Rapid and Green Analytical Method for the Determination of Quinoline Alkaloids from Cinchona succirubra Based on Microwave-Integrated Extraction and Leaching (MIEL) Prior to High Performance Liquid Chromatography

Quinas contains several compounds, such as quinoline alkaloids, principally quinine, quinidine, cinchonine and cichonidine. Identified from barks of Cinchona, quinine is still commonly used to treat human malaria. Microwave-Integrated Extraction and Leaching (MIEL) is proposed for the extraction of quinoline alkaloids from bark of Cinchona succirubra. The process is performed in four steps, which ensures complete, rapid and accurate extraction of the samples. Optimal conditions for extraction were obtained using a response surface methodology reached from a central composite design. The MIEL extraction has been compared with a conventional technique soxhlet extraction. The extracts of quinoline alkaloids from C. succirubra obtained by these two different methods were compared by HPLC. The extracts obtained by MIEL in 32 min were quantitatively (yield) and qualitatively (quinine, quinidine, cinchonine, cinchonidine) similar to those obtained by conventional Soxhlet extraction in 3 hours. MIEL is a green technology that serves as a good alternative for the extraction of Cinchona alkaloids.     

Metabolic Effects of Krill Oil are Essentially Similar to Those of Fish Oil but at Lower Dose of EPA and DHA,in Healthy Volunteers

The purpose of the present study is to investigate the effects of krill oil and fish oil on serum lipids and markers of oxidative stress and inflammation and to evaluate if different molecular forms, triacylglycerol and phospholipids, of omega-3 polyunsaturated fatty acids (PUFAs) influence the plasma level of EPA and DHA differently. One hundred thirteen subjects with normal or slightly elevated total blood cholesterol and/or triglyceride levels were randomized into three groups and given either six capsules of krill oil (N = 36; 3.0 g/day, EPA + DHA = 543 mg) or three capsules of fish oil (N = 40; 1.8 g/day, EPA + DHA = 864 mg) daily for 7 weeks. A third group did not receive any supplementation and served as controls (N = 37). A significant increase in plasma EPA, DHA, and DPA was observed in the subjects supplemented with n-3 PUFAs as compared with the controls, but there were no significant differences in the changes in any of the n-3 PUFAs between the fish oil and the krill oil groups. No statistically significant differences in changes in any of the serum lipids or the markers of oxidative stress and inflammation between the study groups were observed. Krill oil and fish oil thus represent comparable dietary sources of n-3 PUFAs, even if the EPA + DHA dose in the krill oil was 62.8% of that in the fish oil.     

A Method for Evaluating Lignin Mobility Distributions Obtained by Capillary Zone Electrophoresis

Abstract

The profile of the mobility distribution of lignin-containing samples depends on type of sample. To facilitate comparison, a procedure for determining the average mobility (μ_av), i.e. the average charge density, of lignin is presented. The procedure is applied to black liquor (Sb), isolated dissolved lignin (Sd) and isolated residual (Sr) lignin samples, obtained from flow-through kraft cooks of softwood. The μ_av of the isolated lignin samples is compared with the concentration of phenol and carboxyl groups and relative molecular size. As the cook proceeds the μ_av for a particular type of lignin sample increases, reflecting an increase in average charge density. The μ_av, measured at pH 12, decreases in the order Sd>Sb>Sr, except at the end of the cook, when the average charge densities of the Sb and Sr samples are similar. Associations between lignin and carbohydrate fragments are proposed to cause the lower mobility of black liquor compared to isolated dissolved lignin. Characterisations performed at pH 10 indicate that the isolated dissolved lignin samples may have a higher pK_a in the middle of the cook than the other samples.     

Preparation of near-infrared absorbing composites comprised of conjugated macroligands on the surface of PbS nanoparticles

We report a facile macroligand strategy towards the synthesis of low-bandgap inorganic-organic composites comprised of semiconductor PbS nanoparticles and functional copolymers. For this, thiol-functional thiophene-based macroligands have been used as coligands for PbS nanoparticles. Thus, solution processable organic-inorganic hybrid materials with absorption in the near-infrared have been obtained. The resulting nanoparticle-polymer composites were characterized in detail by optical and FT-IR spectroscopy as well as TEM showing their potential as novel functional inorganic-organic hybrid materials when applied in initial proof-of-concept hybrid photovoltaic devices.     

Homogeneous dispersion of SiO2 nanoparticles in an hydrosoluble polymeric network

The main difficulty still encountered in the elaboration of polymer/silica nanocomposites is the control of the nanoparticles dispersion homogeneity and the stability of the nanoparticle dispersion in the surrounding substance. The innovative point of this work is the elaboration of hybrid networks in aqueous solution performed with ASE (alkali swellable emulsion) thickeners grafted with silica nanoparticles. The thickening ability of the polymer should favour silica nanoparticles dispersion in fluid matrices. Two ASE copolymers were realised by copolymerisation in emulsion of MA (methacrylic acid) and EA (ethyl acrylate) and/or TFEM (trifluoroethyl methacrylate). The substitution of a part of EA by TFEM gave fluorinated ASE copolymers. Their free acid functions were then coupled with different ratio of amine functionalized silica nanoparticles to afford nanocomposites. The amounts of silica nanoparticles in the copolymers were determined by thermogravimetric experiments. Depending on the silica nanoparticles/copolymer ratio in basic aqueous solutions we achieved stable translucent gel like aqueous suspensions of silica nanoparticles containing 1 wt.% of the polymer/SiO₂ nanocomposite.     

Mycotoxin occurrence in feed and feed raw materials worldwide: long‐term analysis with special focus on Europe and Asia

During an 8‐year period, 17 316 samples of feed and feed raw materials from all over the world were analysed for contamination with aflatoxins, ochratoxin A, zearalenone, deoxynivalenol and fumonisins. Overall, 72% of the samples tested positive for at least one mycotoxin and 38% were found to be co‐contaminated. Mycotoxin concentrations were generally low and the majority of the samples were compliant with the most stringent EU guidance values or maximum levels for mycotoxins in feed. However, in their present state these regulations do not address co‐contamination and associated risks. Long‐term trends are difficult to establish as strong yearly variations were observed regarding mycotoxin prevalence and contamination levels. In some cases unusual weather conditions can be linked with high observed mycotoxin loads. An exception to this rule is South‐East Asia, where a steady increase of aflatoxin prevalence has been observed. The percentage of aflatoxin‐positive samples in this region rose from 32% in 2005 to 71% in 2011. © 2013 Society of Chemical Industry     

The Importance of Crosslinking and Glass Transition Temperature for the Mechanical Strength of Nanofibers Obtained by Green Electrospinning

Crosslinked particles containing butyl acrylate, methyl methacrylate, and allyl methacrylate are prepared by free‐radical emulsion polymerization. The glass transition temperatures of the polymers are varied by the crosslinking densities in the latex particles. Aqueous acrylate dispersions with polymers of different glass transition temperatures are electrospun with PVA as the matrix polymer. The effects of crosslinking density and T_g on the structure and mechanical properties of the fibers are studied. Crosslinking of unreacted allyl groups is induced by UV irradiation to stabilize the fibers by interparticle crosslinking. Both the ability to undergo interparticle crosslinking and the E modulus depend on the merging of the particles during the electrospinning process.

     

Rhodium‐Catalyzed Homogeneous Reductive Amidation of Aldehydes

The catalytic reductive amidation of an aldehyde (hexanal) with an amide (acetamide) is reported. Apart from the desired N‐hexylacetamide, the two isomeric unsaturated intermediates as well as hexanol are produced together with higher mass products that arise from aldol condensation and diamide coupling of the aldehyde. Screening of different catalyst precursor salts, ligands and reaction conditions led to the finding that the catalytic system based on the (cyclooctadiene)rhodium chloride dimer, [Rh(cod)Cl]₂, in combination with the ligand xantphos and an acid co‐catalyst results in high selectivity for the desired product. Under optimized conditions nearly full conversion is reached with high selectivity to the desired N‐alkylamide and with a very high N ‐ alkylamide/alcohol ratio, while producing only small amounts of by‐products. The scope of the reaction has been investigated using different amides as well as aldehydes; the results show the general applicability of this novel reaction, but with electron‐withdrawing amides the selectivity to N‐alkylamide is lower. NMR studies showed that the nucleophilic addition of acetamide to hexanal is acid catalyzed, forming N‐(1‐hydroxyhexyl)acetamide in equilibrium with both hexanal and the dehydrated unsaturated imides. A catalytic mechanism is proposed in which a strong acid such as HOTs acts as a co‐catalyst by establishing a rapid chemical equilibrium between the aldehyde, acetamide and the intermediates. Furthermore, it is proposed that the presence of acid causes a change in catalytic species, enabling a cationic Rh/xantphos hydrogenation catalyst to selectively hydrogenate the intermediates to N‐hexylacetamide in the presence of hexanal.     

Intercomparisons of Mobility Size Spectrometers and Condensation Particle Counters in the Frame of the Spanish Atmospheric Observational Aerosol Network

Red Española de DMAs Ambientales (REDMAAS), the Spanish network of environmental differential mobility analyzers (DMAs), currently comprises six research groups involved in the measurement of atmospheric aerosol size distributions by means of DMAs. The aim of this network is to guarantee the good quality and comparability of the routine measurements carried out at each location and in diverse environments across Spain. In order to achieve this objective, one of its main activities is the annual intercomparison of mobility size spectrometers used within the network (five units of scanning mobility particle sizers [SMPS] and one ultrafine particle monitor [UFPM]). Here we report the 2main results obtained during the 2010–2012 campaigns, including a study on particle deposition in dryers used in ambient air sampling systems. In general, all instruments showed good performance with deviations in accepted tolerance. The intercomparisons have been proved to be a useful exercise to detect instrument problems, such as incorrect calibrations. DMA calibration checks were performed with polystyrene latex reference particles. Deviations of less than 1% were observed during the first year, which increased 4.7% during the last campaign. Some differences among the responses of different condensation particle counter (CPC) models were encountered, being mainly connected to the intrinsic characteristics of each counter. The comparison of UFPM with CPCs has given good results. The SMPS intercomparisons, especially for particles above 20 nm, have been within +/?15% tolerance. Regarding particle deposition in dryers used in sampling systems, particle penetration was lower than predicted by the recommended model. This result was probably due to the fact that not all the possible mechanisms were considered in the model.

Copyright 2015 American Association for Aerosol Research