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.

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.

Sensitive method for determination of piplartine, an alkaloid amide from Piper species, in rat plasma samples by liquid chromatography-tandem mass spectrometry

Piplartine (PPTN) is an alkaloid amide found in Piper species that presents different activities. PPTN determination in rat plasma is necessary to better understand its biological effects. The aim of this study was to develop a sensitive LC-MS/MS method for the determination of PPTN in rat plasma. The performance criteria for linearity, sensitivity, precision, accuracy, recovery, and stability have been assessed and were within the recommended guidelines. The validated method proved to be suitable in a pilot study of PPTN kinetic disposition in rat plasma after a single intraperitoneal dose, and represents an appropriate tool to further pharmacokinetic studies.

Alkaline earth layered benzoates as reusable heterogeneous catalysts for the methyl esterification of benzoic acid

This paper describes the synthesis and characterization of layered barium, calcium and strontium benzoates and evaluates the potential of these materials as catalysts in the synthesis of methyl benzoate. The methyl esterification of benzoic acid was investigated, where the effects of temperature, alcohol:acid molar ratio and amount of catalyst were evaluated. Ester conversions of 65 to 70% were achieved for all the catalysts under the best reaction conditions. The possibility of recycling these metallic benzoates was also demonstrated, evidenced by unaltered catalytic activity for three consecutive reaction cycles.

Multi-component quantitation of loratadine, pseudoephedrine and paracetamol in plasma and pharmaceutical formulations with liquid chromatography-tandem mass spectrometry utilizing a monolithic column

The purpose of this study was to develop a rapid, simple and sensitive quantitation method for pseudoephedrine (PSE), paracetamol (PAR) and loratadine (LOR) in plasma and pharmaceuticals using liquid chromatography-tandem mass spectrometry with a monolithic column. Separation was achieved using a gradient composition of methanol-0.1% formic acid at a flow rate of 1.0 mL min-1. Mass spectral transitions were recorded in SRM mode. System validation was evaluated for precision, specificity and linearity. Limit of detection for pseudoephedrine, paracetamol, and loratadine were determined to be 3.14, 1.86 and 1.44 ng mL-1, respectively, allowing easy determination in plasma with % recovery of 93.12 to 101.56%.

Determination of levodopa in human plasma by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS): application to a bioequivalence study

A sensitive, accurate and simple method using HPLC-MS/MS was developed and validated for levodopa quantitation in human plasma. Analysis was achieved on a pursuit® C18 analytical column (5 µm; 150 x 4.6 mm i.d.) using a mobile phase (methanol and water , 90:10, v/v) containing formic acid 0.5% v/v, after extracting the samples using a simple protein plasma precipitation with perchloric acid. The developed method was validated in accordance with ANVISA guidelines and was successfully applied to a bioequivalence study in 60 healthy volunteers demonstrating the feasibility and reliability of the proposed method.

Use of heterogeneous catalysts in methylic biodiesel production induced by microwave irradiation

The effect of different heterogeneous catalysts on the microwave-assisted transesterification of sunflower oil for the production of methylic biodiesel in a monomode microwave reactor is described. The experiments were carried out at 70 ºC with a 16:1 methanolsunflower oil molar ratio and different heterogeneous basic and acidic catalysts. The results showed that the microwave-heated reactions occur up to four times faster than those carried out with conventional heating. The reactions were performed with 24 catalysts; pure calcium oxide (CaO) and potassium carbonate, either pure or supported by alumina (K2CO3/Al2O3), were the most efficient catalysts.

A NOVEL POLYACRYLAMIDE-BASED HYDROGEL CROSSLINKED WITH CELLULOSE ACETATE AND PREPARED BY PRECIPITATION POLYMERIZATION

The synthesis of polyacrylamide-cellulose acetate hydrogels by precipitation polymerization in acetone solution is reported herein. These hydrogels exhibit smaller swelling ratios and larger compression moduli than homo polyacrylamide hydrogels. For cellulose acetate concentrations above 20 wt.%, hydrogels with N,N'-methylenebisacrylamide as a crosslinker exhibit swelling ratios and compression moduli similar to those of the hydrogels without the crosslinker. A possible explanation for this behavior is that cellulose acetate crosslinks polyacrylamide via free-radical reaction. The hydrogels obtained without the N,N'-methylenebisacrylamide crosslinker exhibit compression moduli up to 1.7 MPa, making them suitable for tissue engineering applications such as cartilage replacement.

Sorption kinetics and intrapaticulate diffusivity of As(III) bioremediation from aqueous solution, using modified and unmodified coconut fiber

The pollution and toxicity problems posed by arsenic in the environment have long been established. Hence, the removal and recovery remedies have been sought, bearing in mind the efficiency, cost effectiveness and environmental friendliness of the methods employed. The sorption kinetics and intraparticulate diffusivity of As (III) bioremediation from aqueous solution using modified and unmodified coconut fiber was investigated. The amount adsorbed increased as time increased, reaching equilibrium at about 60 minutes. The kinetic studies showed that the sorption rates could be described by both pseudo-first order and pseudo-second order process with the later showing a better fit with a value of rate constant of 1.16 x 10-4 min-1 for the three adsorbent types. The mechanism of sorption was found to be particle diffusion controlled. The diffusion and boundary layer effects were also investigation. Therefore, the results show that coconut fiber, both modified and unmodified is an efficient sorbent for the removal of As (III) from industrial effluents with particle diffusion as the predominant mechanism.

Design of an adsorbent employing activated carbon fiber to remove lead

Zorflex® activated carbon fibers (ACF), reference FM100 198B, are used before and after an oxidizing procedure with H3PO4 to study the adsorption of Pb2+. The point of zero charge was determined for the modified and unmodified fiber giving values of 2.3 and 4.3, respectively. After oxidizing the ACF, the fiber showed to have a greater Pb2+ adsorption capacity in comparison with the unmodified fiber, which is related with the acid sites increase, where lead was mainly adsorbed. Determination of the BET area was carried out by nitrogen physisorption at 77K. ACFs presented superficial areas between 1000 and 1500 m²/g showing mostly, a microporous structure. The preliminary design of an adsorbent using the modified fiber is presented where the fiber superior physicochemical properties over the unmodified one are observed.

Reproductive ecology of the exotic tree Muntingia calabura L. (Muntingiaceae) in southeastern Brazil

The exotic tree Muntingia calabura L. (Muntingiaceae), a species native to Central America, is used as fish feed and fiber and cellulose production in Brazil. This study was carried out in urban areas and verified the reproductive biology of this plant species. Flower and fruit morphology, compatibility system, reproductive phenology, pollination and frugivore animals, and germination of disseminated seeds were recorded by standard field and laboratory procedures. This tree is self-compatible and autonomously self-pollinated, with its flowers being mainly visited by bees and its fruits consumed by birds and bats. Germination of its dispersed seeds is fast and occurs at a high rate. The results of this work suggest that M. calabura is very adaptable to cultivated areas,thus being an excellent choice for urban reforestation. However, its reproductive characteristics place this plant as an invasive species with significant potential in southeastern Brazil.

Characterization and treatment of sisal fiber residues for cement-based composite application

Sisal fiber is an important agricultural product used in the manufacture of ropes, rugs and also as a reinforcement of polymeric or cement-based composites. However, during the fiber production process a large amount of residues is generated which currently have a low potential for commercial use. The aim of this study is to characterize the agricultural residues by the production and improvement of sisal fiber, called field bush and refugo and verify the potentiality of their use in the reinforcement of cement-based composites. The residues were treated with wet-dry cycles and evaluated using tensile testing of fibers, scanning electron microscopy (SEM) and Fourier transform infrared (FTIR) spectroscopy. Compatibility with the cement-based matrix was evaluated through the fiber pull-out test and flexural test in composites reinforced with 2 % of sisal residues. The results indicate that the use of treated residue allows the production of composites with good mechanical properties that are superior to the traditional composites reinforced with natural sisal fibers.

Obtention of injectable platelets rich-fibrin (i-PRF) and its polymerization with bone graft: technical note

The use of autologous platelet concentrates, represent a promising and innovator tools in the medicine and dentistry today. The goal is to accelerate hard and soft tissue healing. Among them, the platelet-rich plasma (PRP) is the main alternative for use in liquid form (injectable). These injectable form ofplatelet concentrates are often used in regenerative procedures and demonstrate good results. The aim of this study is to present an alternative to these platelet concentrates using the platelet-rich fibrin in liquid form (injectable) and its use with particulated bone graft materials in the polymerized form.

Stereological study of the elastic fiber and smooth muscle cell system in the bovine and buffalo penis

Samples of ten penises of Mediterranean buffaloes and ten penises of Red Sindhi cattle were used. The thickness of the tunica albuginea (TA), distribution of smooth muscle cells (SMC) and volume density (Vv) of elastic system fibers in TA, corpus cavernosum (CC) and corpus spongiosum (CS) were evaluated. The Vv of elastic system fibers in buffalo and bovine penis was respectively 4.07% ±0.88% and 3.36% ±1.21% in TA; 17.32% ±2.21% and 13.14% ±1.27% (CC), 26.58% ±4.31% and 31.36% ±3.67% (CS). The CC of buffalo presented higher Vv of elastic fibers than bovine, while in the CS the Vv of elastic fibers in buffaloes was smaller than in cattle. The TA thickness showed a significant difference among the species studied. The arrangement of SMC in the bovine penises and in the water buffalo suggests that this pattern is common to animals that have fibroelastic penises.