M��todos para an��lises de HPA e BTEX em ��guas subterr��neas de postos de revenda de combust��veis: um estudo de caso em Campo Grande, MS, Brasil

Two methods using headspace solid-phase microextraction and gas chromatography - mass spectrometry were developed for the determination of polycyclic aromatic hydrocarbons (PAH) and BTEX. Best results were obtained using DVB/CAR/PDMS fiber, with 10 min extraction at 25 ��C and 0.15 min desorption at 260 ��C (BTEX), and PDMS/DVB fiber, with 60 min extraction at 90 ��C, 10% NaCl and 5 min desorption at 270 ��C (PAH). LOD intervals were 3x10-2 - 5x10-2 ��g L-1 (BTEX) and 1.6x10-3 - 1.4 ��g L-1 (PAH). The methods were applied to forty-five groundwater samples from monitoring wells of gas stations and only benzene level exceeded the limit established by Brazilian regulations.

An��lise de f��rmacos em ��guas por SPE-UPLC-ESI-MS/MS

A method was developed for the analysis of 31 pharmaceutical compounds in Lisbon's drinking water system, using solid-phase extraction (SPE) and ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS). The method was validated through estimation of the linearity range, method detection and quantification limits, matrix effects, precision and accuracy. The method detection and quantification limit ranges were 0.009-10 and 0.03-33 ng/L, respectively. Analytes were quantified in water samples collected from the EPAL (Empresa Portuguesa das ��guas Livres S.A.) supply system. Carbamazepine, atenolol, sulfadiazine, sulfamethazine, sulfapyridine, sulfamethoxazole, acetaminophen, caffeine and erythromycin were quantified in the analysed samples.

LC/ESI-MS method applied to characterization of flavonoids glycosides in B. forficata subsp. pruinosa

Bauhinia forficata is used in folk medicine for its hypoglycemiant effect. In the south of Brazil, the subspecies pruinosa is found in a region with the characteristic flora, pampa biome. This species has been consumed by the local population as a tea for diabetes treatment. We studied the chemical composition of hydroethanolic extracts using LC/ESI-MS. The leaf extracts were prepared by percolation with 50% (v/v) ethanol. The chromatographic analyses were performed using a reverse-phase system, gradient elution with acetonitrile:phosphoric acid 0.05%, and ESI-MS in the positive ion mode. The chemical profile of the flavonoids was suggested to involve four quercetin and kaempferol glycosides.

Determina����o de res��duos de agrot��xicos em leite bovino empregando m��todo QuEChERS modificado e GC-MS/MS

Considering the possibility that pesticides used in cattle raising produce residues in milk and cause harm to public health, this study developed a multiresidue method for determination of pesticide residues in bovine milk, using a modified QuEChERS method for sample preparation, and quantification by GC-MS/MS. The method proved to be efficient, resulting in satisfactory recoveries in the range 71.1 to 117.4%, for 45 of the 48 compounds analyzed with RSD values < 17.3%. The method LOD and LOQ were3.0 and 10.0 ��g L-1, respectively, except for cyfluthrin which showed 7.5 and 25.0 ��g L-1.

Determina����o de bromo e iodo em alga marinha comest��vel por ICP-MS ap��s decomposi����o por combust��o iniciada por micro-ondas

A method based on microwave-induced combustion (MIC) was applied for the decomposition of different types of edible seaweed (Nori, Hijiki and Wakame) for subsequent determination of bromine and iodine by inductively coupled plasma mass spectrometry (ICP-MS). Decomposition of 500 mg of each sample was achieved in less than 30 min. A single and diluted solution (150 mmol L-1 (NH4)2CO3) was used for the absorption of both analytes and a reflux step of 5 min was applied to improve analyte recoveries. Accuracy was evaluated using certified reference materials and agreement was between 103 and 108% for both elements.

LC-MS/MS method applied to preclinical pharmacokinetic investigation of olanzapine-loaded lipid-core nanocapsules

In spite of different methods reported in the literature to determine olanzapine in biological fluids, all of them used high volumes of plasma. Therefore, the purpose of this paper was to develop an LC-MS/MS method using small plasma volume (0.1 mL) to apply in a preclinical pharmacokinetic investigation. The method was linear over the concentration ranges of 10 - 1000 ng mL-1. Extraction recoveries, stability, and validation parameters were evaluated. Results were within the acceptable limits of international guidelines. A significant decrease in clearance led to a significant 2.26-times increase in AUC0 - 6h of olanzapine-loaded lipid-core nanocapsules compared with free-olanzapine.

Optimization of chromatographic conditions and comparison of extraction efficiencies of four different methods for determination and quantification of pesticide content in bovine milk by UFLC-MS/MS

This paper describes the optimization of a multiresidue chromatographic analysis for the identification and quantification of 20 pesticides in bovine milk, including three carbamates, a carbamate oxime, six organophosphates, two strobilurins, a pyrethroid, an oxazolidinedione, an aryloxyphenoxypropionate acid/ester, a neonicotinoid, a dicarboximide, and three triazoles. The influences of different chromatographic columns and gradients were evaluated. Furthermore, four different extraction methods were evaluated; each utilized both different solvents, including ethyl acetate, methanol, and acetonitrile, and different workup steps. The best results were obtained by a modified QuEChERS method that lacked a workup step, and that included freezing the sample for 2 hours at -20 &#186;C. The results were satisfactory, yielding coefficients of variation of less than 20%, with the exception of the 50 ��g L-1 sample of famoxadone, and recoveries between 70 and 120%, with the exception of acephate and bifenthrin; however, both analytes exhibited coefficients of variation of less than 20%.

HS-SPME-GC-MS ANALYSIS OF VOLATILE AND SEMI-VOLATILE COMPOUNDS FROM DRIED LEAVES OF Mikania glomerata Sprengel

This paper reports on the identification of volatile and semi-volatile compounds and a comparison of the chromatographic profiles obtained by Headspace Solid-Phase Microextraction/Gas Chromatography with Mass Spectrometry detection (HS-SPME-GC-MS) of dried leaves of Mikania glomerata Sprengel (Asteraceae), also known as 'guaco.' Three different types of commercial SPME fibers were tested: polydimethylsiloxane (PDMS), polydimethylsiloxane/divinylbenzene (PDMS/DVB) and polyacrylate (PA). Fifty-nine compounds were fully identified by HS-SPME-HRGC-MS, including coumarin, a marker for the quality control of guaco-based phytomedicines; most of the other identified compounds were mono- and sesquiterpenes. PA fibers performed better in the analysis of coumarin, while PDMS-DVB proved to be the best choice for a general and non-selective analysis of volatile and semi-volatile guaco-based compounds. The SPME method is faster and requires a smaller sample than conventional hydrodistillation of essential oils, providing a general overview of the volatile and semi-volatile compounds of M. glomerata.

DIRECT INFUSION ESI-MS APPLIED IN THE DETECTION OF BYPRODUCTS DUE TO REDUCTIVE DEGRADATION OF ACETAMIPRID BY ZERO-VALENT IRON

This study investigated the reductive degradation of acetamiprid (5 mg L-1) in aqueous medium (at pH 2.0) induced by zero-valent iron (50 mg). The process was monitored using high-performance liquid chromatography (HPLC) to determine the degradation rate as a function of reaction time, and direct infusion electrospray ionization mass spectrometry (DI-ESI-MS) to search for (and potentially characterize) any possible byproducts formed during degradation. The results obtained via HPLC showed that after 60 min, the degradation of the substrate reached nearly 100% in an acidic medium, whereas the mineralization rate (as determined by total organic carbon measurements) was as low as 3%. Data obtained by DI-ESI-MS showed that byproducts were formed mainly by insertions of hydrogen atoms into the nitrile, imine, and pyridine ring moieties, in addition to the observation of chlorine substitution by hydrogen replacement (hydrodechlorination) reactions.

Astrological prognostications in MS Beinecke 558: "Sonday prime drye wether"

Tutkimukseni k��sittelee 1500-luvun keskivaiheilla kirjoitettua englanninkielist�� k��sikirjoitusta (New Haven, Yale University, Beinecke Rare Book and ManuscriptLibrary MS 558). Olen ty��ss��ni laatinut k��sikirjoituksesta kuvauksen, joka sis��lt����esimerkiksi listan k��sikirjoituksen sis��lt��mist�� teksteist�� sek�� k��sikirjoituksen p����kirjurin k��sialan paleografisen analyysin. Tarkastelemani k��sikirjoitus sis��lt���� paljon astronomista ja astrologista materiaalia. Keskityn erityisesti k��sikirjoituksen sis��lt��miin astrologisiin ennustusteksteihin, jotkaolen jakanut kuuteen kategoriaan. Luokitteluni perustuu osittain Laurel Meansin ja Irma Taavitsaisen tutkimuksiin, jotka koskevat keskienglanninkielist�� astrologista materiaalia.Ty��ss��ni olen soveltanut n��it�� tutkimuksia uuden ajan alun materiaaliin. Olen my��s tarkastellut k��sikirjoituskulttuurin ja kirjapainokulttuurin vuorovaikutusta viideneditoimani esimerkkitekstin kautta. Tutkimustulosteni perusteella k��sikirjoituskulttuuria ja kirjapainokulttuuria ei tulisi n��hd�� vastakohtina. Niiden v��list�� vuorovaikutusta tulisi jatkossa tutkia tarkemmin, sill�� n��in voitaisiin saada uutta tietoa tekstien levitt��misest�� ja levi��misest�� sek�� Englannissa ett�� koko Euroopassa kirjapainotaidon yleistymisen ensimm��isin�� vuosisatoina. T��llaisessa tutkimuksessa tulisi k��ytt���� niin m����r��llisi�� kuin laadullisiakin menetelmi�� ja ottaa huomioon kirjojen luonne sek�� henkisin�� ja taiteellisina tuotoksina ett�� fyysisin�� esinein��.

Desenvolvimento e aplica����o de m��todo GC-MS/MS para an��lise simult��nea de 17 HPAs em material particulado atmosf��rico

Os hidrocarbonetos polic��clicos arom��ticos (HPAs) est��o associados ao aumento da incid��ncia de diversos tipos de c��nceres no homem. Essas mol��culas s��o formadas principalmente na queima incompleta de mat��ria org��nica, sendo encontradas em todos os compartimentos ambientais. ��rg��os regulamentadores das ��reas ambiental e de sa��de ocupacional consideram 17 HPAs como contaminantes atmosf��ricos priorit��rios. Este trabalho apresenta um m��todo para an��lise simult��nea destes HPAs utilizando-se a cromatografia a g��s acoplada �� espectrometria de massas operando no modo tandem (GC-MS/MS). Os limites de detec����o e quantifica����o do m��todo mostraram-se at�� 5 vezes inferiores aos obtidos no m��todo GC-MS (SCAN). O m��todo mostrou-se seletivo para an��lise de HPAs em extratos de amostras de material particulado atmosf��rico. Uma an��lise comparativa de dois sistemas de solventes (diclorometano/metanol 4:1 v/v e hexano/acetona 1:1 v/v) para a extra����o de HPAs, utilizando amostras de material particulado atmosf��rico, revelou que ambas as misturas de solventes possuem poder de extra����o semelhante. Os resultados sugerem que �� poss��vel realizar extra����o de HPAs de material particulado atmosf��rico em ultra-som com a mistura hexano/acetona (1:1), que �� menos t��xica em rela����o �� mistura diclorometano/metanol (4:1), bastante utilizada nestas an��lises, sem perdas significativas na exatid��o do m��todo.

Capacita����o do m��dico para comunicar m��s not��cias �� crian��a

O movimento de humaniza����o na sa��de impulsionou pesquisas sobre a inclus��o de assuntos pol��micos nos curr��culos m��dicos, assim como de estrat��gias inovadoras para capacitar futuros profissionais. Com o objetivo de incluir no curr��culo atividades que habilitem os alunos de medicina a enfrentar situa����es dif��ceis, este estudo investigou a opini��o de m��dicos que atendem crian��as a respeito de como dar �� crian��a informa����es sobre doen��as de progn��stico incerto e como os profissionais se instrumentaram para enfrentar essas situa����es. Para tanto, 53 m��dicos responderam a um question��rio semi-estruturado. A maioria dos m��dicos opinou que a crian��a tem direito a essas informa����es e 70% da amostra j�� haviam enfrentado essa situa����o. Independentemente do tempo de formados, 48% dos sujeitos discutiram o assunto na gradua����o e resid��ncia, mas apenas 30% relataram ter recebido habilita����o espec��fica. Os m��dicos mais velhos disseram ter aprendido observando modelos. Discute-se a necessidade de contemplar novos conhecimentos cient��ficos e novas estrat��gias de aprendizagem, como o role-playing, para t��picos que, ao lado do conhecimento cient��fico, envolvem fatores emocionais e de ordem ��tica e legal.

Uso do protocolo Spikes no ensino de habilidades em transmiss��o de m��s not��cias

O termo "m�� not��cia" designa qualquer informa����o transmitida ao paciente ou a seus familiares que implique, direta ou indiretamente, alguma altera����o negativa na vida destes. Por ser uma tarefa t��o estressante, muitos m��dicos a evitam ou a realizam de maneira inadequada. Esse fato traz in��meras consequ��ncias negativas para o paciente e seus familiares. Embora seja objeto de estudo em diversos cursos de Medicina em n��vel internacional, o tema ainda �� pouco abordado por professores e estudantes no contexto brasileiro. O protocolo Spikes descreve de maneira did��tica seis passos para comunicar m��s not��cias. Esses passos foram utilizados em aula para alunos do terceiro semestre do curso de Medicina da Universidade Estadual do Cear��. Em seguida, os alunos avaliaram o m��todo por meio de perguntas abertas. De maneira geral, foi considerado um modelo v��lido, apesar de serem consideradas poss��veis limita����es, como a necessidade de ser individualizado e adaptado a cada situa����o.

Treinamento m��dico para comunica����o de m��s not��cias: revis��o da literatura

Nos ��ltimos anos, diretrizes para a comunica����o m��dica de m��s not��cias aos pacientes foram publicadas. Treinamentos para esta tarefa passaram a ser inclu��dos nos curr��culos de gradua����o, especializa����o e educa����o m��dica continuada. O objetivo desta revis��o foi avaliar as evid��ncias existentes na literatura sobre a efic��cia destes treinamentos. Apenas sete estudos controlados, quatro dos quais randomizados, foram encontrados. Quatro deles indicam melhora dos aprendizes que foram treinados. Estes achados mostram que o treinamento em comunica����o de m��s not��cias pode ser eficaz para m��dicos e estudantes, mas h�� importantes limita����es que impedem conclus��es definitivas. Estas limita����es s��o discutidas.