Desenvolvimento e validação de metodologia de análise de misturas biodiesel: diesel utilizando cromatografia gasosa-espectrometria de massas

The aim of this work was to develop and validate a method of analysis of biodiesel:diesel blends using HRGC-MS in SIM mode. The proposed method is applicable to biodiesel from linoleic oils, such as soybean oil. The following results were obtained: linearity over the methyl linoleate concentration range of 250-2500 mg L-1 (R² > 0.999); limits of detection and quantification of 2 and 5 mg L-1, respectively; recovery from 82 to 96% of biodiesel in diesel and repeatability < 2% (RSD). Comparison between two operators showed that it is not necessary the same operator to do the analysis.

Migration of Tinuvin P, a UV stabilizer, from PET bottles into fatty-food simulants

Tinuvin P migration from Polyethyleneterephthalate (PET) bottles was investigated using several fatty-food simulants such as olive oil, soybean oil, n-heptane and iso-octane, at exposure conditions of 2-10 days at 40 degrees C (total immersion). The stability of several UV stabilizers (BHT, Cyasorb UV 5411, Tinuvin P, Tinuvin 326 and Tinuvin 327) in n-heptane and iso-octane was also studied. After 10 days at 40 degrees C, losses of 6% and 20% in iso-octane and n-heptane respectively, were verified for Tinuvin P. Other UV stabilizers at the same experimental conditions showed higher losses (up to 30% for Tinuvin 327). These results confirm that, when carrying out specific migration studies, the stability of the substance of interest should be established in the food simulant to avoid underestimating the real migration behaviour. In order to quantify UV stabilizer migration, n-heptane and iso-octane solutions were concentrated and directly analysed by SIM mode GC-MS. For olive and soybean oils, Tinuvin P was isolated using size-exclusion chromatography and quantified by SIM mode GC-MS. Iso-octane proved to be a move suitable fatty-food simulant than n-heptane for the migration study of Tinuvin P from PET. Higher levels of Tinuvin P migrated to olive and soybean oils rather than to n-heptane. These results suggest that the MERCOSUL recommended official methods for specific migration studies should be revised since the migration levels using n-heptane as a fatty-food simulant could be underestimated when compared to edible oils. Copyright (C) 1999 John Wiley & Sons, Ltd.

Determination of buprofezin, pyridaben, and tebufenpyrad residues by gas chromatography mass-selective detection in clementine citrus

A gas chromatography-mass-selective (GC-MS) detection method to determine buprofezin, pyridaben, and tebufenpyrad on the pulp, peel, and whole fruit of clementines is described. The extraction/partition procedure was performed in one step and no cleanup was necessary with the GC-MS in the SIM-mode pesticide determination. Recovery ranged from 75 to 124% with coefficients of variance ranging between 1 and 13%. The limit of determination was 0.01 mg/kg for all pesticides. The field trials showed a similar degradative behavior for all active ingredients (AI), with a great residue decrease during the first week and stability in the second. Just after treatment buprofezin and tebufenpyrad showed lower residues than the maximum residue limit (MRL) fixed in Italy, while pyridaben was below the MRL after a week.

Quantification of sex pheromone from Anocentor nitens by gas chromatography-mass spectrometry-selected ion monitoring

Two highly sensitive and selective methods based on gas chromatography coupled to mass spectrometry (GC-MS) in the selected ion monitoring (SIM) mode have been developed for the quantification of 2,6-dichlorophenol (2,6-DCP), a sex pheromone of the tick females of Anocentor nitens. Standard addition method and calibration curve techniques using 5-bromine-4-hydroxy-3- methoxybenzaldehyde (5-BrV) as internal standard (IS) afforded detection limit of 0.1ngml-1. The calibration curve was linear over the concentration range from 0.5 to 500ngml-1 for 2,6-DCP. Results show that the concentration range of sex pheromone in the extracts samples was 1.08-10.35ngml-1. The methods developed provided reliable procedures to determine amounts of 2,6-DCP present in ticks. © 2003 Elsevier B.V. All rights reserved.

Método multiresiduo para determinar pesticidas en frutas por extracción con fluido supercrítico

A rapid and reliable method for the determination of 25 compounds selected from four classes of pesticides in samples of fresh apples, grapes, pears, and strawberries purchased at a local supermarket, is presented. The study describes two different methods of extraction: solid-liquid extraction with acetone and supercritical fluid extraction. Clean-up was based on aminopropyl cartridge extraction followed by gas chromatography with an electron capture detector for simultaneous determinations. Confirmatory analysis was carried out by gas chromatography with mass spectrometry in the selected-ion monitoring (SIM) mode. Extraction efficiencies were directly compared and the methods were applied to the analysis of real samples. Recoveries for a majority of pesticides from standard samples at enrichment levels of 0.04-0.10 mg/ kg ranged from 77 to 96 % for both methods. The supercritical fluid extraction method showed good limits of detection (less than 0.01 mg/kg, depending on the pesticide and matrix) as well as minimizing environmental concerns, time, and laboratory effort. © 2006 Centro de Información Tecnológica.

Biomimetic in vitro oxidation of lapachol: A model to predict and analyse the in vivo phase I metabolism of bioactive compounds

The bioactive naphtoquinone lapachol was studied in vitro by a biomimetic model with Jacobsen catalyst (manganese(III) salen) and iodosylbenzene as oxidizing agent. Eleven oxidation derivatives were thus identified and two competitive oxidation pathways postulated. Similar to Mn(III) porphyrins, Jacobsen catalyst mainly induced the formation of para-naphtoquinone derivatives of lapachol, but also of two ortho-derivatives. The oxidation products were used to develop a GC MS (SIM mode) method for the identification of potential phase I metabolites in vivo. Plasma analysis of Wistar rats orally administered with lapachol revealed two metabolites, alpha-lapachone and dehydro-alpha-lapachone. Hence, the biomimetic model with a manganese salen complex has evidenced its use as a valuable tool to predict and elucidate the in vivo phase I metabolism of lapachol and possibly also of other bioactive natural compounds. (C) 2012 Elsevier Masson SAS. All rights reserved.

La Revue musicale.

Merged into La Revue musicale. Sim.

al-Dafʼ al-matīn fī al-radd ʻalá ḥaḍrat Qāsim Bik Amīn ʻan taḥrīr al-marʼah [microform] /

Microfilm.

Kitāb dīwān Ṣafī al-Dīn Abū al-Muḥāsin ʻAbd al-ʻAzīz ibn Sarāyā ibn Abī al-Qāsim al-Ḥillī.

Mode of access: Internet.

Medicina Britannica; or A treatise on such physical plants, as are generally to be found in the fields or gardens in Great Britain: containing a particular account of their nature, virtues and uses : Together with the observations of the most learned physicians ... communicated to the late ... Mr. Ray, and Dr. Sim. Pauli ...

Includes note by John Cruso.

Samchʻŏk Sim Ssi sebo.

Movable type.

Structural Connectivity Of The Default Mode Network And Cognition In Alzheimer׳s Disease.

Disconnectivity between the Default Mode Network (DMN) nodes can cause clinical symptoms and cognitive deficits in Alzheimer׳s disease (AD). We aimed to examine the structural connectivity between DMN nodes, to verify the extent in which white matter disconnection affects cognitive performance. MRI data of 76 subjects (25 mild AD, 21 amnestic Mild Cognitive Impairment subjects and 30 controls) were acquired on a 3.0T scanner. ExploreDTI software (fractional Anisotropy threshold=0.25 and the angular threshold=60°) calculated axial, radial, and mean diffusivities, fractional anisotropy and streamline count. AD patients showed lower fractional anisotropy (P=0.01) and streamline count (P=0.029), and higher radial diffusivity (P=0.014) than controls in the cingulum. After correction for white matter atrophy, only fractional anisotropy and radial diffusivity remained significantly lower in AD compared to controls (P=0.003 and P=0.05). In the parahippocampal bundle, AD patients had lower mean and radial diffusivities (P=0.048 and P=0.013) compared to controls, from which only radial diffusivity survived for white matter adjustment (P=0.05). Regression models revealed that cognitive performance is also accounted for by white matter microstructural values. Structural connectivity within the DMN is important to the execution of high-complexity tasks, probably due to its relevant role in the integration of the network.

Whole Cortical And Default Mode Network Mean Functional Connectivity As Potential Biomarkers For Mild Alzheimer's Disease.

The search for an Alzheimer's disease (AD) biomarker is one of the most relevant contemporary research topics due to the high prevalence and social costs of the disease. Functional connectivity (FC) of the default mode network (DMN) is a plausible candidate for such a biomarker. We evaluated 22 patients with mild AD and 26 age- and gender-matched healthy controls. All subjects underwent resting functional magnetic resonance imaging (fMRI) in a 3.0 T scanner. To identify the DMN, seed-based FC of the posterior cingulate was calculated. We also measured the sensitivity/specificity of the method, and verified a correlation with cognitive performance. We found a significant difference between patients with mild AD and controls in average z-scores: DMN, whole cortical positive (WCP) and absolute values. DMN individual values showed a sensitivity of 77.3% and specificity of 70%. DMN and WCP values were correlated to global cognition and episodic memory performance. We showed that individual measures of DMN connectivity could be considered a promising method to differentiate AD, even at an early phase, from normal aging. Further studies with larger numbers of participants, as well as validation of normal values, are needed for more definitive conclusions.