Analysis of Insect Cuticular Compounds by Non-lethal Solid Phase Micro Extraction with Styrene-Divinylbenzene Copolymers

Insect cuticular hydrocarbons including relatively non-volatile chemicals play important roles in cuticle protection and chemical communication. The conventional procedures for extracting cuticular compounds from insects require toxic solvents, or non-destructive techniques that do not allow storage of subsequent samples, such as the use of SPME fibers. In this study, we describe and tested a non-lethal process for extracting cuticular hydrocarbons with styrene-divinylbenzene copolymers, and illustrate the method with two species of bees and one species of beetle. The results demonstrate that these compounds can be efficiently trapped by ChromosorbA (R) (SUPELCO) and that this method can be used as an alternative to existing methods.

Surface treatment of dental porcelain with CO2 laser: porosity analysis and AFM.

The effect of CO2 continuous laser irradiation on the surface properties of veneering porcelains has already been tested. The surface observed after laser irradiation is similar to that achieved by auto-glaze in terms of roughness and color parameters (Sgura R, et al. Dental Materials 2011;27(Suppl. 1):e72–73). The purpose of this study was to analyze the surface porosity of porcelain discs after CO2 laser treatment and compare it to auto-glaze treatment, in furnace. A morphological analysis of the porcelain surface was conducted using atomic force microscopy (AFM) and conventional optical microscopy (OM).

Supercritical CO2 extraction of phenolic compounds from Baccharis dracunculifolia

Extracts from Baccharis dracunculifolia leaves were obtained using the following solvents: supercritical carbon dioxide (SC-CO2), ethanol and methanol. Supercritical extraction was carried out at temperatures of 40, 50 and 60 degrees C and pressures of 20, 30 and 40 MPa. Four phenolic compounds were analysed in the extracts by high-performance liquid chromatography: 3,5-diprenyl-4-hydroxycinnamic acid (DHCA or artepillin C); 3-prenyl-4-hydroxycinnamic acid (PHCA); 4-hydroxycinnamic acid (p-coumaric acid) and 4-methoxy-3,5,7-trihydroxyflavone (kaempferide). The global extraction yields (X-0) obtained by the conventional methods with ethanol and methanol were higher than those obtained by SC-CO2. However on analysing the components of interest extracted at 60 degrees C and 40 MPa, the extraction yields of kaempferide, DHCA and PHCA were 156%, 98% and 64% higher, respectively, than in the ethanolic extracts. Only the p-coumaric acid extraction yield was better when extracted using the conventional method. (C) 2008 Elsevier B.V. All rights reserved.

Fluoride plus CO2 laser against the progression of caries in root dentin

Purpose: To evaluate the effect of a 1.23% acidulated phosphate fluoride (APF) gel combined with CO2 laser in protecting carious root dentin against further cariogenic challenges. Methods: After a 7-day lead-in period, 12 volunteers wore an intraoral palatal device containing four carious root dentin slabs, treated with APF and APF+CO2 or placebo and placebo+CO2. After a 14-day wash-out period, volunteers were crossed-over to the other treatment arm. During both intraoral phases, specimens were submitted to cariogenic challenges and then evaluated for cross-sectional Knoop microhardness. Results: Two-way ANOVA demonstrated that there was significant effect for both main factors: CO2 laser irradiation (P< 0.0001) and gel treatment (P< 0.0001), and that there was no interaction between them (P= 0.4706). Protection of carious root dentin against further cariogenic challenges may be provided by APF fluoride gel and CO2 laser, but no additive benefit was found by combining such strategies. (Am J Dent 2012;25:114-117).

In Situ Effect of Dentifrices Associated to CO2 Laser in the Permeability of Eroded Root Dentin

Objective: The aim of this study was to evaluate, through a crossover 2 x 2 in situ trial, the effect of a desensitizing dentifrice associated with CO2 laser irradiation to control the permeability of eroded root dentin. Background data: Facing the increased prevalence of erosive lesion and the need for preventive means to control painful symptoms related to them. Methods: Eighty slabs of bovine root dentin were subjected to initial erosive challenge (citric acid 0.3%, 2 h), followed by a remineralizing period in artificial saliva (24 h). Specimens were then divided according to dentin treatment: desensitizing dentifrice, desensitizing dentifrice + CO2 laser, fluoride anticavity dentifrice. and fluoride anticavity dentifrice + CO2 laser. After a 2-day lead-in period, 10 volunteers wore an intraoral palatal appliance containing four root dentin slabs, in two phases of 5 days each. During the intraoral phase, one side of the appliance was immersed in 0.3% citric acid, and the opposite side was immersed in deionized water, four times a day. One hour after the immersions, all specimens were brushed with dentifrice slurry provided by the researcher. After a 7-day washout period, volunteers were crossed over on the different dentifrice group. Each phase having been completed, the specimens were evaluated for permeability through an optical microscope. Results: Data were analyzed using ANOVA and no significant difference (p = 0.272) was found between the surface treatments performed on bovine root dentin. Conclusions: It can be concluded that fluoride anticavity or desensitizing dentifrice, regardless of the association with the CO2 laser irradiation, was able to control the permeability of eroded root dentin.

Thermal decomposition kinetics of Brazilian limestones: effect of CO2 partial pressure

The influence of the partial pressure of carbon dioxide (CO2) on the thermal decomposition process of a calcite (CI) and a dolomite (DP) is investigated in this paper using a thermogravimetric analyser. The tests were non-isothermal at five different heating rates in dynamic atmosphere of air with 0% and 15% carbon dioxide (CO2). In the atmosphere without CO2, the average activation energies (E-alpha) were 197.4 kJ mol(-1) and 188.1 kJ mol(-1) for CI and DP, respectively. For the DP with 15% CO2, two decomposition steps were observed, indicating a change of mechanism. The values of E-alpha for 15% CO2 were 378.7 kJ mol(-1) for the CI, and 299.8 kJ mol(-1) (first decomposition) and 453.4 kJ mol(-1) (second decomposition) for the DP, showing that the determination of E-alpha for DP should in this case be considered separately in those two distinct regions. The results obtained in this study are relevant to understanding the behaviour changes in the thermal decomposition of limestones with CO2 partial pressure when applied to technologies, such as carbon capture and storage (CCS), in which carbon dioxide is present in high concentrations.

Analysis of carvedilol enantiomers in human plasma using chiral stationary phase column and liquid chromatography with tandem mass spectrometry

Carvedilol is an antihypertensive drug available as a racemic mixture. (-)-(S)-carvedilol is responsible for the nonselective beta-blocker activity but both enantiomers present similar activity on a1-adrenergic receptor. To our knowledge, this is the first study of carvedilol enantiomers in human plasma using a chiral stationary phase column and liquid chromatography with tandem mass spectrometry. The method involves plasma extraction with diisopropyl ether using metoprolol as internal standard and direct separation of the carvedilol enantiomers on a Chirobiotic T (R) (Teicoplanin) column. Protonated ions [M + H]+ and their respective ion products were monitored at transitions of 407 > 100 for the carvedilol enantiomers and 268 > 116 for the internal standard. The quantification limit was 0.2 ng ml-1 for both enantiomers in plasma. The method was applied to study enantioselectivity in the pharmacokinetics of carvedilol administered as a single dose of 25 mg to a hypertensive patient. The results showed a higher plasma concentration of (+)-(R)-carvedilol (AUC08 205.52 vs. 82.61 (ng h) ml-1), with an enantiomer ratio of 2.48. Chirality, 2012. (C) 2012 Wiley Periodicals, Inc.

FTIR and SEM analysis of CO2 laser irradiated human enamel

Objectives: Considering the enamel chemical structure, especially carbonate band, which has a major role in the caries prevention, the objective of the present study was to assess the chemical alterations on the enamel irradiated with CO2 laser by means of FTIR spectroscopy and SEM analysis. Design: The enamel surfaces were analysed on a spectrometer for acquisition of the absorption spectrum relative to the chemical composition of the control sample. The irradiation was conducted with a 10.6-mu m CO2 laser (0.55 W, 660 W/cm(2)). The carbonate absorption band at 1600-1291 cm(-1) as well as the water absorption band at 3793-2652 cm(-1) was measured in each sample after the irradiation. The water band was measured again 24-h after the irradiation. The band area of each chemical compound was delimited, the background was subtracted, and the area under each band was integrated. Each area was normalized by the phosphate band (1190-702 cm(-1)). Results: There was a statistically significant decrease (p < 0.05) in the water content after irradiation (control: 0.184 +/- 0.04; irradiated: 0.078 +/- 0.026), which increased again after rehydration (0.145 +/- 0.038). The carbonate/phosphate ratio was measured initially (0.112 +/- 0.029) and its reduction after irradiation indicated the carbonate loss (0.088 +/- 0.014) (p < 0.05). Conclusion: The 10.6-mu m CO2 laser irradiation diminishes the carbonate and water contents in the enamel after irradiation. (C) 2012 Elsevier Ltd. All rights reserved.

Comparison of extraction and transesterification methods on the determination of the fatty acid contents of three Brazilian seaweed species

Seaweeds are photosynthetic organisms important to their ecosystem and constitute a source of compounds with several different applications in the pharmaceutical, cosmetic and biotechnology industries, such as triacylglycerols, which can be converted to fatty acid methyl esters that make up biodiesel, an alternative source of fuel applied in economic important areas. This study evaluates the fatty acid profiles and concentrations of three Brazilian seaweed species, Hypnea musciformis (Wulfen) J.V. Lamouroux (Rhodophya), Sargassum cymosum C. Agardh (Heterokontophyta), and Ulva lactuca L. (Chlorophyta), comparing three extraction methods (Bligh & Dyer - B&D; AOAC Official Methods - AOM; and extraction with methanol and ultrasound - EMU) and two transesterification methods (7% BF3 in methanol - BF3; and 5% HCl in methanol - HCl). The fatty acid contents of the three species of seaweeds were significantly different when extracted and transesterified by the different methods. Moreover, the best method for one species was not the same for the other species. The best extraction and transesterification methods for H. musciformis, S. cymosum and U. lactuca were, respectively, AOM-HCl, B&D-BF3 and B&D-BF3/B&D-HCl. These results point to a matrix effect and the method used for the analysis of the fatty acid content of different organisms should be selected carefully.

Enantioselective analysis of unbound tramadol, O-desmethyltramadol and N-desmethyltramadol in plasma by ultrafiltration and LC-MS/MS: Application to clinical pharmacokinetics

This study describes the enantioselective analysis of unbound and total concentrations of tramadol and its main metabolites O-desmethyltramadol (M1) and N-desmethyltramadol (M2) in human plasma. Sample preparation was preceded by an ultrafiltration step to separate the unbound drug. Both the ultrafiltrate and plasma samples were submitted to liquid/liquid extraction with methyl t-butyl ether. Separation was performed on a Chiralpak (R) AD column and tandem mass spectrometry consisting of an electrospray ionization source, positive ion mode and multiple reaction monitoring was used as the detection system. Linearity was observed in the following ranges: 0.2-600 and 0.5-250 ng/mL for analysis of total and unbound concentrations of the tramadol enantiomers, respectively, and 0.1-300 and 0.25-125 ng/mL for total and unbound concentrations of the M1 and M2 enantiomers, respectively. The lower limits of quantitation were 0.2 and 0.5 ng/mL for analysis of total and unbound concentration of each tramadol enantiomer, respectively, and 0.1 and 0.25 ng/mL for total and unbound concentrations of M1 and M2 enantiomers, respectively. Intra- and interassay reproducibility and inaccuracy did not exceed 15%. Clinical application of the method to patients with neuropathic pain showed plasma accumulation of (+)-tramadol and (+)-M2 after a single oral dose of racemic tramadol. Fractions unbound of tramadol, M1 or M2 were not enantioselective in the patients investigated. (C) 2011 Elsevier B.V. All rights reserved.

Coupling Between GABA(A)-R Ligand-Binding Activity and Membrane Organization in beta-Cyclodextrin-Treated Synaptosomal Membranes from Bovine Brain Cortex: New Insights from EPR Experiments

Correlations between GABA(A) receptor (GABA(A)-R) activity and molecular organization of synaptosomal membranes (SM) were studied along the protocol for cholesterol (Cho) extraction with beta-cyclodextrin (beta-CD). The mere pre-incubation (PI) at 37A degrees C accompanying the beta-CD treatment was an underlying source of perturbations increasing [H-3]-FNZ maximal binding (70%) and K (d) (38%), plus a stiffening of SMs' hydrocarbon core region. The latter was inferred from an increased compressibility modulus (K) of SM-derived Langmuir films, a blue-shifted DPH fluorescence emission spectrum and the hysteresis in DPH fluorescence anisotropy (A (DPH)) in SMs submitted to a heating-cooling cycle (4-37-4A degrees C) with A (DPH,heating) < A (DPH,cooling). Compared with PI samples, the beta-CD treatment reduced B (max) by 5% which correlated with a 45%-decrement in the relative Cho content of SM, a decrease in K and in the order parameter in the EPR spectrum of a lipid spin probe labeled at C5 (5-SASL), and significantly increased A (TMA-DPH). PI, but not beta-CD treatment, could affect the binding affinity. EPR spectra of 5-SASL complexes with beta-CD-, SM-partitioned, and free in solution showed that, contrary to what is usually assumed, beta-CD is not completely eliminated from the system through centrifugation washings. It was concluded that beta-CD treatment involves effects of at least three different types of events affecting membrane organization: (a) effect of PI on membrane annealing, (b) effect of residual beta-CD on SM organization, and (c) Cho depletion. Consequently, molecular stiffness increases within the membrane core and decreases near the polar head groups, leading to a net increase in GABA(A)-R density, relative to untreated samples.

Método Mehlich 3 como substituinte ao HCl para extração de Cobre e Zinco em solos com alto teor de matéria orgânica do sul do Brasil

No presente trabalho, foram comparados dois métodos de extração de cobre (Cu) e zinco (Zn) em solos com teor de matéria orgânica (MO) maior que 50g kg-1. Os métodos de extração comparados foram: Extração com HCl 0,1mol L-1 (método padrão para os estados do Rio Grande do Sul e Santa Catarina) e Mehlich 3. Este trabalho foi realizado no Laboratório de Química e Fertilidade do Solo da Universidade do Estado de Santa Catarina (UDESC), no ano de 2009. As duas metodologias de extração foram aplicadas em 286 amostras de solo provenientes do Laboratório de Análise do Solo da UDESC, todas com mais de 50g kg-1 de MO. Os teores de cobre e zinco nos extratos foram determinados por espectrometria de absorção atômica com chama. Os resultados mostraram que houve correlação significativa entre os métodos, Cu (r=0,80) e Zn (r=0,93). A solução de Mehlich 3 extraiu mais cobre e menos zinco, quando comparada à solução de HCl 0,1mol L-1. O Mehlich 3 demonstrou ser eficiente na extração de cobre e zinco em solos com alto teor de MO, podendo substituir o método atual.

Proinflammatory and Antiinflammatory Cytokine Levels in Complicated and Noncomplicated Parapneumonic Pleural Effusions

Objectives: This study aimed to evaluate a panel of proinflammatory and antiinflammatory cytokines in noncomplicated and complicated parapneumonic pleural effusions and to correlate their levels with pleural fluid biochemical parameters. Methods: Serum and pleural effusion were collected from 60 patients with noncomplicated (n = 26) or complicated (n = 34) parapneumonic effusions and assayed for cytologic, biochemical, and proinflammatory and antiinflammatory cytokines. Student t test was used to compare serum and pleural fluid values, Spearman correlation to analyze the relationship between pleural fluid cytokines and biochemical parameters, and accuracy of pleural fluid cytokine levels to determine the optimal cutoff value for identification of complicated effusions. Corrections for multiple comparisons were applied and a P value < .05 was accepted as significant. Results: Serum and pleural fluid cytokine levels of IL-8, vascular endothelial growth factor (VEGF), IL-10, and tumor necrosis factor (TNF) soluble receptor (sR) II were similar between groups. In contrast, complicated effusions had higher levels of pleural fluid IL-1 beta, IL-1 receptor antagonist (ra), and TNF sRI. Negative correlations were found between pleural fluid glucose with IL-1 beta and TNF sRI and positive correlations between lactic dehydrogenate (LDH) with IL-1 beta, IL-8, and VEGF. Pleural fluid levels of IL-1 beta, IL-1ra, and TNF sRI were more accurate than IL-8, VEGF, IL-10, and TNF sRII in discriminating complicated effusions. Conclusions: Both proinflammatory and antiinflammatory cytokine levels in pleural fluid are elevated in complicated in comparison with noncomplicated parapneumonic pleural effusions, and they correlate with both pleural fluid glucose and LDH levels. IL-1 beta, IL-1ra, and TNF sRI had higher sensitivity and specificity than IL-8, VEGF, IL-10, and TNF sRII in discriminating complicated effusions. CHEST 2012; 141( 1):183-189

Cooking Effects on Iron and Proteins Content of Beans (Phaseolus Vulgaris L.) by GF AAS and MALDI-TOF MS

The effects of domestic cooking on proteins, organic compounds and Fe distribution in beans (Phaseolus vulgaris L.) were investigated. Sequential extraction with different extractant solutions (mixture of methanol and chloroform 1:2 v/v, water, 0.5 mol L-1 NaCl, 70% v/v ethanol and 0.5 mol L-1 NaOH) were used for extracting lipids, albumins, globulins, prolamins and glutelins, respectively. Iron determination by graphite furnace atomic absorption spectrometry (GF AAS), proteins by Bradford method and organic compounds by matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS) were carried out in this work. High concentration of albumins, globulins and glutelins were found in raw beans, while in the cooked beans, albumins and glutelins are main proteins types. The MALDI-TOF MS spectra of raw and cooked beans revealed that the domestic cooking altered the molecular weight of the organic compounds, since that in the cooked beans were found compounds between 2 and 3.5 kDa, which were not presented in the raw beans. Besides this, in cooked beans were also observed the presence of four compounds of high molecular weight (12-16 kDa), being that in the raw grains there is only one (ca. 15.2 kDa). In raw grains is possible to observe that Fe is mainly associated to albumins, globulins and glutelins. For cooked grains, Fe is associated to albumins and globulins.

Mimosine and Cyclophosphamide: a Potential New Combination Therapy Used to Prevent Tumor Development

The effects of mimosine (MI), which is an amino acid that is derived from Leucaena leucocephala, were evaluated on the growth of ascitic Ehrlich tumors, and the effects of the combination treatment of MI and cyclophosphamide (CY) on tumor growth were also assessed. Mice were divided into groups that received the following treatments over the course of 20 days: phosphate buffer solution (CO), MI, Ehrlich cells (E), E plus CY (EC), E plus MI (EM) and E plus MI and CY (EMC). No signs of toxicity were detected in the mice from the MI group. The mice from the EMC group showed reductions in body weights when compared with those from the E group. The animals from the EC, EM and EMC groups showed reductions in ascitic volume compared with those from the E group. The mice from the EMC group showed reductions in total cell numbers of ascitic fluid compared with those from the E, EC and EM groups. The combination of MI and CY was the most effective treatment for Ehrlich tumor ascites.