Determination of anticonvulsants in human plasma using SPME in a heated interface coupled online to liquid chromatography (SPME-LC)

A simple and sensitive method using solid phase microextraction (SPME) and liquid chromatography (LC) with heated online desorption (SPME-LC) was developed and validated to analyze anticonvulsants (AEDs) in human plasma samples. A heated lab-made interface chamber was used in the desorption procedure, which allowed the transference of the whole extracted sample. The SPME conditions were optimized by applying an experimental design. Important factors are discussed such as fiber coating types, pH, extraction time and desorption conditions. The drugs were analyzed by LC, using a C18 column (150 mm 4.6 mm 5 mm); and 50 mmol L1 , pH ¼ 5.50 ammonium acetate buffer : acetonitrile : methanol (55 : 22 : 23 v/v) as the mobile phase with a flow rate of 0.8 mL min1 . The suggested method presented precision (intra-assay and inter-assay), linearity and limit of quantification (LOQ) all adequate for the therapeutic drug monitoring (TDM) of AEDs in plasma.

Analysis of Steroids using Solid Phase Microextraction-Gas Chromatography-Mass Spectrometry-Mass Spectrometry (SPME-GC-MS-MS)

Direct immersion SPME-GC-MS-MS was used for the analysis of steroids in water at part-per-trillion(ppt) and lower concentrations. The method was validated and extended to real sample analysis. The method were linear from 0.01 to 5 ng/ml with precision less than 10% relative standard deviation for a steroid mixture at 1 ng/ml. Limit of quantitation and limit of detection was found to be 200- 1200 pg/L and 30-200 pg/L respectively and recoveries ranged from 88-103 %. To understand the extraction efficiency of the fiber, a depletion study was performed. The fiber/ sample partition coefficients for the steroids were determined to be 1.0 x 104 to 1.5 x 104 . The extraction was performed without derivatization or the use of an internal standard. SPMEGC-MS-MS effectively demonstrated ultra-trace level detection of steroids in water.

Bacterial cellulose-hydroxyapatite composites with osteogenic growth peptide (OGP) or pentapeptide OGP on bone regeneration in critical-size calvarial defect model

This study aimed to evaluate the potential of bacterial cellulose-hydroxyapatite (BC-HA) composites associated with osteogenic growth peptide (OGP) or pentapeptide OGP(10–14) in bone regeneration in critical-size calvarial defects in mice. In this study, the BC-HA, BC-HA-OGP, and BC-HA-OGP(10–14) membranes were analyzed at 3, 7, 15, 30, 60, and 90 days. In each period, the specimens were evaluated by micro-computed tomography (µCT), descriptive histology, gene expression of bone biomarkers by qPCR and VEGFR-2 (vascular endothelial growth factor) quantification by ELISA. Three days post-operative, Runx2, Tnfrsf11b and Bglap bone biomarkers were upregulated mainly by BC-HA OGP and BC-HA OGP(10–14) membranes, suggesting an acceleration of the osteoblast differentiation/activity with the use of these biomaterials. At 60 and 90 days, a high percentage of bone formation was observed by µCT for BC-HA and BC-HA OGP(10–14) membranes. High expression of some bone biomarkers, such as Alpl, Spp1, and Tnfrsf11b, was also observed for the same membranes on days 60 and 90. In conclusion, the BC-HA membrane promoted a better bone formation in critical-size mice calvarial defects. Nevertheless, incorporation of the peptides at the concentration of 10−9 mol L−1 did not improve bone regeneration potential in the long-term.

Determination of uronic acids in sugarcane bagasse by anion-exchange chromatography using an electrode modified with copper nanoparticles

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

Determination of estrogenic mycotoxins in environmental water samples by low-toxicity dispersive liquid-liquid microextraction and liquid chromatography-tandem mass spectrometry

A novel, simple, rapid and eco-friendly method based on dispersive liquid-liquid microextraction using a bromosolvent was developed to determine six estrogenic mycotoxins (zearalenone, zearalanone, alpha-zearalanol, beta-zearalanol, alpha-zearalenol and beta-zearalenol) in water samples by liquid chromatography-electrospray ionization tandem mass spectrometry in the negative mode (LC-ESI-MS/MS). The optimal conditions for this method include the use of 100 mu L bromocyclohexane as an extraction solvent (using a non-dispersion solvent), 10 mL of aqueous sample (adjusted to pH 4), a vortex extraction time of 2 min, centrifugation for 10 min at 3500 rpm and no ionic strength adjustment. The calibration function was linear and was verified by applying the Mandel fitting test with a 95% confidence level. No matrix effect was observed. According to the relative standard deviations (RSDs), the precision was better than 13% for the repeatability and intermediate precision. The average recoveries of the spiked compounds ranged from 81 to 118%. The method limits of detection (LOD) and quantification (LOQ) considering a 125-fold pre-concentration step were 4-20 and 8-40 ng L-1, respectively. Next, the method was applied to the analysis of the environmental aqueous samples, demonstrating the presence of beta-zearalanol and zearalanone in the river water samples. (C) 2015 Elsevier B.V. All rights reserved.

Development of a comprehensive method for analyzing clerodane-type diterpenes and phenolic compounds from Casearia sylvestris Swartz (Salicaceae) based on ultra high performance liquid chromatography combined with chemometric tools

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

Hydroxyapatite and a new fibrin sealant derived from snake venom as scaffold to treatment of cranial defects in rats

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

Rapid and sensitive ultra-high-pressure liquid chromatography method for quantification of antichagasic benznidazole in plasma: application in a preclinical pharmacokinetic study

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

The effect of polymerization mode on monomer conversion, free radical entrapment, and interaction with hydroxyapatite of commercial self-adhesive cements

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Hydroxyapatite coating deposited on grade 4 titanium by plasma electrolytic oxidation

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

Structural characterization of novel chemotactic and mastoparan peptides from the venom of the social wasp Agelaia pallipes pallipes by high-performance liquid chromatography/electrospray ionization tandem mass spectrometry

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Determination of water insoluble dyes used as marking of commercial petroleum products using high-performance liquid chromatography with electrochemical detection

This paper describes an analytical method using high-performance liquid chromatographic (HPLC) separationcoupled with electrochemical detection to detect three dyes, Solvent Blue 14 (SB-14), Solvent Blue 35 (SB-35) andSolvent Red 24 (SR-24). The dyes were eluted and separated using a reversed-phase column (C-8) under isocraticelution with the mobile phase containing a mixture of acetonitrile/ammonium acetate (5.0 mmol L1) at the ratio of75: 25 (v/v). Two sample pretreatment methods were tested and successfully applied to quantify SB14, SB-35 and SR-24 dyes in gasoline samples. The proposed method was simple, fast and suitable to detect and quantify marker dyes ingasoline sample at low concentration.

A simple high-performance liquid chromatography assay for on-line determination of catecholamines in adrenal gland by direct injection on an ISRP column

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

Effect of trimetaphosphate and fluoride association on hydroxyapatite dissolution and precipitation in vitro

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