Estudio del calzado laboral de uso más frecuente (2ª parte)

Sin duda alguna es de vital importancia el perfecto conocimiento del calzado por parte del podólogo, tanto de su morfología como de la influencia de éste sobre el pie. Teniendo en cuenta que ocupamos la mayor parte de nuestro tiempo en desarrollar una actividad profesional, fácilmente podremos deducir que el calzado laboral repercute en gran medida en el pie del usuario y, por lo tanto, también en su rendimiento.

Estudio del calzado laboral de uso más frecuente (Conclusión)

Sin duda alguna es de vital importancia el perfecto conocimiento del calzado por parte del podólogo, tanto de su morfología como de la influencia de éste sobre el pie. Teniendo en cuenta que ocupamos la mayor parte de nuestro tiempo en desarrollar una actividad profesional, fácilmente podremos deducir que el calzado laboral repercute en gran medida en el pie del usuario y, por lo tanto, también en su rendimiento.

Eletroforese capilar acoplada à espectrometria de massas (CE-MS): vinte anos de desenvolvimento

CE-MS has been increasingly used for analysis of a vast array of compounds. This article reviews the different electrophoretic modes, interfaces and mass analyzers that are commonly used in the CE-MS coupling, as well as the technique advantages and performance characteristics. A large compilation of CE-MS applications is also presented. Therefore, this review is both a guide for beginners and a collection of key references for people who are familiar to the technique. Furthermore, this is the first CE-MS review published in a Brazilian journal and marks the installation of the first two commercial CE-MS units in Sao Paulo State.

Processos físico-químicos em drenagem ácida de mina em mineração de carvão no sul do Brasil

Acid mine drainage generated from coal mine showed a pH of 3.2, high concentrations of SO4(2-), Al, Fe, Mn, Zn and minor As, Cd, Co, Cr, Cu, Ni and Pb. The major reduction in the concentration occurred for Al, As, Cr, Fe and Pb after the treatment with CaO. The evolution of these acid waters within the tributary stream showed decreasing concentration for all soluble constituents, except Al. This natural attenuation was controlled by pH (6.4 to 10.8) as a result of concurrent mixing with tributary stream and reaction with local bedrock that contains limestone. Aluminum increasing concentration during this evolution seems to be related to an input of Al-enriched waters due to the leaching of silicate minerals in alkaline conditions.

Evaluation of sample processing methods for the polar contaminant analysis of sewage sludge using liquid chromatography - mass spectrometry (LC/MS)

Monitoring of sewage sludge has proved the presence of many polar anthropogenic pollutants since LC/MS techniques came into routine use. While advanced techniques may improve characterizations, flawed sample processing procedures, however, may disturb or disguise the presence and fate of many target compounds present in this type of complex matrix before analytical process starts. Freeze-drying or oven-drying, in combination with centrifugation or filtration as sample processing techniques were performed followed by visual pattern recognition of target compounds for assessment of pretreatment processes. The results shown that oven-drying affected the sludge characterization, while freeze-drying led to less analytical misinterpretations.

MSPD procedure combined with GC-MS for the determination of procymidone, bifenthrin, malathion and pirimicarb in honey

A method based on matrix solid-phase dispersion and gas chromatography-mass spectrometry to determine procymidone, malathion, bifenthrin and pirimicarb in honey is described. The best results were obtained using 1.0 g of honey, 1.0 g of silica-gel as dispersant sorbent and acetonitrile as eluting solvent. The method was validated by fortified honey samples at three concentration levels (0.2, 0.5 to 1.0 mg kg-1). Average recoveries (n=7) ranged from 54 to 84%, with relative standard deviations between 3.7 and 8.5%. Detection and quantification limits attained by the developed method ranged from 0.02 to 0.08 mg kg-1 and 0.07 to 0.25 mg kg-1 for the honey, respectively.

Development and validation of a method for the analysis of tetracyclines in chicken-muscle by liquid chromatography-electrospray-mass spectrometry in tandem (LC-ESI-MS/MS)

A LC-ESI-MS/MS method was developed and validated according to the European Union decision 2002/657/EC, for the determination of tetracyclines (TCs) in chicken-muscle since Europe is one of the main markets for Brazilian products. Linearity of r > 0.9979, limits of quantification in the range of 7.0-35.0 ng/g, average recoveries of 89.38 - 106.27%, within-day and between-day precision were adequate for all TCs. The decision limit and the detection capability were 93.00-106.46 ng/g and 95.84-114.38 ng/g, respectively. This method is suitable for application in surveillance programmes of residues of TCs in chicken-muscle samples.

Uso da técnica HRICP-MS na avaliação dos isótopos de boro em eucalipto

The 10B isotope tracer technique is essential to study the B mobility in plants. Factors that can influence the quality of measured B isotope ratios were optimized experimentally using High Resolution Inductively Coupled Plasma Mass Spectrometry (HRICP-MS). An isotopically certified standard (NIST SRM-951) was used. The best combination was obtained using a resolution of 400, a RF power of 1250 W, followed by 15 measurements over a 10-s integration period each (15*10). Utilizing this approach it was possible to obtain a precision of 0.3 % in standard material and 2z % in the experimental samples. The results show the importance of establishing optimized work conditions before carrying out the analytical series.

Otimização e validação de método empregando quechers modificado e lc-esi-ms/ms para determinação de agrotóxicos em cebola

An evaluation of the pesticides extraction from onion using a modern sample preparation method (QuEChERS) and determination by liquid chromatography tandem mass spectrometry was carried out. All the calibration curves showed r>0.99. The recoveries ranged between 61.8 and 120.0% with relative standard deviation lower than 20% for all compounds. Due to the occurrence of matrix effect, the quantification was performed using matrix-matched calibration. The limits of quantification of the method were between 0.0005 and 0.05 mg kg-1. The method shows the advantages of not require the clean-up step and consume low volume of organic solvents, decreasing time, costs and residues.

A sensitive and robust lc-ms/ms method with monolithic column and electrospray ionization for the quantitation of efavirenz in human plasma: application to a bioequivalence study

An LC-MS/MS method has been developed for the determination of efavirenz (EFZ) in human plasma using hydrochlorothiazide as internal standard (I.S.). An ESI negative mode with multiple reaction-monitoring was used monitoring the transitions m/z 313.88→69.24 (EFZ) and 296.02→204.76 (I.S.). Samples were extracted using liquid-liquid extraction. The total run time was 2.0 min. The separation was achieved with HPLC-RP using a monolithic column. The assay was linear in the concentration range of 100 - 5000 ng mL-1. The mean recovery was 83%. Intra- and inter-day precision were < 9.5% and < 8.9%, respectively and accuracy was in the range ± 8.33%. The method was successfully applied to a bioequivalence study.

Avaliação da eficiência das técnicas ESI-MS e ATR/FTIR na determinação de adulteração de BX com querosene e óleo residual

Direct infusion electrospray ionization mass spectrometry in the negative ion mode, ESI(-)-MS and Fourier transform infrared spectroscopy (FTIR) were used together with partial least squares (PLS) as a tool to determine B3 adulteration (B3 - mixture of 3% v/v of biodiesel in diesel) with kerosene and residual oil.

Development and validation of a method for the analysis of Ochratoxin A in roasted coffee by liquid chromatography/electrospray-mass spectrometry in Tandem (LC/ESI-MS/MS)

A method using LC/ESI-MS/MS for the quantitative analysis of Ochratoxin A in roasted coffee was described. Linearity was demonstrated (r = 0.9175). The limits of detection and quantification were 1.0 and 3.0 ng g-1, respectively. Trueness, repeatability and intermediate precision values were 89.0-108.8%; 2.4-13.7%; 12.5-17.8%, respectively. To the best of our knowledge, this is the first report in which Ochratoxin A in roasted coffee is analysed by LC/ESI-MS/MS, contributing to the field of mycotoxin analysis, and it will be used for future production of Certified Reference Material.

Validação de método multirresíduo para determinação de pesticidas em alimentos empregando QuEChERS E UPLC-MS/MS

This paper presents a practical and rapid method which was validated for simultaneous quantification and confirmation of 29 pesticides in fruits and vegetables using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The samples were extracted following the method known as QuEChERS. Using the developed chromatographic conditions, the pesticides can be separated in less than 9 min. Two multiple reaction monitoring (MRM) assays were used for each pesticide. Four representative matrices (lettuce, tomato, apple and grapes) were selected to investigate the effect in recoveries and precision. Typical recoveries ranged from 70-120%, with relative standard deviation (RSDs) lower than 20%.

Desreplicação de alcaloides aporfínicos e oxoaporfínicos de Unonopsis guatterioides por ESI-IT-MS

The dereplication of aporphine and oxoaporphine alkaloids by direct infusion in ESI-IT-MSn system was applied for alkaloidal fractions of the Unonopsis guatterioides (Annonaceae). Its main advantage over other dereplication methods is the ability to quickly identify substances in complex mixtures without the use of coupled techniques and expensive databases. By only the fragmentation keys and comparison with literature data the aporphine alkaloids anonaine, asimilobine and nornuciferine were identified. The nornuciferine is being reported for the first time in Unonopsis. The oxoaporphine alkaloids liriodenine and lisycamine were identified in the alkaloidal fractions by comparison with the fragmentations of authentic samples.

Caracterização e classificação quanto ao risco ambiental do estéril da mina de cromita do município de Andorinha, Bahia

The mineral waste studied was host rock from a chromite mine located in Andorinha/Bahia, extracted and stockpiled in yards without specific application. Host rock was submitted to chemical analysis, XRD, SEM-EDS, IR and TGA and classified according to ABNT standards for solid waste classification. Analyses confirmed that this host rock, classified as ultrabasic, consists mainly of dolomite, calcite and diopside. Hazard assessment results showed this host rock should be classified as class II B - inert waste, important for its potential application in agriculture as a soil acidity correction agent.