In2O3 microcrystals obtained from rapid calcination in domestic microwave oven

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Rapid, quantitative determination of polar compounds in fats and oils by solid-phase extraction and size-exclusion chromatography using monostearin as internal standard

A rapid and simple method was developed for quantitation of polar compounds in fats and oils using monostearin as internal standard. Starting from 50 mg of oil sample, polar compounds were obtained by solid-phase extraction (silica cartridges) and subsequently separated by high-performance size-exclusion chromatography into triglyceride polymers, triglyceride dimers, oxidized triglyceride monomers, diglycerides, internal standard and fatty acids. Quantitation of total polar compounds was achieved through the internal standard method and then amounts of each group of compounds could be calculated. A pool of polar compounds was used to check linearity, precision and accuracy of the method, as well as the solid-phase extraction recovery. The procedure was applied to samples with different content of polar compounds and good quantitative results were obtained, especially for samples of low alteration level.

Structural and electrical properties of strontium barium niobate thin films crystallized by conventional furnace and rapid-thermal annealing process

Strontium barium niobate (SBN) thin films were crystallized by conventional electric furnace annealing and by rapid-thermal annealing (RTA) at different temperatures. The average grain size of films was 70 nm and thickness around 500 nm. Using x-ray diffraction, we identified the presence of polycrystalline SBN phase for films annealed from 500 to 700 °C in both cases. Phases such as SrNb2O6 and BaNb2O6 were predominantly crystallized in films annealed at 500 °C, disappearing at higher temperatures. Dielectric and ferroelectric parameters obtained from films crystallized by conventional furnace and RTA presented essentially the same values.

A simple and rapid extraction for gas chromatographic determination of thiabendazole and imazalil residues in lemons

A rapid and efficient method is described for the determination of thiabendazole and imazalil residues in lemons (peel and pulp). The procedure is based on the extraction with an hexane:ethyl acetate mixture (1:1, v/v) and gas chromatographic analysis using thermionic specific detection (TSD). The possibility of matrix effect was also studied. Mean recoveries from 8 replicates of fortified samples ranged from 79% to 109%, with relative standard deviation values between 2.4% to 12.8%. The detection and quantification limits of the method were 0.2 mg kg-1 and 0.5 mg kg-1, respectively.

A simplified spectrophotometric method for routine analysis of saccharin in commercial noncaloric sweeteners

A simple, rapid, and sensitive spectrophotometric method for routine analysis of saccharin in commercial noncaloric sweeteners is proposed. This method is based on the reaction of saccharin with tetrachloro-p-benzoquinone (p-chloranil) accelerated by hydrogen peroxide and conducted in an ethanol:acetone (4:1) medium, producing a violet-red compound (γ max = 550 nm). Beer's law is obeyed in a concentration range of 2.05 × 10 -4 to 3.00 × 10 -3 M with an excellent correlation coefficient (r = 0.9998). The detection limit was 1.55 × 10 -5 M, and the effect of interferences on the spectrophotometric measurements was evaluated. The proposed procedure was applied successfully to the determination of saccharin in noncaloric sweeteners. Recoveries were within 99.2-104.3% with standard deviations ranging from to 0.5-1.6%. Results of the proposed method compare very favorably with those given by the high-performance liquid chromatography method recommended by the Food and Drug Administration.

Periodontal effects of rapid maxillary expansion with tooth-tissue-borne and tooth-borne expanders: A computed tomography evaluation

Introduction: The force delivered during rapid maxillary expansion (RME) produces areas of compression on the periodontal ligament of the supporting teeth. The resulting alveolar bone resorption can lead to unwanted tooth movement in the same direction. The purpose of this study was to evaluate periodontal changes by means of computed tomography after RME with tooth-tissue-borne and tooth-borne expanders. Methods: The sample comprised 8 girls, 11 to 14 years old, with Class I or II malocclusions with unilateral or bilateral posterior crossbites Four girls were treated with tooth-tissue-borne Haas-type expanders, and 4 were treated with tooth-borne Hyrax expanders. The appliances were activated up to the full 7-mm capacity of the expansion screw. Spiral CT scans were taken before expansion and after the 3-month retention period when the expander was removed. One-millimeter thick axial sections were exposed parallel to the palatal plane, comprising the dentoalveolar area and the base of the maxilla up to the inferior third of the nasal cavity. Multiplanar reconstruction was used to measure buccal and lingual bone plate thickness and buccal alveolar bone crest level by means of the computerized method. Results and Conclusions: RME reduced the buccal bone plate thickness of supporting teeth 0.6 to 0.9 mm and increased the lingual bone plate thickness 0.8 to 1.3 mm. The increase in lingual bone plate thickness of the maxillary posterior teeth was greater in the tooth-borne expansion group than in the tooth-tissue-borne group. RME induced bone dehiscences on the anchorage teeth's buccal aspect (7.1 ± 4.6 mm at the first premolars and 3.8 ± 4.4 mm at the mesiobuccal area of the first molars), especially in subjects with thinner buccal bone plates. The tooth-borne expander produced greater reduction of first premolar buccal alveolar bone crest level than did the tooth-tissue-borne expander. © 2006 American Association of Orthodontists.

Development and validation of HPLC method for quantitative analysis of triamcinolone in biodegradable microparticles

A simple, rapid, selective and specific high performance liquid chromatographic (HPLC) method for quantitative analysis of the triamcinolone in polylactide-co-glycolide acid (PLGA) microparticles was developed. The chromatographic parameters were reversed-phase C18 column, 250mm x 4.6mm, with particle size 5 μm. The column oven was thermostated at 35°C ± 2°C. The mobile phase was methanol/water 45:55 (v/v) and elution was isocratic at a flow-rate of 1 mL.mL-1. The determinations were performed using a UV-Vis detector at 239 nm. The injected sample volume was 10 μL. The standard curve was linear (r2 > 0.999) in the concentration range 100-2500 ng.mL-1. The method showed adequate precision, with a relative standard deviation (RSD) was smaller than 3%. The accuracy was analyzed by adding a standard drug and good recovery values were obtained for all drug concentrations used. The method showed specificity and selectivity with linearity in the working range and good precision and accuracy, making it very suitable for quantitation of triamcinolone in PLGA microparticles.

Analysis of polymerization time on abrasive wear of dental resins

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Integrated analysis of halogenated organic pollutants in sub-millilitre volumes of venous and umbilical cord blood sera

A rapid, robust and economical method for the analysis of persistent halogenated organic compounds in small volumes of human serum and umbilical cord blood is described. The pollutants studied cover a broad range of molecules of contemporary epidemiological and legislative concern, including polychlorobiphenyls (PCBs), polychlorobenzenes (CBs), hexachlorocyclohexanes (HCHs), DDTs, polychlorostyrenes (PCSs) and polybromodiphenyl ethers (PBDEs). Extraction and clean-up with n-hexane and concentrated sulphuric acid was followed with analysis by gas chromatography coupled to electron capture (GC-ECD) and GC coupled to negative ion chemical ionisation mass spectrometry (GC-NICI-MS). The advantages of this method rest in the broad range of analytes and its simplicity and robustness, while the use of concentrated sulphuric acid extraction/clean-up destroys viruses that may be present in the samples. Small volumes of reference serum between 50 and 1000 μL were extracted and the limits of detection/quantification and repeatability were determined. Recoveries of spiked compounds for the extraction of small volumes (≥300 μL) of the spiked reference serum were between 90% and 120%. The coefficients of variation of repeatability ranged from 0.1-14%, depending on the compound. Samples of 4-year-old serum and umbilical cord blood (n = 73 and 40, respectively) from a population inhabiting a village near a chloro-alkali plant were screened for the above-mentioned halogenated pollutants using this method and the results are briefly described. © 2010 Springer-Verlag.

Recent applications of analytical techniques for quantitative pharmaceutical analysis: A review

The intension of this paper was to review and discuss some of the current quantitative analytical procedures which are used for quality control of pharmaceutical products. The selected papers were organized according to the analytical technique employed. Several techniques like ultraviolet/visible spectrophotometry, fluorimetry, titrimetry, electroanalytical techniques, chromatographic methods (thin-layer chromatography, gas chromatography and high-performance liquid chromatography), capillary electrophoresis and vibrational spectroscopies are the main techniques that have been used for the quantitative analysis of pharmaceutical compounds. In conclusion, although simple techniques such as UV/VIS spectrophotometry and TLC are still extensively employed, HPLC is the most popular instrumental technique used for the analysis of pharmaceuticals. Besides, a review of recent works in the area of pharmaceutical analysis showed a trend in the application of techniques increasingly rapid such as ultra performance liquid chromatography and the use of sensitive and specific detectors as mass spectrometers.

Comparative study of the healing process when using Vicryl®, Vicryl Rapid®, Vicryl Plus®, and Monocryl® sutures in the rat dermal tissue

Introduction: Various types of sutures are available in the market with different constitutions. However, there is a lack of research to assess and quantify the behavior of these materials. Resources and materials: This study comes benchmark wires polyglactin 910 (Vicryl ®), irradiated polyglactin 910 (Vicryl Rapid ®), polyglactin 910 treated with triclosan (Vicryl Plus ®), and poliglecaprone 25 (Monocryl ®). For this, we used 40 rats that were divided into two groups, underwent two skin incisions longitudinal 2-cm long. In Group A, simple interrupted sutures using irradiated polyglactin 910 on the right and left side of polyglactin 910, and in group B, polyglactin 910 with triclosan on the right and the left poliglecaprone 25 were made. At 2, 7, 14, and 28 days after surgery, the ten animals were killed per period, and the samples were processed for histomorphologic and histometric analysis. Conclusions: The results demonstrated that the wire poliglecaprone 25 showed better biological response, with less inflammatory infiltrates and rapid organization of connective tissue. © 2012 Springer-Verlag Berlin Heidelberg.

Fatigue and rapid hamstring/quadriceps force capacity in professional soccer players

The aim of this study was to investigate the effect of fatigue induced by an exhaustive laboratory-based soccer-specific exercise on different hamstrings/quadriceps (H:Q) ratios of soccer players. Twenty-two male professional soccer players (23·1 ± 3·4 year) performed maximal eccentric (ecc) and concentric (con) contractions for knee extensors (KE) and flexors (KF) at 60° s-1 and 180° s-1 to assess conventional (Hcon:Qcon) and functional (Hecc:Qcon) ratios. Additionally, they performed maximal voluntary isometric contraction for KE and KF, from which the maximal muscle strength, rate of force development (RFD) and RFD H:Q strength ratio (RFDH:Q) were extracted. Thereafter, subjects were performed an exhaustive laboratory-based soccer-specific exercise and a posttest similar to the pretest. There was significant reduction in Hcon:Qcon (0·60 ± 0·06 versus 0·58 ± 0·06, P<0·05) and in Hecc:Qcon (1·29 ± 0·2 versus 1·16 ± 0·2, P<0·01) after the soccer-specific exercise. However, no significant difference between Pre and Post exercise conditions was found for RFDH:Q at 0-50 (0·53 ± 0·23 versus 0·57 ± 0·24, P>0·05) and 0-100 ms (0·53 ± 0·17 versus 0·55 ± 0·17, P>0·05). In conclusion, H:Q strength ratios based on peak force values are more affected by fatigue than RFDH:Q obtained during early contraction phase. Thus, fatigue induced by soccer-specific intermittent protocol seems not reduce the potential for knee joint stabilization during the initial phase of voluntary muscle contraction. copy; 2012 Scandinavian Society of Clinical Physiology and Nuclear Medicine.

A simple, rapid method for the extraction of whole fire ant venom (Insecta: Formicidae: Solenopsis)

The invasive fire ant Solenopsis invicta is medically important because its venom is highly potent. However, almost nothing is known about fire ant venom proteins because obtaining even milligram-amounts of these proteins has been prohibitively challenging. We present a simple and fast method of obtaining whole venom compounds from large quantities of fire ants. For this, we separate the ants are from the nest soil, immerse them in dual-phase mixture of apolar organic solvent and water, and evaporate each solvent phase in separate. The remaining extract from the aqueous phase is largely made up of ant venom proteins. We confirmed this by using 2D gel electrophoresis while also demonstrating that our new approach yields the same proteins obtained by other authors using less efficient traditional methods. © 2013 Elsevier Ltd.

Rapid determination of furosemide by combined spot test/diffuse reflectance spectroscopy to detect doping in sport

This paper describes the development and application of a simple, cheap, and clean method for the quantification of furosemide in urine samples from athletes, to detect doping, using a combined spot test/diffuse reflectance spectroscopy procedure. The method is based on the complexation reaction of furosemide (5-(aminosulfonyl)-4-chloro-2-((furanylmethyl)amino)benzoic acid, dissolved in ethanol, with FeCl3 and the surfactant dodecyltrimethylammonium bromide (DTAB) in aqueous solution, yielding a colored compound on the surface of a filter paper. The reagent concentrations were optimized using a chemometric experimental design. The reflectometric measurements of the complex formed were carried out at 477nm. The linear range obtained was 1.65-9.00×10-3molL-1 of furosemide (R=0.997), and the detection and quantification limits were 4.9×10-4 and 1.62×10-3molL-1, respectively. The proposed method was successfully applied in the analysis of furosemide in spiked urine, demonstrating that it is a reliable alternative method for the detection of furosemide doping in sport. © 2012 Elsevier B.V..