One-step microwave synthesis of palladium-carbon nanotubes hybrids with improved catalytic performance

7 páginas, 7 figuras, 3 tablas.-- El pdf del artículo es la versión pre-print.A fast and easy one-step linker-free approach for the synthesis of palladium nanoparticle/multiwall carbon nanotube (Pd-NP/MWCNT)hybrid materials is described using microwave irradiation for the effective decomposition of Pd2dba3 complex in the presence of MWCNTs. High loadings of Pd nanoparticles (up to 40 wt.%) having sizes between 3 and 5 nm are deposited on the surface of MWCNTs within a time of only 2 minutess. The Pd-NP/MWCNT materials serve as efficient catalysts in C-C coupling as well as in hydrogenation reactions, all characterized by high conversion rates using a small amount of catalysts, high turnover frequency values and good recyclbility.Financial support from the Spanish Ministerio de Ciencia e Innovación (MICINN) and the European Regional Development Fund (ERDF) under projects CTQ2008-01784 and MAT2007-66927-C02-01, and the Gobierno de Aragón (DGAPI086- 08) is gratefully acknowledged. M.C. thanks MICINN for her Grant No. BES-2008-003503.Peer reviewe

Russian roulette with unlicensed fat-burner drug 2,4-dinitrophenol (DNP) : evidence from a multidisciplinary study of the internet, bodybuilding supplements and DNP users

BACKGROUND: 2,4-Dinitrophenol (DNP) poses serious health-risks to humans. The aims of this three-stage multidisciplinary project were, for the first time, to assess the risks to the general public from fraudulent sale of or adulteration/contamination with DNP; and to investigate motives, reasons and risk-management among DNP-user bodybuilders and avid exercisers. METHODS: Using multiple search-engines and guidance for Internet research, online retailers and bodybuilding forums/blogs were systematically explored for availability of DNP, advice offered on DNP use and user profiles. Ninety-eight pre-workout and weight-loss supplements were purchased and analysed for DNP using liquid-chromatography-mass-spectrometry. Psychosocial variables were captured in an international sample of 35 DNP users (26.06 ± 6.10 years, 94.3 % male) with an anonymous, semi-qualitative self-reported survey. RESULTS: Although an industrial chemical, evidence from the Internet showed that DNP is sold 'as is', in capsules or tablets to suit human consumption, and is used 'uncut'. Analytical results confirmed that DNP is not on the supplement market disguised under fictitious supplement names, but infrequently was present as contaminant in some supplements (14/98) at low concentration (<100mcg/kg). Users make conscious and 'informed' decisions about DNP; are well-prepared for the side-effects and show nonchalant attitude toward self-experimentation with DNP. Steps are often taken to ensure that DNP is genuine. Personal experience with performance- and appearance enhancing substances appears to be a gateway to DNP. Advice on DNP and experiences are shared online. The significant discrepancy between the normative perception and the actual visibility suggests that DNP use is-contrary to the Internet accounts-a highly concealed and lonesome activity in real life. Positive experiences with the expected weight-loss prevail over the negative experiences from side effects (all but two users considered using DNP again) and help with using DNP safely is considered preferable over scare-tactics. CONCLUSION: Legislation banning DNP sale for human consumption protects the general public but DNP is sold 'as is' and used 'uncut' by determined users who are not dissuaded from experimenting with DNP based on health threats. Further research with stakeholders' active participation is imperative for targeted, proactive public health policies and harm-reduction measures for DNP, and other illicit supplements

UNEQUAL PATTERNS OF DEVELOPMENT OF SUCCINATE-DEHYDROGENASE and ACETYLCHOLINESTERASE IN PURKINJE CELL BODIES and GRANULE CELLS ISOLATED IN BULK FROM THE CEREBELLAR CORTEX OF THE IMMATURE RAT 1

–A preparative procedure for the isolation in bulk of two cellular populations of the cerebellar cortex of the immature rat, the granule cells and the Purkinje cell bodies, is described. The procedure is used to delineate the developmental pattern of succinate-INT-reduclase (EC 1.3.99.1) and acetylcholinesterase (EC 3.1.1.7) in the crucial period of cerebellar maturation, i.e. between 12 and 19 days postnatally. Although the overall yield of neuronal RNA diminished with age, the proportion of RNA in the Purkinje cell body fraction increased while that in the granule cells decreased and microscopic examination of the fractions confirmed this result. The yields of succinate-INT-reductase and of acetylcholinesterase in the fractions paralleled the yields of RNA. A significant finding was the trend toward diminishing specific activities (units/Μg of RNA) with age of both enzymes in the Purkinje cell bodies as against the opposite, upward trend of their specific activities in the granule cells. An additional finding of interest was the different ratio of true acetylcholinesterase/total cholinesterase activity in the two cell types, with the granule cells consistently exhibiting higher true acetylcholinesterase values than the Purkinje cell bodies. The present report thus supplements the histoenzymological data on the developing rat cerebellum in that it reveals specific differences in the enzymatic development of two different cerebellar types, a finding which was greatly facilitated by the availability of the procedure for their bulk isolation.Peer Reviewedhttp://deepblue.lib.umich.edu/bitstream/2027.42/66200/1/j.1471-4159.1974.tb12210.x.pd

Quick and efficient extraction of uranium from a contaminated solution by a calixarene nanoemulsion

cited By 14This work aims to evaluate the efficiency of a calixarene emulsion for uranium extraction from a contaminated solution prior to apply such a delivery system to uranium skin decontamination. For this purpose, various experimental parameters that can influence the efficiency of the calixarene emulsion on uranium extraction were determined. The results show that the calixarene nanoemulsion effect can be observed after a very short time of contact with uranium-contaminated solution (5. min) and that it is still efficient in case of small volumes of contaminated solution. The pH of the contaminated solution was found to be the most important parameter affecting the calixarene nanoemulsion efficiency with a dramatic reduction of the uranium extraction rate in case of acidification of the contaminated medium. This lack of efficiency can be overcome by buffering the nanoemulsion continuous phase. The obtained results reveal that the calixarene nanoemulsion could represent a promising system for the emergency treatment of uranium cutaneous contamination. © 2010 Elsevier B.V

Association of a Love wave sensor to thin film molecularly imprinted polymers for nucleosides analogs detection

International audienceThe overall objective of this work is to develop and validate a quantitative, non-invasive therapeutic tool to detect selected urinary modified nucleosides as biomarkers of colorectal cancer chemotherapy and to monitor in fine the efficiency of the chemotherapy. Our methodology takes the advantage of high sensitivity of acoustic biosensor combined with high selectivity and robustness of thin molecularly imprinted polymer (MIP) film. In this paper we present a process based on a thin film of a MIP of adenosine 5'-monophosphate (AMP) coating on the sensor surface which is compatible with the acoustic wave propagation. Detection tests of AMP have been performed in aqueous media. The sensor response was recorded in terms of synchronous frequency and total insertion losses after both steps: extraction from, rebinding by the MIP layer. A frequency decrease of 6.875 Hz was recorded for 25μg/mL AMP concentration

Impact of the uranium (VI) speciation in mineralised urines on its extraction by calix[6]arene bearing hydroxamic groups used in chromatography columns

International audienceActinides determination in urine samples is part of the analyses performed to monitor internal contamination in case of an accident or a terrorist attack involving nuclear matter. Mineralisation is the first step of any of these analyses. It aims at reducing the sample volume and at destroying all organic compounds present. The mineralisation protocol is usually based on a wet ashing step, followed by actinides co-precipitation and a furnace ashing step, before redissolution and the quantification of the actinides by the appropriate techniques. Amongst the existing methods to perform the actinides co-precipitation, alkali-earth (typically calcium) precipitation is widely used. In the present work, the extraction of uranium(VI), plutonium(IV) and americium(III) from the redissolution solutions (called "mineralised urines") on calix[6]arene columns bearing hydroxamic groups was investigated as such an extraction is a necessary step before their determination by ICP-MS or alpha spectrometry. Difficulties were encountered in the transfer of uranium(VI) from raw to mineralised urines, with yield of transfer ranging between 0% and 85%, compared to about 90% for Pu and Am, depending on the starting raw urines. To understand the origin of such a difficulty, the speciation of uranium (VI) in mineralised urines was investigated by computer simulation using the MEDUSA software and the associated HYDRA database, compiled with recently published data. These calculations showed that the presence of phosphates in the "mineralised urines" leads to the formation of strong uranyl-phosphate complexes (such as UO2HPO4) which compete with the uranium (VI) extraction by the calix[6]arene bearing hydroxamic groups. The extraction constant of uranium (VI) by calix[6]arene bearing hydroxamic groups was determined in a 0.04 mol L-1 sodium nitrate solution (log K=4.86±0.03) and implemented in an extraction model taking into account the speciation in the aqueous phase. This model allowed to simulate satisfactorily the experimental uranium extraction data and to support the preliminary conclusions about the role of the phosphates present in mineralised urines. These calculations also showed that the phosphate/calcium ratio is a key parameter as far as the efficiency of the uranium (VI) extraction by the calix[6]arene columns is concerned. It predicted that the addition of CaCl2 in mineralised urines would release uranium (VI) from phosphates by forming calcium (II)-phosphate complexes and thus facilitate the uranium (VI) extraction on calix[6]arene columns. These predictions were confirmed experimentally as the addition of 0.1 mol L-1 CaCl2 to a mineralised urine containing naturally a high concentration of phosphate (typically 0.04 mol L-1) significantly increased the percentage of uranium (VI) extraction on the calix[6]arene columns. © 2015 Elsevier B.V. All rights reserved

Love Wave Sensor Based on Thin Film Molecularly Imprinted Polymer: Study of VOCs Adsorption

International audienceThe overall objective of this work is to develop and to validate a quantitative, non-invasive diagnosis tool to monitor the efficiency of colorectal cancer chemotherapy. This paper deals with the validation of a molecularly imprinted polymer (MIP) thin film’s coating process, allowing high sensitivity of the resulting microsensor. After description of the Love wave sensor and of the MIP coating process, the functionality of the resulting device is proved with electrical characterization. Deep characterization of the thin film - morphology and print effect - is proposed, based on dynamical responses observed under exposure to different vapors. Results point out a good reproducibility of polymeric films. MIP layers increased responses of sensors to vapors by a factor 3 to 4 compared to bare devices or to devices coated with non-imprinted polymer (NIP). For example, exposure to 4000mg/m3 (2126ppm) of ethanol in nitrogen induced a frequency shift of -1.4/-0.4kHz with MIP/NIP-coated sensor, respectively