine botanical origin of acetic acid and also can detect synthetic acid, were applied to detect undeclared addition of synthetic acetic acid to canned products. The aim of the study was to improve the extraction technique for the SNIF-NMR (²H/¹H; site-specific natural isotopic fractionation-nuclear magnetic resonance) and IRMS (¹³C/¹²C; isotope ratio mass spectrometry) isotope methods and for an atypical matrix and to determine isotope ratios in canned vegetables pickle to prove their adulteration or authenticity. The following set of canned products was analysed: pickled cucumbers (n = 16) and one vinegar pickle purchased in the Czech market and six model (cucumber) pickles. The determined ratios of ²H/¹H and ¹³C/¹²C for the pickled cucumbers proved to be authentic ranged from 89.4 to 107.0 ppm and from ?28.7 to ?15.6 ‰, respectively; for the synthetic acetic acids diluted with water they ranged from 114.2 to 129.0 ppm and from ?44.9 to ?33.4 ‰, respectively. Isotope analyses were confirmed as a reliable tool for assessing authenticity of canned products. The method enables detection of synthetic acetic acid addition into vinegars and canned vegetables containing vinegar pickle up from 20 % (of total acidity).     

Separation of selective organic acids from wastewater through a polyol supported liquid membrane

Pesticide toxicity databases usually include data on pure chemicals (active ingredients). Technical pesticides formulations, however, are mixtures with adjuvants as applied to fields/crops. Two formulations of the same pesticide can differ in their environmental fate and their toxicity. This work presents the evaluation of the toxicity of the dinitroaniline herbicide, pendimethalin by simultaneous analysis of its respiration rate and generation of a membrane potential (Δ Ψ) in rat liver mitochondria. Chromatography grade pendimethalin (8.2·10^?5 ‐ 5.47·10^?4 M or 23 – 154 ppm) caused lower enhancement of the mitochondrial respiration and decrease of the Δ Ψ than technical grade pendimethalin (Stomp), i.e. the mixture of pure ingredient and adjuvant(s). These effects are comparable to those of 2,4‐dinitrophenol. Pure and technical grade pendimethalin acts as an uncoupler of oxidative phosphorylation in mitochondria (enhances respiration and diminishes Δ Ψ). These data conflict with the statement, presented in the US EPA manual Recognition and Management of Pesticides Poisonings, that pendimethalin does not act as an uncoupler of oxidative phosphorylation.     

Experimental Investigation of the Properties of Lime-Based Plaster-Containing PCM for Enhancing the Heat-Storage Capacity of Building Envelopes

Experimental analysis of a wide range of properties of a lightweight plaster which should enhance the heat-storage capacity of building envelopes is presented. The basic physical characteristics, namely, the bulk density, matrix density, total open porosity, and pore-size distribution are measured at first. Then, the compressive strength is determined for an assessment of mechanical performance of the plaster. The thermal conductivity and thermal diffusivity are studied using an impulse technique. Differential scanning calorimetry measurements are performed as well, in order to identify the temperature range and latent heat of the phase change and to determine the specific heat capacity as a function of temperature. Durability properties are assessed using the measurement of the water absorption coefficient and sorption and desorption isotherms. The experimental results indicate a good capability of the designed plaster to moderate effectively the interior climate of buildings.     

Development of a solid self-microemulsifying drug delivery system (SMEDDS) for solubility enhancement of naproxen

Context: Comparative evaluation of liquid and solid self-microemulsifying drug delivery systems (SMEDDS) as promising approaches for solubility enhancement.

Objective: The aim of this work was to develop, characterize, and evaluate a solid SMEDDS prepared via spray-drying of a liquid SMEDDS based on Gelucire® 44/14 to improve the solubility and dissolution rate of naproxen.

Material and methods: Various oils and co-surfactants in combination with Gelucire® 44/14 were evaluated during excipient selection study, solubility testing, and construction of (pseudo)ternary diagrams. The selected system was further evaluated for naproxen solubility, self-microemulsification ability, and in vitro dissolution of naproxen. In addition, its transformation into a solid SMEDDS by spray-drying using maltodextrin as a solid carrier was performed. Scanning electron microscopy (SEM), differential scanning calorimetry (DSC), and X-ray diffraction (XRD) were used to evaluate the physical characteristics of the solid SMEDDS obtained.

Results: The selected formulation of SMEDDS was comprised of Miglyol 812®, Peceol?, Gelucire® 44/14, and Solutol® HS 15. The liquid and solid SMEDDS formed a microemulsion after dilution with comparable average droplet size and exhibited uniform droplet size distribution. In the solid SMEDDS, liquid SMEDDS was adsorbed onto the surface of maltodextrin and formed smooth granular particles with the encapsulated drug predominantly in a dissolved state and partially in an amorphous state. Overall, incorporation of naproxen in SMEDDS, either liquid or solid, resulted in improved solubility and dissolution rate compared to pure naproxen.

Conclusion: This study indicates that a liquid and solid SMEDDS is a strategy for solubility enhancement in the future development of orally delivered dosage forms.     

Reconstructing the microstructure of polyimide–silicalite mixed‐matrix membranes and their particle connectivity using FIB‐SEM tomography

Properties of a composite material made of a continuous matrix and particles often depend on microscopic details, such as contacts between particles. Focusing on processing raw focused‐ion beam scanning electron microscope (FIB‐SEM) tomography data, we reconstructed three mixed‐matrix membrane samples made of 6FDA‐ODA polyimide and silicalite‐1 particles. In the first step of image processing, backscattered electron (BSE) and secondary electron (SE) signals were mixed in a ratio that was expected to obtain a segmented 3D image with a realistic volume fraction of silicalite‐1. Second, after spatial alignment of the stacked FIB‐SEM data, the 3D image was smoothed using adaptive median and anisotropic nonlinear diffusion filters. Third, the image was segmented using the power watershed method coupled with a seeding algorithm based on geodesic reconstruction from the markers. If the resulting volume fraction did not match the target value quantified by chemical analysis of the sample, the BSE and SE signals were mixed in another ratio and the procedure was repeated until the target volume fraction was achieved. Otherwise, the segmented 3D image (replica) was accepted and its microstructure was thoroughly characterized with special attention paid to connectivity of the silicalite phase. In terms of the phase connectivity, Monte Carlo simulations based on the pure‐phase permeability values enabled us to calculate the effective permeability tensor, the main diagonal elements of which were compared with the experimental permeability. In line with the hypothesis proposed in our recent paper (?apek, P. et al. (2014) Comput. Mater. Sci. 89 , 142–156), the results confirmed that the existence of particle clusters was a key microstructural feature determining effective permeability.     

Sequential processing of quantitative phase images for the study of cell behaviour in real‐time digital holographic microscopy

Transmitted light holographic microscopy is particularly used for quantitative phase imaging of transparent microscopic objects such as living cells. The study of the cell is based on extraction of the dynamic data on cell behaviour from the time‐lapse sequence of the phase images. However, the phase images are affected by the phase aberrations that make the analysis particularly difficult. This is because the phase deformation is prone to change during long‐term experiments. Here, we present a novel algorithm for sequential processing of living cells phase images in a time‐lapse sequence. The algorithm compensates for the deformation of a phase image using weighted least‐squares surface fitting. Moreover, it identifies and segments the individual cells in the phase image. All these procedures are performed automatically and applied immediately after obtaining every single phase image. This property of the algorithm is important for real‐time cell quantitative phase imaging and instantaneous control of the course of the experiment by playback of the recorded sequence up to actual time. Such operator's intervention is a forerunner of process automation derived from image analysis. The efficiency of the propounded algorithm is demonstrated on images of rat fibrosarcoma cells using an off‐axis holographic microscope.     

Aroma profiles of five basil (Ocimum basilicum L.) cultivars grown under conventional and organic conditions

A headspace solid-phase microextraction (HS-SPME) method coupled to gas chromatography–ion trap mass spectrometry (GC–ITMS) has been developed and applied for profiling of volatile compounds released from five Ocimum basilicum L. cultivars grown under both organic and conventional conditions. Comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC×GC–TOFMS) was employed for confirmation of identity of volatiles extracted from the basil headspace by SPME.     

Tree Recovery in PIM Sparse Mode

A PIM–SM-built multicast tree must be restructured when the underlying unicast routing tables change. We describe the PIM–SM recovery mechanisms and evaluate the recovery performance, showing its dependence on a range of network and session parameters. Our results show that a substantial packet loss can be caused by nonreductive, benign events in the network, such as an addition of a new link. We propose and evaluate an improvement to the standard PIM–SM recovery procedure aimed to reduce the packet loss caused by the benign events. Our evaluation shows that the data loss caused by these events can be significantly decreased regardless of the topology and session parameters.     

Guided-wave Electro-optic X-type Switches: Symmetry,Switching Characteristics and Cross-talk

Abstract

The influence of branching asymmetry and electrode offset on the switching characteristics and cross-talk of X-type switches is analysed theoretically. The relationship between the switch symmetry (i.e. the existence of a plane or centre of inversion) and the switching characteristics is found. Cross-talk levels of slightly asymmetric Ti:LiNbO₃ switches are calculated.