899 resultados para High-performance Liquid Chromatography-mass Spectrometry (hplc-ms)


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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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The synthesis of a series of omega-hydroxyfatty acid (omega-OHFA) monomers and their methyl ester derivatives (Me-omega-OHFA) from mono-unsaturated fatty acids and alcohols via ozonolysis-reduction/crossmetathesis reactions is described. Melt polycondensation of the monomers yielded thermoplastic poly(omega-hydroxyfatty acid)s [-(CH2)(n)-COO-](x) with medium (n = 8 and 12) and long (n = 17) repeating monomer units. The omega-OHFAs and Me-omega-OHFAs were all obtained in good yield (>= 80%) and purity (>= 97%) as established by H-1 NMR, Fourier Transform infra-red spectroscopy (FT-IR), mass spectroscopy (ESI-MS) and high performance liquid chromatography (HPLC) analyses. The average molecular size (M-n) and distribution (PDI) of the poly(omega-hydroxyfatty acid)s (P(omega-OHFA)s) and poly(omega-hydroxyfatty ester) s (P(Me-omega-OHFA) s) as determined by GPC varied with organo-metallic Ti(IV) isopropoxide [Ti(OiPr)(4)] polycondensation catalyst amount, reaction time and temperature. An optimization of the polymerization process provided P(omega-OHFA) s and P(Me-omega-OHFA) s with M-n and PDI values desirable for high end applications. Co-polymerization of the long chain (n = 12) and medium chain (n = 8) Me-omega-OHFAs by melt polycondensation yielded poly(omega-hydroxy tridecanoate/omega-hydroxy nonanoate) random co-polyesters (M-n = 11000- 18500 g mol(-1)) with varying molar compositions.

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Indiscriminate and inappropriate use of pesticides in agriculture has been pointed out for increasing health problems and environmental damage. Considering that water resources are the principal destiny of those compounds after application, the present study presents optimization and validation of two simple and effi cient analytical methods for pesticides quantifi cation in both surface and groundwater. Were selected the pesticides more commonly used at Dourados (MS - Brazil), region with intense agricultural activity. Pesticides were preconcentrated by solid-phase extraction using C18 (500 mg) cartridges and then divided in two groups for elution and quantifi cation: 2.4-D and 2.4-DCP were eluted with methanol and quantifi ed by high performance liquid chromatography with ultra-violet detector (HPLC-UV) while atrazine, DIA, DEA, trifl uralin and methyl parathion were eluted with ethylacetate (1:1, v/v) and quantifi ed by gas chromatography with thermionic specifi c detector (GC-TSD). The methods showed satisfactory accuracy (76-107%) and precision (<12%) for the substances analyzed at the fortifi ed levels selected for the study, except for DIA (<51%). Study of pesticide stability also presented good results: C18 cartridges could be stored for at least for 21 days at -20ºC with no signs of the compounds degradability. Both methods limits of quantifi cation of the pesticides (0.22 - 0.48 μg L-1) are in accordance to the levels currently established by the Brazilian national legislation for pesticides in water. Although only the pesticide 2.4-D has been detected in two distinct collection points in the study period of time, this work warns for the requirement of systematical analysis of pesticides presence in water destined to human consume, principally in areas of intense agriculture activity. Such monitoring can provide subsidies for public environmental policies.

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Due to the large amount of pesticides applied in agriculture, mainly herbicides, there is a growing concern about a possible environmental contamination with these products, including water bodies. Given the above, the aim of the present work was to detect and quantify herbicides through multiresidue analysis in water samples collected in semi-artesian wells and springs in a rural area of the city of Jaboticabal (SP). Samples were collected from 32 wells and 13 water springs, in three different seasons: October 2010, February 2011 and May 2011. Additionally, samples at a residence in the urban area were also collected. Analysis using high performance liquid chromatography coupled to mass spectrometry was performed and herbicides ametryn, amicarbazone, clomazone, diclosulan, diuron, hexazinone, imazapic, imazapyr, isoxaflutole, S-metolachlor, sulfentrazone, sulfometuron-methyl, and tebuthiuron were evaluated. In semi-artesian wells, an incresed quantity of herbicides was found in comparison with the water springs. Among the tested herbicides, hexazinone, imazapyr and sulfentrazone were detected in measurable amounts in accordance with the analytical method applied, while clomazone was the most common herbicide being detected in more than 60% of the samples. Ametryn, diuron and amicarbazone herbicides were also detected. Diclosulan, imazapic, isoxaflutole, S-metolachlor, sulfometuron-methyl, and tebuthiuron were not detected in any sample. Inappropriate use of these products without prior knowledge of the behavior of the soil can lead to groundwaters and water springs contamination, thus an ongoing monitoring of this resource becomes very important.

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Synthacaine is a New Psychoactive Substance which is, due to its inherent psychoactive properties, reported to imitate the effects of cocaine and is therefore consequently branded as legal cocaine. The only analytical approach reported to date for the sensing of Synthacaine is mass spectrometry. In this paper, we explore and evaluate a range of potential analytical techniques for its quantification and potential use in the field screening Synthacaine using Raman spectroscopy, presumptive (colour) testing, High Performance Liquid Chromatography (HPLC) and electrochemistry. HPLC analysis of street samples reveals that Synthacaine comprises a mixture of methiopropamine (MPA) and 2-aminoindane (2-AI). Raman spectroscopy and presumptive (colour) tests, the Marquis, Mandelin, Simon's and Robadope test, are evaluated towards a potential in-the-field screening approach but are found to not be able to discriminate between the two when they are both present in the same sample, as is the case in the real street samples. We report for the first time a novel indirect electrochemical protocol for the sensing of MPA and 2-AI which is independently validated in street samples with HPLC. This novel electrochemical approach based upon one-shot disposable cost effective screen-printed graphite macroelectrodes holds potential for in-the-field screening for Synthacaine.

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Pós-graduação em Agronomia (Proteção de Plantas) - FCA

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)