Antitumoral melatonin-loaded nanostructured lipid carriers.

Aim: Cancer constitutes the second leading cause of death worldwide, with conventional therapies limited by significant side effects. Melatonin (MEL), a natural compound with antitumoral properties, suffers from instability and low solubility. To overcome these issues, MEL was encapsulated into nanostructured lipid carriers (MEL-NLC) containing rosehip oil to enhance stability and boost its antitumoral activity. Methods: MEL-NLC were optimized by a design of experiments approach and characterized for their physicochemical properties. Stability and biopharmaceutical behavior were assessed, along with interaction studies and in vitro antitumoral efficacy against various cancer cell lines. Results: Optimized MEL-NLC exhibited desirable physicochemical characteristics, including small particle size and sustained MEL release, along with long-term stability. In vitro studies demonstrated that MEL-NLC selectively induced cytotoxicity in several cancer cell lines while sparing healthy cells. Conclusion: MEL-NLC represent a promising alternative for cancer, combining enhanced stability and targeted antitumoral activity, potentially overcoming the limitations of conventional treatments.

Despite current advances, cancer is the second cause of death worldwide, but conventional therapies have side effects and limited efficacy. Natural therapies are emerging as suitable alternatives and, among them, Melatonin is a well-known compound with antitumoral properties. However, it is degraded by light, decreasing its therapeutical activity. In order to effectively deliver Melatonin into cancer cells, it has been encapsulated into biodegradable nanoparticles containing rosehip oil, which may boost the antitumoral properties. These nanoparticles have been optimized, showing a small size and a high Melatonin encapsulation, sustained drug release and good stability. Furthermore, in vitro studies demonstrated antitumoral activity against several cancer cell lines, also showing a high internalization inside them. Moreover, studies conducted using chicken embryonated eggs, showed that nanoparticles were non-toxic, thus confirming its promising therapeutical applications.

Combination of Indomethacin with Nanostructured Lipid Carriers for Effective Anticancer Therapy.

Purpose: The anticancer potential of indomethacin and other nonsteroidal anti-inflammatory drugs (NSAIDs) in vitro, in vivo, and in clinical trials is well known and widely reported in the literature, along with their side effects, which are mainly observed in the gastrointestinal tract. Here, we present a strategy for the application of the old drug indomethacin as an anticancer agent by encapsulating it in nanostructured lipid carriers (NLC). We describe the production method of IND-NLC, their physicochemical parameters, and the results of their antiproliferative activity against selected cancer cell lines, which were found to be higher compared to the activity of free indomethacin. Methods: IND-NLC were fabricated using the hot high-pressure homogenization method. The nanocarriers were physicochemically characterized, and their biopharmaceutical behaviour and therapeutic efficacy were evaluated in vitro. Results: Lipid nanoparticles IND-NLC exhibited a particle size of 168.1 nm, a negative surface charge (-30.1 mV), low polydispersity index (PDI of 0.139), and high encapsulation efficiency (over 99%). IND-NLC were stable for over 60 days and retained integrity during storage at 4 °C and 25 °C. The potential therapeutic benefits of IND-NLC were screened using in vitro cancer models, where nanocarriers with encapsulated drug effectively inhibited the growth of breast cancer cell line MDA-MB-468 at dosage 15.7 µM. Conclusion: We successfully developed IND-NLC for delivery of indomethacin to cancer cells and confirmed their antitumoral efficacy in in vitro studies. The results suggest that indomethacin encapsulated in lipid nanoparticles possesses high anticancer potential. Moreover, the presented strategy is highly promising and may offer a new alternative for future therapeutic drug innovations.

Determination of Fe, Cu, and Pb in edible oils using choline chloride:ethylene glycol deep eutectic solvent-based dispersive liquid-liquid microextraction associated with microwave-induced plasma optical emission spectrometry.

A new simple, fast and environmentally friendly deep eutectic solvent based dispersive liquid-liquid microextraction (DES-based DLLME) methodology assisted by vortex is presented for the separation and preconcentration of three elements (i.e., Fe, Cu and Pb) from edible oil samples (i.e., soybean, sunflower, rapeseed, sesame, and olive oil) prior to the determination by microwave-induced plasma optical emission spectrometry (MIP-OES). The deep eutectic solvent selected as extractant (i.e., choline chloride and ethylene glycol, 1:2) is synthesized and characterized by Fourier transform infrared spectroscopy (FT-IR), proton nuclear magnetic resonance spectroscopy (1H NMR) and differential scanning calorimetry (DSC), and the extraction conditions are optimized by a two steps experimental design. Under the optimum extraction conditions (i.e., diluted sample weight: 8.6 g; DES volume: 100 µL; extraction time: 1 min; centrifugation time and speed: 3 min and 3000 rpm; and dispersion system: vortex) the analytical method presents excellent linearity (i.e., R2 values higher than 0.99) in the range 10-500 µg kg-1, repeatability (i.e., CV values lower than 9.2%), and limits of detection (LOD) values of 3, 2 and 0.7 µg kg-1 for Pb, Fe and Cu, respectively. None of the analytes displayed amounts over the upper limit permitted by law, and recovery values of all analytes evaluated in the different samples using external standard calibration were close to 100%, which excludes significant matrix effects. Finally, AGREEprep metric has been used to evaluate the method greenness (final score of 0.47) and it has been compared successfully with previous publications for the same type of analytes and matrices.

Dually Active Apigenin-Loaded Nanostructured Lipid Carriers for Cancer Treatment.

Purpose: Cancer is one of the major causes of death worldwide affecting more than 19 million people. Traditional cancer therapies have many adverse effects and often result in unsatisfactory outcomes. Natural flavones, such as apigenin (APG), have demonstrated excellent antitumoral properties. However, they have a low aqueous solubility. To overcome this drawback, APG can be encapsulated in nanostructured lipid carriers (NLC). Therefore, we developed dual NLC encapsulating APG (APG-NLC) with a lipid matrix containing rosehip oil, which is known for its anti-inflammatory and antioxidant properties. Methods: Optimisation, physicochemical characterisation, biopharmaceutical behaviour, and therapeutic efficacy of this novel nanostructured system were assessed. Results: APG-NLC were optimized obtaining an average particle size below 200 nm, a surface charge of -20 mV, and an encapsulation efficiency over 99%. The APG-NLC released APG in a sustained manner, and the results showed that the formulation was stable for more than 10 months. In vitro studies showed that APG-NLC possess significant antiangiogenic activity in ovo and selective antiproliferative activity in several cancer cell lines without exhibiting toxicity in healthy cells. Conclusion: APG-NLC containing rosehip oil were optimised. They exhibit suitable physicochemical parameters, storage stability for more than 10 months, and prolonged APG release. Moreover, APG-NLC were internalised inside tumour cells, showing the capacity to cause cytotoxicity in cancer cells without damaging healthy cells.

A novel non-invasive colorectal cancer diagnostic method: Volatile organic compounds as biomarkers.

INTRODUCTION: Population-based fecal tests for colorectal cancer (CRC) screening have shown to reduce mortality thanks to the early detection of the disease. However, currently available fecal tests are limited in their sensitivity and specificity. Our aim is to look for volatile organic compounds in fecal samples as biomarkers for CRC detection. MATERIAL AND METHODS: Eighty participants were included; 24 had adenocarcinoma, 24 had adenomatous polyps and 32 presented no neoplasms. Fecal samples were collected 48 h preceding the colonoscopy from all participants, except CRC patient samples that were collected after 3-4 weeks from the colonoscopy. Magnetic headspace adsorptive extraction (Mag-HSAE) followed by thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS) was performed on stool samples to identify volatile organic compounds as biomarkers. RESULTS: p-Cresol was significantly more abundant in the cancer samples (P < 0.001) with an area under the curve (AUC) of 0.85 (CI 95%; 0.737-0.953), having a sensitivity and specificity of 83% and 82%, respectively. In addition, 3(4H)-dibenzofuranone,4a,9b-dihydro-8,9b-dimethyl- (3(4H)-DBZ) was also more abundant in the cancer samples (P < 0.001) with an AUC of 0.77 (CI 95%; 0.635-0.905), sensitivity of 78% and specificity of 75%. When combined (p-cresol and 3(4H)-DBZ), the AUC was 0.86, sensitivity 87% and specificity 79%. p-Cresol also appeared to be promising as a biomarker for pre-malignant lesions with an AUC of 0.69 (CI 95%; 0.534-0.862), sensitivity 83% and specificity 63%, P = 0.045. CONCLUSIONS: Volatile organic compounds emitted from feces and determined by a sensitive analytical methodology (Mag-HSAE-TD-GC-MS), employing a magnetic graphene oxide as extractant phase, could be used as a potential screening technology for CRC and pre-malignant lesions.

Magnetic dispersive solid-phase extraction using ZSM-5 zeolite/Fe2O3 composite coupled with screen-printed electrodes based electrochemical detector for determination of cadmium in urine samples.

A novel, simple, fast, sensitive and environmentally friendly approach is presented to determine cadmium in urine samples, combining magnetic dispersive solid-phase extraction (MDSPE) for sample preparation and screen-printed carbon electrodes (SPCEs) for square-wave anodic stripping voltammetry. This association involves the miniaturization of sample preparation and measurement process. Firstly, cadmium was extracted directly from urine samples employing a ZSM-5/Fe2O3, then, the composite enriched with cadmium was deposited onto the SPCE and finally covered with a suitable electrolyte for electrochemical detection. Thereby, the elution and detection of cadmium were carried out in a single step. To optimize experimental parameters affecting MDSPE, a two-step multivariate strategy has been employed. The method has been evaluated under optimized extraction/elution conditions (i.e., type of sorbent, ZSM-5/Fe2O3; amount of sorbent, 10 mg; sample pH, 6.8; extraction time, 5.5 min; and HCl concentration, 0.5 M) using standard addition calibration. Standard addition calibration curves gave a good linearity in the range from 0 to 30 µg L-1 with correlation coefficients ranging from 0.997 to 0.998 (N = 7). The limit of detection, evaluated empirically and statistically, ranged from 0.5 to 1.0 µg L-1 and from 0.4 to 0.8 µg L-1, respectively, which are lower than the threshold level established by the Ministry of Labour and Social Affairs (Spain) and World Health Organization for normal cadmium content in urine (i.e., 3.4 and 4.0 µg L-1, respectively). The repeatability of the proposed method was evaluated at 5 and 20 µg L-1 spiking levels obtaining coefficients of variation ranged between 12 and 15% (n = 6). A certified reference material (REC-8848/Level II) was analyzed to assess method accuracy finding 92% and 1.3 µg L-1 as the recovery (trueness) and standard deviation values, respectively. Finally, the method was applied to spiked urine samples, obtaining good agreement between spiked and found concentrations (recovery ranged from 89 to 98% and CV values ranged from 7% to 14%). Therefore, this is a new and successful contribution to the portable total analytical systems.

Determination of four bisphenols in water and urine samples by magnetic dispersive solid-phase extraction using a modified zeolite/iron oxide composite prior to liquid chromatography diode array detection.

A novel approach is presented to determine four bisphenols in water and urine samples, employing magnetic dispersive solid-phase extraction combined with liquid chromatography and diode array detection. A modified zeolite-based magnetic composite was used as an efficient sorbent, combining the advantages of magnetic materials with the remarkable properties of zeolites. A multivariate optimization design was employed to optimize some experimental factors affecting magnetic dispersive solid-phase extraction. The method was evaluated under optimized conditions (i.e., amount of sorbent, 50 mg; sample pH, unadjusted; NaCl concentration, 1.25%; extraction and elution time, 2 min; eluent solvent, ethanol; eluent solvent volume, 400 µL), obtaining good linearity with correlation coefficients ranging between 0.995 and 0.999 (N = 5) (from 2 to 250 µg/L for bisphenol A, bisphenol AP, and bisphenol P and from 5 to 250 µg/L for bisphenol AF). Method repeatability was assessed obtaining coefficients of variation between 3 and 11% (n = 6). Finally, the method was applied to spiked real samples, obtaining for water samples relative recoveries between 83 and 105%, and for urine samples between 81 and 108% for bisphenol A, bisphenol AP, and bisphenol AF, and between 47 and 59% for bisphenol P.

A modified zeolite/iron oxide composite as a sorbent for magnetic dispersive solid-phase extraction for the preconcentration of nonsteroidal anti-inflammatory drugs in water and urine samples.

This study is the first to use a new ZSM-5 zeolite-based composite decorated with iron oxide magnetic nanoparticles and modified with hexadecyltrimethylammonium bromide surfactant (i.e., HDTMA-ZSM-5/Fe2O3) as an efficient sorbent for magnetic dispersive solid-phase extraction (MDSPE) of nonsteroidal anti-inflammatory drugs in water and urine samples with subsequent measurement by liquid chromatography diode array detection. Experimental factors affecting MDSPE were optimized using a multivariate optimization strategy. The optimum experimental conditions were: amount of sorbent, 40 mg; sample pH, 2.2; NaCl concentration, 2.5%; extraction time, 2 min; eluent solvent, methanol; eluent solvent volume, 424 µL; and elution time, 2 min. The linearity of the method was studied from 3.3 to 400 µg L-1 (N = 8) for ketoprofen, from 1.7 to 400 µg L-1 (N = 8) for felbinac, from 6.6 to 400 µg L-1 (N = 7) for diclofenac and from 9.9 to 400 µg L-1 (N = 6) for ibuprofen. Method repeatability was evaluated at 10 and 200 µg L-1 spiking levels, obtaining coefficients of variation between 2 and 5% (n = 6). Limits of detection, determined empirically, were 1.0 µg L-1 , 0.5 µg L-1, 2.0 µg L-1 and 3.0 µg L-1 for ketoprofen, felbinac, diclofenac and ibuprofen, respectively. Tap water, reservoir water, wastewater and five urine samples were selected to assess method applicability. Recovery values ranged between 86-107% and 80-112% for water and urine samples, respectively, showing negligible matrix effects. Finally, this method was employed to monitor ibuprofen excretion in real urine samples.

Pruebas Terapéuticas Con Fines Diagnósticos En Trastornos Del Movimiento / Therapeutic Tests For The Diagnosis Of Movement Disorders

Resumen El diagnóstico en medicina tiene su piedra angular en la obtención de la historia clínica y la exploración física; sin embargo, en algunas de las patologías el uso de pruebas diagnósticas es de gran utilidad como apoyo para confirmar o descartar una enfermedad. Las pruebas diagnósticas incluyen una amplia variedad de procedimientos y dentro de estas se incluyen las pruebas terapéuticas, también llamadas desafíos o retos, en los que se administra una sustancia activa para evaluar la respuesta y apoyar la impresión diagnóstica. En el contexto de los trastornos del movimiento las pruebas terapéuticas más frecuentemente utilizadas son la de levodopa, apomorfina y etanol. En esta revisión se presenta, describe y discute el alcance y utilidad de estas.

Abstract The diagnosis in medicine has its cornerstone in obtaining the clinical history and in the physical examination. However, in some of the pathologies the use of diagnostic tests is very useful as a support to confirm or rule out a disease. Diagnostic tests include a wide variety of procedures and these include therapeutic tests, also called challenges, in which an active substance is administered to evaluate the response and support the presumptive diagnosis. In the context of movement disorders, the most frequently used therapeutic tests are those with levodopa, apomorphine and ethanol. In this review we present, describe and discuss the scope and usefulness of these challenges.

Determination of siloxanes in water samples employing graphene oxide/Fe3 O4 nanocomposite as sorbent for magnetic solid-phase extraction prior to GC-MS.

A new, fast, simple, and environmentally friendly analytical method has been developed to determine six siloxanes in water samples: octamethyltrisiloxane, octamethylcyclotetrasiloxane, decamethyltetrasiloxane, decamethylcyclopentasiloxane, dodecamethylpentasiloxane and dodecamethylcyclohexasiloxane. The analytical method consists of magnetic solid-phase extraction employing graphene oxide/Fe3 O4 as sorbent for the separation and preconcentration of siloxanes prior to GC-MS determination. The extraction procedure was optimized by means of a Plackett-Burman design. Under the optimized extraction conditions (graphene oxide/Fe3 O4 , 20 mg; extraction time, 10 min; eluent volume, 0.5 mL ACN; elution time, 2.5 min; sample volume, 20 mL), the method rendered repeatability levels with a relative standard deviation between 9 and 20% (n = 6, 10 µg/L). Methodological limits of detection ranged from 0.003 to 0.1 µg/L. The linearity of the method was studied between the methodological limit of quantification and 100 µg/L, obtaining correlation coefficient values between 0.990 and 0.999. The applicability of the method was assessed by analyzing drinking, river and wastewater samples. Relative recovery values ranged between 70 and 120% (1 and 60 µg/L spiking level) showing that the matrix had a negligible effect on extraction. Finally, the greenness of this method was confirmed by the semiquantitative Eco-Scale metrics.

Rapid determination of hydrophilic phenols in olive oil by vortex-assisted reversed-phase dispersive liquid-liquid microextraction and screen-printed carbon electrodes.

A novel approach is presented to determine hydrophilic phenols in olive oil samples, employing vortex-assisted reversed-phase dispersive liquid-liquid microextraction (RP-DLLME) for sample preparation and screen-printed carbon electrodes for voltammetric analysis. The oxidation of oleuropein, hydroxytyrosol, caffeic acid, ferulic acid and tyrosol was investigated, being caffeic acid and tyrosol selected for quantification. A matrix-matching calibration using sunflower oil as analyte-free sample diluted with hexane was employed to compensate matrix effects. Samples were analyzed under optimized RP-DLLME conditions, i.e., extractant phase, 1M HCl; extractant volume, 100µL; extraction time, 2min; centrifugation time, 10min; centrifugation speed, 4000rpm. The working range showed a good linearity between 0.075 and 2.5mgL-1 (r = 0.998, N = 7) for caffeic acid, and between 0.075 and 3mgL-1 (r = 0.999, N = 8) for tyrosol. The methodological limit of detection was empirically established at 0.022mgL-1 for both analytes, which is significantly lower than average contents found in olive oil samples. The repeatability was evaluated at two different spiking levels (i.e., 0.5mgL-1 and 2mgL-1) and coefficients of variation ranged from 8% to 11% (n = 5). The applicability of the proposed method was tested in olive oil samples of different quality (i.e., refined olive oil, virgin olive oil and extra virgin olive oil). Relative recoveries varied between 83% and 108% showing negligible matrix effects. Finally, fifteen samples were analyzed by the proposed method and a high correlation with the traditional Folin-Ciocalteu spectrophotometric method was obtained. Thereafter, the concentrations of the fifteen oil samples were employed as input variables in linear discriminant analysis in order to distinguish between olive oils of different quality.

Hydrophilic magnetic ionic liquid for magnetic headspace single-drop microextraction of chlorobenzenes prior to thermal desorption-gas chromatography-mass spectrometry.

A new, fast, easy to handle, and environmentally friendly magnetic headspace single-drop microextraction (Mag-HS-SDME) based on a magnetic ionic liquid (MIL) as an extractant solvent is presented. A small drop of the MIL 1-ethyl-3-methylimidazolium tetraisothiocyanatocobaltate(II) ([Emim]2[Co(NCS)4]) is located on one end of a small neodymium magnet to extract nine chlorobenzenes (1,2-dichlorobenzene, 1,3-dichlorobenzene, 1,4-dichlorobenzene, 1,2,3-trichlorobenzene, 1,2,4-trichlorobenzene, 1,3,5-trichlorobenzene, 1,2,3,4-tetrachlorobenzene, 1,2,4,5-tetrachlorobenzene, and pentachlorobenzene) as model analytes from water samples prior to thermal desorption-gas chromatography-mass spectrometry determination. A multivariate optimization strategy was employed to optimize experimental parameters affecting Mag-HS-SDME. The method was evaluated under optimized extraction conditions (i.e., sample volume, 20 mL; MIL volume, 1 µL; extraction time, 10 min; stirring speed, 1500 rpm; and ionic strength, 15% NaCl (w/v)), obtaining a linear response from 0.05 to 5 µg L-1 for all analytes. The repeatability of the proposed method was evaluated at 0.7 and 3 µg L-1 spiking levels and coefficients of variation ranged between 3 and 18% (n = 3). Limits of detection were in the order of nanograms per liter ranging from 4 ng L-1 for 1,4-dichlorobenzene and 1,2,3,4-tetrachlorobenzene to 8 ng L-1 for 1,2,4,5-tetrachlorobenzene. Finally, tap water, pond water, and wastewater were selected as real water samples to assess the applicability of the method. Relative recoveries varied between 82 and 114% showing negligible matrix effects. Graphical abstract Magnetic headspace single-drop microextraction followed by thermal desorption-gas chromatography-mass spectrometry.

Magnetic headspace adsorptive extraction of chlorobenzenes prior to thermal desorption gas chromatography-mass spectrometry.

This study presents a new, user-friendly, cost-effective and portable headspace solid-phase extraction technique based on graphene oxide decorated with iron oxide magnetic nanoparticles as sorbent, located on one end of a small neodymium magnet. Hence, the new headspace solid-phase extraction technique has been called Magnetic Headspace Adsorptive Extraction (Mag-HSAE). In order to assess Mag-HSAE technique applicability to model analytes, some chlorobenzenes were extracted from water samples prior to gas chromatography-mass spectrometry determination. A multivariate approach was employed to optimize the experimental parameters affecting Mag-HSAE. The method was evaluated under optimized extraction conditions (i.e., sample volume, 20 mL; extraction time, 30 min; sorbent amount, 10 mg; stirring speed, 1500 rpm, and ionic strength, non-significant), obtaining a linear response from 0.5 to 100 ng L-1 for 1,3-DCB, 1,4-DCB, 1,2-DCB, 1,3,5-TCB, 1,2,4-TCB and 1,2,3-TCB; from 0.5 to 75 ng L-1 for 1,2,4,5-TeCB, and PeCB; and from 1 to 75 ng L-1 for 1,2,3,4-TeCB. The repeatability of the proposed method was evaluated at 10 ng L-1 and 50 ng L-1 spiking levels, and coefficients of variation ranged between 1.5 and 9.5% (n = 5). Limits of detection values were found between 93 and 301 pg L-1. Finally, tap, mineral and effluent water were selected as real water samples to assess method applicability. Relative recoveries varied between 86 and 110% showing negligible matrix effects.

Graphene oxide/Fe3O4 as sorbent for magnetic solid-phase extraction coupled with liquid chromatography to determine 2,4,6-trinitrotoluene in water samples.

A fast, simple, economical, and environmentally friendly magnetic solid-phase extraction (MSPE) procedure has been developed to preconcentrate 2,4,6-trinitrotoluene (TNT) from water samples prior to determination by liquid chromatography-UV-Vis employing graphene oxide/Fe3O4 nanocomposite as sorbent. The nanocomposite synthesis was investigated, and the MSPE was optimized by a multivariate approach. The optimum MSPE conditions were 40 mg of nanocomposite, 10 min of vortex extraction, 1 mL of acetonitrile as eluent, and 6 min of desorption in an ultrasonic bath. Under the optimized experimental conditions, the method was evaluated to obtain a preconcentration factor of 153. The linearity of the method was studied from 1 to 100 µg L-1 (N = 5), obtaining a correlation coefficient of 0.994. The relative standard deviation and limit of detection were found to be 12% (n = 6, 10 µg L-1) and 0.3 µg L-1, respectively. The applicability of the method was investigated, analyzing three types of water samples (i.e., reservoir and drinking water and effluent wastewater) and recovery values ranged between 87 and 120% (50 µg L-1 spiking level), showing that the matrix had a negligible effect upon extraction. Finally, the semiquantitative Eco-Scale metrics confirmed the greenness of the developed method.

Zeolite/iron oxide composite as sorbent for magnetic solid-phase extraction of benzene, toluene, ethylbenzene and xylenes from water samples prior to gas chromatography⬜mass spectrometry.

This study reports a new composite based on ZSM-5 zeolite decorated with iron oxide magnetic nanoparticles as a valuable sorbent for magnetic solid-phase extraction (MSPE). A proposal is made to determine benzene, toluene, ethylbenzene and xylenes (BTEX) as model analytes in water samples using gas chromatography-mass spectrometry. A two-step multivariate optimization strategy, using Plackett⬜Burman and circumscribed central composite designs, was employed to optimize experimental parameters affecting MSPE. The method was evaluated under optimized extraction conditions (i.e., amount of sorbent, 138mg; extraction time, 11min; sample pH, pH of water (i.e., 5.5⬜6.5); eluent solvent volume, 0.5mL; and elution time, 5min), obtaining a linear response from 1 to 100µgL(↙1) for benzene; from 10 to 100µgL(↙1) for toluene, ethylbenzene and o-xylene; and from 10 to 75µgL(↙1) for m,p-xylene. The repeatability of the proposed method was evaluated at a 40µgL(↙1) spiking level and coefficients of variation ranged between 8 and 11% (n=5). Limits of detection were found to be 0.3µgL(↙1) for benzene and 3µgL(↙1) for the other analytes. These values satisfy the current normative of the Environmental Protection Agency and European Union for BTEX content in waters for human consumption. Finally, drinking water, wastewater and river water were selected as real water samples to assess the applicability of the method. Relative recoveries varied between 85% and 114% showing negligible matrix effects.

Diagnóstico inicial de febre reumática: avaliação da aplicabilidade dos critérios de Jones / Case series study with an initial diagnosis of rheumatic fever, hospitalized in a university hospital: evaluation of applicability of Jones Criteria

Introdução: A febre reumática (FR) é uma doença inflamatória que ocorre após infecção pelo estreptococo beta-hemolítico do grupo A, em indivíduos geneticamente predispostos, principalmente entre 5 e 15 anos, sem predomínio de sexo. O diagnóstico é clínico, através dos Critérios de Jones (CJ). Estatísticas indicam que o Brasil apresenta elevada incidência da doença. Objetivo: Avaliar o perfil de apresentação clínico-laboratorial e os desfechos em uma série de casos internados com diagnóstico inicial de FR. Metodologia: Estudo tipo série de casos com perfil observacional, descritivo e retrospectivo, realizado no Hospital Universitário Alcides Carneiro, em Campina Grande-PB. Resultados: Foram analisados 26 prontuários de pacientes, com idade média de 11,8 anos e procedentes de 11 municípios da Paraíba. A distribuição por sexo foi 61,5% feminino e 38,5% masculino. O diagnóstico foi confirmado em 50% dos pacientes. Daqueles que confirmaram o diagnóstico através dos CJ, associados ou não ao ecocardiograma, 40% apresentaram um critério maior e dois ou mais critérios menores. Houve simultaneidade dos seguintes critérios maiores: artrite e cardite em 40%; coreia e cardite em 10%; artrite, coreia e cardite em 10%. Coreia como sintoma isolado foi verificado em 10% desses pacientes. Conclusão: As dificuldades diagnósticas descritas pela literatura, devido à inespecificidade dos CJ, inexistência de sinal patognomônico ou teste laboratorial específico, além da grande variabilidade de manifestações clínicas foram também observadas neste estudo. As autoras sugerem uma revisão dos critérios clínicos e laboratoriais de forma a aumentar a sensibilidade diagnóstica na febre reumática.

Microwave-Assisted Extraction of Phenolic Compounds from Almond Skin Byproducts (Prunus amygdalus): A Multivariate Analysis Approach.

A microwave-assisted extraction (MAE) procedure to isolate phenolic compounds from almond skin byproducts was optimized. A three-level, three-factor Box-Behnken design was used to evaluate the effect of almond skin weight, microwave power, and irradiation time on total phenolic content (TPC) and antioxidant activity (DPPH). Almond skin weight was the most important parameter in the studied responses. The best extraction was achieved using 4 g, 60 s, 100 W, and 60 mL of 70% (v/v) ethanol. TPC, antioxidant activity (DPPH, FRAP), and chemical composition (HPLC-DAD-ESI-MS/MS) were determined by using the optimized method from seven different almond cultivars. Successful discrimination was obtained for all cultivars by using multivariate linear discriminant analysis (LDA), suggesting the influence of cultivar type on polyphenol content and antioxidant activity. The results show the potential of almond skin as a natural source of phenolics and the effectiveness of MAE for the reutilization of these byproducts.

Violência e família: possibilidades vinculativas e formas de subjetivação / Violence and family: binding possibilities and forms of subjectivity / La violencia y la familia: posibilidades de enlace y formas de subjetividad

Este artigo apresenta estudos realizados a partir do atendimento psicoterápico de base psicanalítica à mãe e à filha de uma família que têm a violência como principal elemento articulador de sua história. O homem contemporâneo, em sua busca incessante pela felicidade, vê-se impossibilitado de ter assegurada a satisfação plena de seus desejos, instalando um paradoxo. Essa análise possibilitou um olhar diferenciado sobre o sujeito contemporâneo e as estratégias deste para lidar com a questão do desamparo. A família apresentada ilustra como o vínculo se estabelece e se mantém através de um acordo inconsciente imposto ou mutuamente concluído. Trata-se de um conluio que possibilita a continuidade dos investimentos e dos benefícios ligados à subsistência do contrato narcísico. Os sujeitos, imbuídos da relação violenta, retratam que, ao tentar escapar do enfrentamento da violência fundamental, se lançam ao desamparo. Deste modo resta-lhes a destruição do outro como alternativa para afirmação da singularidade e alívio de sua tensão pulsional.

This article presents achieved studies from a family's psychoanalytic psychotherapy whose main articulator element of its history is the violence. Modern man, in his relentless pursuit of happiness, finds himself unable to be assured of full satisfaction of their desires, installing a paradox. This analysis allowed to discover a different point of view about the contemporary subject and his strategies for dealing with this helplessness issue. The family presented in this study illustrates the way how the link is established and maintained through an unconscious agreement, which is imposed or mutually concluded. It is a collusion that enables continued investments and benefits related to subsistence of the narcissistic contract. Subjects, which are imbued with the violent relationship, portray that the subject is cast helpless to try to avoid facing the fundamental violence. That implies to the subject try to destroy the other as the alternative to assert their own singularity and relieving their pulsional tensions.

Este trabajo presenta los estudios realizados a partir de terapia psicoanalítica para una madre y su hija de una familia que tiene la violencia como elemento articulador principal de su historia. El hombre moderno, en su incesante búsqueda de la felicidad, se ve incapaz de haber asegurado la plena satisfacción de sus deseos, instalando una paradoja. Este análisis permitió una visión diferenciada del sujeto contemporáneo y sus estrategias para hacer frente a la cuestión del desamparo. Esta familia ilustra cómo se establece y se mantiene el vinculo mediante un acuerdo inconsciente que se le impuso o mutuamente finalizado. Este es un truco que permite la continuación de las inversiones y los beneficios relacionados con la subsistencia del contrato narcisista. Los sujetos, imbuidos de la relación violenta, retratan que al intentar hacer frente a esta violencia fundamental, se lanzan el desamparo. De este modo, sigue siendo para ellos la destrucción del otro como alternativa para hacer valer la singularidad y el alivio de su tensión pulsional.

Determination of cyclic and linear siloxanes in wastewater samples by ultrasound-assisted dispersive liquid-liquid microextraction followed by gas chromatography-mass spectrometry.

A fast, simple and environmentally friendly ultrasound-assisted dispersive liquid-liquid microextraction (USA-DLLME) procedure has been developed to preconcentrate eight cyclic and linear siloxanes from wastewater samples prior to quantification by gas chromatography-mass spectrometry (GC-MS). A two-stage multivariate optimization approach has been developed employing a Plackett-Burman design for screening and selecting the significant factors involved in the USA-DLLME procedure, which was later optimized by means of a circumscribed central composite design. The optimum conditions were: extractant solvent volume, 13 µL; solvent type, chlorobenzene; sample volume, 13 mL; centrifugation speed, 2300 rpm; centrifugation time, 5 min; and sonication time, 2 min. Under the optimized experimental conditions the method gave levels of repeatability with coefficients of variation between 10 and 24% (n=7). Limits of detection were between 0.002 and 1.4 µg L(-1). Calculated calibration curves gave high levels of linearity with correlation coefficient values between 0.991 and 0.9997. Finally, the proposed method was applied for the analysis of wastewater samples. Relative recovery values ranged between 71 and 116% showing that the matrix had a negligible effect upon extraction. To our knowledge, this is the first time that combines LLME and GC-MS for the analysis of methylsiloxanes in wastewater samples.

Ocorrência de dor na coluna vertebral e sua relação com a qualidade de vida de manicures e pedicures / Occurrence of spinal column pain and its relation to the quality of life of manicures and pedicures / Ocurrencia de dolor de espalda y su relación con la calidad de vida de manicuras y pedicuras

Analisar em manicures e pedicures a ocorrência de dor na coluna vertebral e verificar sua relação com a qualidade de vida. Métodos: Realizou-se, no período de fevereiro a junho de 2010, uma pesquisa quantitativa, do tipo transversal e descritiva, envolvendo 30 profissionais entre 18 e 45 anos com, no mínimo, um ano de profissão. Após seleção, aplicaram-se dois questionários: o SF-36 e outro, elaborado pelas pesquisadoras, com questões referentes à atividade ocupacional (jornada e tempo de serviço), presença de dor e suas características (local, tipo, frequência e intensidade). Resultados: Das 30 participantes, 76,7% (n=23) relataram dor, sendo 63,3% (n=19) na coluna lombar e 46,7% (n=14) do tipo crônica (com duração há mais de 6 meses). Relatou-se frequência de dor diária em 36,7% (n=11), com média de intensidade de 6,1±2,24. A idade e o tempo de serviço apresentaram-se maior no grupo com dor, com 34,2±6,80 e 12,3±6,39 anos, respectivamente. Na qualidade de vida do grupo sem dor, os domínios ?capacidade funcional?, ?dor? e ?estado geral de saúde? obtiveram maiores pontuações em relação ao grupo com dor (p<0,05). Conclusão: Detectou-se elevada presença de dor na coluna vertebral das manicures e pedicures avaliadas, principalmente na região lombar, levando a limitações funcionais e, consequentemente, ao comprometimento na qualidade de vida...

To analyze the occurrence of spine column pain in manicures/pedicures and verify its relationship with quality of life. Methods: A quantitative and descriptive crosssectional research conducted from February to June 2010 with 30 professionals aged between 18 and 45 years and with at least one year of work experience. After selection, two questionnaires were applied: the SF-36 and another developed by the researchers with questions related to occupation (working hours and length of service), occurrence of pain and its characteristics (location, type, frequency and intensity). Results: Of the 30 participants, 76.7% (n=23) reported pain, with 63.3% (n=19) occurrence in the lumbar spine and 46.7% (n=14) occurrence of chronic type (lasting more than 6 months). A total of 36.7% (n=11) of interviewees reported daily pain with an average intensity of 6.1+2.24. Age and length of service rates were higher in the group of people who felt pain (34.2+6.80 and 12.3+6.39 years respectively). Regarding the quality of life in the group of people who did not feel pain, the domains ?functional capacity?, ?pain? and ?general health status? had higher scores when compared to the group of people who felt pain (p<0.05). Conclusion: It was detected a high occurrence of spinal column pain among manicures / pedicures, especially in the lumbar spine, leading to functional limitations, and a consequent change in quality of life...

Analizar la ocurrencia de dolor de espalda en manicuras y pedicuras y verificar su relación con la calidad de vida. Métodos: Una investigación cualitativa se realizó en el período entre febrero y junio de 2010, del tipo trasversal y descriptiva involucrando 30 profesionales entre los 18 y 45 años con un mínimo de un año de profesión. Después de la selección fueron aplicados dos cuestionarios: el SF-36 y otro elaborado por las investigadoras con preguntas sobre la actividad ocupacional (jornada y tiempo de servicio), presencia de dolor y sus características (local, tipo, frecuencia e intensidad). Resultados: De las 30 participantes, el 76,7% (n=23) relataron dolor, siendo el 63,3% (n=19) en La lumbar y el 46,7% (n=14) del tipo crónica (con duración de más de seis meses). Se relató la frecuencia de dolor diaria enel 36,7% (n=11) con media de intensidad de 6,1±2,24. La edad y el tiempo de servicio se presentaron mayores en el grupo com dolor con 34,2±6,80 e 12,3±6,39 años, respectivamente. Respecto la calidad de vida del grupo sin dolor, los dominios ?capacidad funcional?, ?dolor? y ?estado general de salud? obtuvieron mayores puntuaciones en relación al grupo con dolor (p<0,05). Conclusión: Se detectó elevada presencia de dolor de espalda de las manicuras y pedicuras evaluadas, principalmente en La lumbar, llevando a limitaciones funcionales y, en consecuencia, AL comprometimiento de la calidad de vida...