Advances in sample preparation and HPLC-MS/MS methods for determining amyloid-ß peptide in biological samples: a review.

Alzheimer's disease (AD), a neurological disorder, is a major public health concern and the most common form of dementia. Its typical symptoms include memory loss, confusion, changes in personality, and cognitive impairment, which result in patients gradually losing independence. Over the last decades, some studies have focused on searching for effective biomarkers as early diagnostic indicators of AD. Amyloid-ß (Aß) peptides have been consolidated as reliable AD biomarkers and have been incorporated into modern diagnostic research criteria. However, quantitative analysis of Aß peptides in biological samples remains a challenge because both the sample and the physical-chemical properties of these peptides are complex. During clinical routine, Aß peptides are measured in the cerebrospinal fluid by immunoassays, but the availability of a specific antibody is critical-in some cases, an antibody may not exist, or its specificity may be inadequate, leading to low sensitivity and false results. HPLC-MS/MS has been reported as a sensitive and selective method for determining different fragments of Aß peptides in biological samples simultaneously. Developments in sample preparation techniques (preconcentration platforms) such as immunoprecipitation, 96-well plate SPME, online SPME, and fiber-in-tube SPME have enabled not only effective enrichment of Aß peptides present at trace levels in biological samples, but also efficient exclusion of interferents from the sample matrix (sample cleanup). This high extraction efficiency has provided MS platforms with higher sensitivity. Recently, methods affording LLOQ values as low as 5 pg mL-1 have been reported. Such low LLOQ values are adequate for quantifying Aß peptides in complex matrixes including cerebrospinal fluid (CSF) and plasma samples. This review summarizes the advances in mass spectrometry (MS)-based methods for quantifying Aß peptides and covers the period 1992-2022. Important considerations regarding the development of the HPLC-MS/MS method such as the sample preparation step, optimization of the HPLC-MS/MS parameters, and matrix effects are described. Clinical applications, difficulties related to analysis of plasma samples, and future trends of these MS/MS-based methods are also discussed.

Antifungal efficacy of atorvastatin-containing emulgel in the treatment of oral and vulvovaginal candidiasis.

Drug repositioning has been an important ally in the search for new antifungal drugs. Statins are drugs that act to prevent sterol synthesis in both humans and fungi and for this reason they are promissory candidates to be repositioned to treat mycoses. In this study we evaluated the antifungal activity of atorvastatin by in vitro tests to determine the minimum inhibitory concentration against azole resistant Candida albicans and its mechanisms of action. Moreover, the efficacy of both atorvastatin-loaded oral and vaginal emulgels (0.75%, 1.5% and 3% w/w) was evaluated by means of in vivo experimental models of oral and vulvovaginal candidiasis, respectively. The results showed that atorvastatin minimal inhibitory concentration against C. albicans was 31.25 µg/ml. In oral candidiasis experiments, the group treated with oral emulgel containing 3.0% atorvastatin showcased total reduction in fungal load after nine days of treatment. Intravaginal delivery atorvastatin emulgel showed considerable effectiveness at the concentration of 3% (65% of fungal burden reduction) after nine days of treatment. From these findings, it is possible to assert that atorvastatin may be promising for drug repositioning towards the treatment of these opportunistic mycoses.

Atorvastatin is a statin drug that presents antifungal activity. This study showed that atorvastatin-containing oral and vaginal emulgels were able to treat vulvovaginal and oral candidiasis of infected animal model. Therefore, we showcased that atorvastatin may be a possible therapeutic agent in order to be a used to control opportunistic mucosal fungal infections caused by Candida albicans.

Novel materials as capillary coatings for in-tube solid-phase microextraction for bioanalysis.

In-tube solid-phase microextraction with a capillary column as extraction device can be directly coupled with high-performance liquid chromatography systems (HPLC). The in-tube solid-phase microextraction technique has been continuously developed since it was introduced in 1997. New couplings have also been evaluated on the basis of state-of-the-art HPLC instruments. Different types of capillaries (wall-coated open tubular, porous layer open tubular, sorbent-packed, porous monolithic rods, or fiber-packed) with selective stationary phases (monoliths, magnetic nanoparticles, conducting polymers, restricted access materials, ionic liquids, carbon, deep eutectic solvents, and hybrid materials) have been developed to boost in-tube solid-phase microextraction performance (sorption capacity and selectivity). This technique has been successfully applied to analyze biological samples (serum, plasma, whole blood, hair, urine, milk, skin, and saliva) for therapeutic drug monitoring, to study biomarkers, to detect illicit drugs, to conduct metabolomics studies, and to assess exposure to drugs. This review describes current advances in in-tube solid-phase microextraction extraction devices and their application in bioanalysis.

Tunable Silver-Containing Stationary Phases for Multidimensional Gas Chromatography.

To achieve high separation power of complex samples using multidimensional gas chromatography (MDGC), the selectivity of the employed stationary phases is crucial. The nonpolar × polar column combination remains the most popular column set used in MDGC. However, resolution of mixtures containing light analytes possessing very similar properties remains a formidable challenge. The development of stationary phases that offer unique separation mechanisms have the potential to significantly improve MDGC separations, particularly in resolving coeluting peaks in complex samples. For the first time, a stationary phase containing silver(I) ions was successfully designed and employed as a second-dimension column using comprehensive two-dimensional gas chromatography (GC × GC) for the separation of mixtures containing alkynes, dienes, terpenes, esters, aldehydes, and ketones. Compared with a widely used nonpolar and polar column set, the silver-based column exhibited superior performance by providing better chromatographic resolution of coeluting compounds. A mixture of unsaturated fatty acids was successfully separated using a GC × GC method in which the elution order in the second dimension was highly dependent on the number of double bonds within the analytes.

A column switching ultrahigh-performance liquid chromatography-tandem mass spectrometry method to determine anandamide and 2-arachidonoylglycerol in plasma samples.

This study reports a fast, sensitive, and selective column switching ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method to determine the endocannabinoids (eCBs), anandamide (AEA), and 2-arachidonoylglycerol (2-AG) in plasma samples. This bidimensional system used a restricted access media column (RP-8 ADS, 25 mm × 4 mm × 25 µM) in the first dimension and a core-shell Kinetex C18 (100 mm × 2, 1.7 mm × 1 µM) column in the second dimension, followed by detection in a mass spectrometer triple quadrupole (multiple reactions monitoring mode) operating in the positive mode. RP-8 ADS was used for trace enrichment of eCBs (reverse phase partitioning) and macromolecular matrix size exclusion; the core-shell column was used for the chromatographic separation. The column switching UHPLC-MS/MS method presented a linear range spanning from 0.1 ng mL-1 (LOQ) to 6 ng mL-1 for AEA and from 0.04 ng mL-1 (LOQ) to 10 ng mL-1 for 2-AG. Excluding the LLOQ values, the precision assays provided coefficients of variation lower than 8% and accuracy with relative standard error values lower than 14%. Neither carryover nor matrix effects were detected. This high-throughput column switching method compared to conventional methods is time saving as it involves fewer steps, consumes less solvent, and presents lower LLOQ. The column switching UHPLC-MS/MS method was successfully applied to determine AEA and 2-AG in plasma samples obtained from Alzheimer's disease patients. Graphical abstract A column switching ultra high-performance liquid chromatography-tandem mass spectrometry method using RP-8 ADS column and core shell column to determine endocannabinoids in plasma samples.

Bisphenol A release from orthodontic adhesives measured in vitro and in vivo with gas chromatography.

INTRODUCTION: The objectives of this study were to quantify in vitro the Bisphenol A (BPA) release from 5 orthodontic composites and to assess in vivo the BPA level in patients' saliva and urine after bracket bonding with an orthodontic adhesive system. METHODS: For the in-vitro portion of this study, 5 orthodontic composites were evaluated: Eagle Spectrum (American Orthodontics, Sheboygan, Wis), Enlight (Ormco, Orange, Calif), Light Bond (Reliance Orthodontic Products, Itasca, Ill), Mono Lok II (Rocky Mountain Orthodontics, Denver, Colo), and Transbond XT (3M Unitek, Monrovia, Calif). Simulating intraoral conditions, the specimens were immersed in a water/ethanol solution, and the BPA (ng.g-1) liberation was measured after 30 minutes, 24 hours, 1 day, 1 week, and 1 month by the gas chromatography system coupled with mass spectrometry. Twenty patients indicated for fixed orthodontic treatment participated in the in-vivo study. Saliva samples were collected before bracket bonding and then 30 minutes, 24 hours, 1 day, 1 week, and 1 month after bonding the brackets. Urine samples were collected before bonding and then at 1 day, 1 week, and 1 month after bonding. The results were analyzed statistically using analysis of variance and Tukey posttest, with a significance level of 5%. RESULTS: All composites evaluated in vitro released small amounts of BPA. Enlight composite showed the greatest release, at 1 month. Regarding the in-vivo study, the mean BPA level in saliva increased significantly only at 30 minutes after bonding in comparison with measurements recorded before bonding. CONCLUSIONS: All orthodontic composites released BPA in vitro. Enlight and Light Bond had, respectively, the highest and lowest BPA releases in vitro. The in-vivo experiment showed that bracket bonding with the Transbond XT orthodontic adhesive system resulted in increased BPA levels in saliva and urine. The levels were significant but still lower than the reference dose for daily ingestion.

Organic-silica hybrid monolithic sorbents for sample preparation techniques: A review on advances in synthesis, characterization, and applications.

Organic-silica hybrid monolithic materials have attracted considerable attention as potential stationary phases in separation science. These materials combine the advantages of organic polymer and silica-based monoliths, including easy preparation, lower back pressure, high permeability, excellent mechanical strength, thermal stability, and tunable surface chemistry with high surface area and selectivity. The outstanding chromatographic efficiency as stationary phase of hybrid monolithic capillary columns for capillary liquid chromatography and capillary electrochromatography has been reported in many papers. Organic-silica hybrid monolithic materials have also been extensively used in the field of sample preparation. Owing to their surface functionalities, these porous sorbents offer unique selectivity for pre-concentration of different analytes in the most complex matrixes by fast dynamic transport. These sorbents not only improve the analytical method sensitivity, but also introduce novelties in terms of extraction devices and instrument coupling strategies. The current review covers the period spanning from 2017 to 2023 and describes the properties of organic-inorganic hybrid monolithic materials, the present status of this technology and summarizes recent developments in their use as innovative sorbents for microextraction sample preparation techniques (solid phase microextraction with pipette tip, offline in-tube SPME, in-tube SPME online with LC, and in-tube SPME directly coupled with mass spectrometry). Aspects such as the synthesis methods (sol-gel process, one-pot approach, and polyhedral oligomeric silsesquioxanes-based procedure), characterization techniques, and strategies to improve extraction efficiency in various applications in different areas (environmental, food, bioanalysis, and proteomics) are also discussed.

Fiber-in-tube SPME-CapLC-MS/MS method to determine Aß peptides in cerebrospinal fluid obtained from Alzheimer's patients.

Mass spectrometry is characterized by its high sensitivity, ability to measure very low analyte concentrations, specificity to distinguish between closely related compounds, availability to generate high-throughput methods for screening, and high multiplexing capacity. This technique has been used as a platform to analyze fluid biomarkers for Alzheimer's disease. However, more effective sample preparation procedures, preferably antibody-independent, and more automated mass spectrometry platforms with improved sensitivity, chromatographic separation, and high throughput are needed for this purpose. This short communication discusses the development of a fiber-in-tube SPME-CapLC-MS/MS method to determine Aß peptides in cerebrospinal fluid obtained from Alzheimer's disease patients. To obtain the fiber-in-tube SPME capillary, we longitudinally packed 22 nitinol fibers coated with a zwitterionic polymeric ionic liquid into the same length of the PEEK tube. In addition, this communication compares this fiber-in-tube SPME method with the conventional HPLC scale (HPLC-MS/MS) and when directly coupled to CapESI-MS/MS without chromatographic separation, and, as a case study, discusses the benefits and challenges inherent in miniaturizing the flow scale of the sample preparation technique (fiber-in-tube SPME) to the CapLC-MS/MS system. Fiber-in-tube SPME-CapLC-MS/MS provided LLOQ ranging from 0.09 to 0.10 ng mL-1, accuracy ranging from 91 to 117 % (recovery), and reproducibility of less than 18 % (RSD). Analysis of the cerebrospinal fluid samples obtained from Alzheimer's disease patients evidenced that the method is robust. At the capillary scale (10 µL min-1), this innovative method presented higher analytical sensitivity than the conventional HPLC-MS/MS scale. Although fiber-in-tube SPME directly coupled to CapESI-MS/MS offers advantages in terms of high throughput, the sample was dispersed and non-quantitatively desorbed from the capillary at low flow rate. These results highlighted that chromatographic separation is important to decrease the matrix effect and to achieve higher detectability, which is indispensable for bioanalysis.

Direct coupling of fiber-in-tube solid-phase microextraction with tandem mass spectrometry to determine amyloid beta peptides as biomarkers for Alzheimer's disease in cerebrospinal fluid samples.

Current research efforts at neurological diseases have focused on identifying novel biomarkers to aid in diagnosis, to provide accurate prognostic information, and to monitor disease progression. This study presents the direct coupling of fiber-in-tube solid-phase microextraction to tandem mass spectrometry as a reliable method to determine amyloid beta peptides (Aß38, Aß40, and Aß42) as biomarkers for Alzheimer's disease in cerebrospinal fluid (CSF) samples. To obtain the biocompatible fiber-in-tube SPME capillary, a PEEK tube segment was longitudinally packed with fine fibers [nitinol wires coated with a zwitterionic polymeric ionic liquid], to act as selective extraction medium. The fiber-in-tube SPME-MS/MS method integrated analyte extraction/enrichment and sample cleanup (exclusion of interferents) into one step. The method provided lower limits of quantification (LLOQ: 0.2 ng mL-1 for Aß38 and 0.1 ng mL-1 for Aß40 and Aß42), high precision (CV lower than 11.6%), and high accuracy (relative standard deviation lower than 15.1%). This method was successfully applied to determine Aß peptides in CSF samples obtained from AD patients (n = 8) and controls (healthy volunteers, n = 10). Results showed that Aß42 levels in the CSF samples obtained from AD patients were significantly lower compared to healthy controls (p < 0.05). On the basis of the ROC analysis results, the Aß42/Aß40 ratio (AUC = 0.950, p < 0.01; 95%) performed significantly better than Aß42 alone (AUC = 0.913, p < 0.01; 95%) in discriminating between AD patients and healthy controls and presented better diagnostic ability for AD. The novelties of this study are not only related to evaluating Aß peptides as AD biomarkers, but also to demonstrating direct online coupling of fiber-in-tube SPME with MS/MS as a quantitative high-throughput method for bioanalysis.

Crosslinked zwitterionic polymeric ionic liquid-functionalized nitinol wires for fiber-in-tube solid-phase microextraction and UHPLC-MS/MS as an amyloid beta peptide binding protein assay in biological fluids.

Alzheimer disease (AD) is a neurodegenerative disorder characterized by extracellular accumulation of amyloid-ß peptide (Aß) in the brain interstitium. Human serum albumin (HSA) highly binds to Aß in blood plasma and is thought to inhibit plaque formation in peripheral tissue. Thus, the evaluation of albumin binding to Aß is an important key to understand the dynamics of these molecules in the biological system of patients with AD. In this work, a fiber-in-tube solid-phase microextraction (fiber-in-tube SPME) and ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was developed to estimate Aß fraction binding to HSA in cerebrospinal fluid (CSF) and plasma samples. Crosslinked zwitterionic polymeric ionic liquid (zwitterionic PIL)-coated nitinol wires were developed and packed into a polyether ether ketone (PEEK) capillary for a fiber-in-tube SPME and UHPLC-MS/MS method. Zwitterionic PIL sorbent was synthetized from 1-vinyl-3-(butanesulfonate)imidazolium ([VIm+C4SO3-]) and 1,12-di(3-vinylimidazolium)dodecane dibromide ([(VIm)2C12]2[Br]) monomers by in-situ thermally-initiated polymerization. Morphological characterization by scanning electron microscopy (SEM) and atomic force microscopy (AFM) revealed a decrease in the surface roughness of the nitinol wires from ∼17 nm to 1 nm after the in-situ polymerization. The zwitterionic PIL sorbent selectively preconcentrates Aß through a two-pronged interaction mechanism. The fiber-in-tube SPME and UHPLC-MS/MS method presented lower limits of quantification (LLOQ) of 0.4 ng mL-1 for Aß38 and 0.3 ng mL-1 for Aß40 and Aß42, a linear range from LLOQ values to 15 ng mL-1 with coefficients of determination higher than 0.99, precision with coefficient of variation (CV) values ranging from 2.1 to 7.3% and accuracy with relative standard deviation (RSD) values from -0.3 to 7.4. This method was successfully applied to evaluate the binding of HSA to Aß in cerebrospinal fluid (CSF) and plasma samples.

Current advances and applications of online sample preparation techniques for miniaturized liquid chromatography systems.

Miniaturized liquid chromatography (LC) has been recognized as one of the most important analytical methods in several research fields. Reduced analytical work-scale provides superior chromatographic resolution and decreases sample and organic solvent consumption. However, frequent clogging of tubing connections and use of small sample volumes are significant limitations when high throughput and sensitive analyses are required. Effective sample preparation could help to overcome these limitations. Online coupling of sample preparation techniques (such as column switching and in-tube solid-phase microextraction) with these miniaturized systems may result in more sensitive and reproducible analyses, improving analytical efficiency. This review describes the most common online miniaturized LC configurations, and the main applications of current online sample preparation techniques coupled to miniaturized LC systems in the bioanalytical, omics, and environmental areas. Relevant features, and challenges of these systems, and innovative sorbents, including restricted access materials, monoliths, and immunosorbents is also discussed.

Validation study of the use of the HRVCAM software for the evaluation of heart rate and heart rate variability at rest.

Aims: The existing instruments for assessing heart rate (HR) and heart rate variability (HRV) require contact area. This is difficult to obtain from specific groups of patients and from those moving. The aim of this study was to validate the use of the HRVCam software for measuring HR and HRV in healthy adults. Methods and results: The HR and HRV variables were evaluated in terms of time and frequency using a webcam and Polar® S810i. The Shapiro-Wilk test was used to test the normality of the data, and the Pearson's correlation coefficient (r) was used to identify the possible correlation between the two instruments. The size of the effect was calculated based on a generalized linear model, and the Bland-Altman plots were used to analyse the agreement between the methods. The level of significance for all analyses was set at P < 0.05. We evaluated 102 participants, of whom 52% were men; 83.3% were aged between 18 and 29.9 years; and 84.3% were single. Conclusion: There was a good agreement and moderate to strong correlations among all analysed variables. The biases were low, except for the low frequency/high frequency measures. Moreover, the difference between the samples was small to moderate. The results of this study corroborate the use of HRVCam for measuring HR and HRV.

Innovative extraction materials for fiber-in-tube solid phase microextraction: A review.

Fiber-in-tube solid-phase microextraction (fiber-in-tube SPME) with short capillary longitudinally packed with fine fibers as extraction device allows direct coupling to high performance liquid chromatography (HPLC) systems to determine weakly volatile or thermally labile compounds. This technique associates the advantages of miniaturized and analytical on-line systems. Major achievements include the use of different capillaries (fused-silica, copper, stainless steel, polyetheretherketone (PEEK), or poly(tetrafluoroethylene) (PTFE)) that are packed with neat fibers (Zylon®, silk, or Kevlar 29®) or fibers (stainless steel, basalt, or carbon) functionalized with selective coatings (aerogels, ionic liquids (ILs), polymeric ionic liquids (PILs), molecularly imprinted polymers (MIPs), layered double hydroxides (LDHs), or conducting polymer). This review outlines the fundamental theory and the innovative extraction materials for fiber-in-tube SPME-HPLC systems and highlights their main applications in environmental and bioanalyses.

In-tube solid-phase microextraction directly coupled to tandem mass spectrometry for anandamide and 2-arachidonoylglycerol determination in rat brain samples from an animal model of Parkinson's disease.

To evaluate the endocannabinoid system in an animal model of Parkinson's disease, in-tube solid-phase microextraction (in-tube SPME) was directly coupled to a tandem mass spectrometry (MS/MS) system for determination of the endocannabinoids anandamide (AEA) and 2-arachidonoylglycerol (2-AG) in rat brain samples. In-tube SPME-which consisted of a microtube of restricted access material (RAM) with a hydrophilic diol external surface and a hydrophobic octyl inner surface-efficiently excluded (up to 95%) macromolecules from the biological samples and selectively pre-concentrated the analytes. In-tube SPME parameters, such as sample volume, mobile phases, flow rate, and pre-concentration time, were evaluated to improve the extraction efficiency and throughput performance. The selectivity of the in-tube SPME and MS/MS (MRM mode) techniques allowed them to be directly coupled online, which dismissed the need for the chromatographic separation step. The in-tube SPME-MS/MS method was validated and shown to be linear from 6.0 to 30.0 ng mL-1 for AEA and from 10.0 to 100.0 ng mL-1 for 2-AG; the intra- and inter-assay accuracy and precision were lower than 15%. Parallelism between the calibration curves constructed in the matrix and aqueous solution confirmed that there was no matrix effect. The method allowed endogenous concentrations of AEA and 2-AG to be determined in rat brain striatum from unilaterally 6-hydroxydopamine-lesioned animals. The concentrations of these endocannabinoids in striatum ipsilateral and contralateral to the lesion differed significantly (p<0.001).

Umbelliferone (7-hydroxycoumarin): A non-toxic antidiarrheal and antiulcerogenic coumarin.

Gastrointestinal diseases are very common problems; available treatments are very limited and come with a range of side effects. Coumarins are an extensive class of phenolic compounds that can be found in plants, fungi and bacteria. The 7-hydroxycoumarin, also known as umbelliferone (UMB), is a compound that comes from coumarin and has been showing biological activities in other studies. As of this scenario, the present study was designed to evaluate the acute oral toxicity, mutagenic, antidiarrheal, anti-bacterial, and antiulcerogenic effects, and antioxidant capacity of UMB. An investigation was conducted through the hippocratic screening method and through histopathological analysis in animals to evaluate the effects of acute oral administration of a dose of 50, 100 and 200 mg/kg of UMB. A micronucleus test on peripheral blood of Swiss mice, which were orally treated with three doses (50, 100 and 200 mg/kg), was conducted to evaluate mutagenic activities. The antiulcerogenic activity was accomplished through the ethanol-induced damage method. Antidiarrheal activities were tested for inducing diarrhea with castor oil and evaluating intestinal transit duration; additionally, the antimicrobial effect against some enteropathogenic bacteria was analyzed. Finally, the antioxidant capability was determined by the capacity of the UMB sample to kidnap the stable radical 2,2-diphenyl-1-picrylhydrazyl. Of the evaluated doses, signs of toxicity after acute administration of the compound were not observed. UMB presented antiulcerogenic activity (100 and 200 mg/kg), which was explained because of its antioxidant capacity. A gastro protective effect was similar to the positive control, and the UMB was able to significantly reduce intestinal transit, and also diarrheal symptoms. Furthermore, UMB had an anti-bacterial effect with minimum inhibitory concentration fluctuating between 62.5 and 1000 µg/mL. Based on these findings, we can suggest that UMB has important biological activities in vivo and in vitro and is not toxic under the evaluated circumstances, which demonstrates its large potential for pharmacological use.

Polymeric ionic liquid open tubular capillary column for on-line in-tube SPME coupled with UHPLC-MS/MS to determine endocannabinoids in plasma samples.

This manuscript describes the development of wall-coated open tubular capillary column with polymeric ionic liquids (PILs) for on-line in-tube solid phase microextraction coupled with ultra high-performance liquid chromatography tandem mass spectrometry (in-tube SPME/UHPLC-MS/MS) to determine anandamide (AEA) and 2-arachidonoyl glycerol (2 A G) in plasma samples. Selective PILs were synthetized from the [VC6IM][Cl], [VC16IM][Br], and [(VIM)2C10]2 [Br] - ionic liquids - by in-situ thermal-initiated polymerization in a fused silica capillary column for in-tube SPME. The synthesis procedure was optimized, and the capillary columns were characterized using spectroscopic and chromatography techniques. The chemically bonded and cross-linked PIL-based sorbent phase (thickness coating: 1.7 µm) presented high chemical and mechanical stability. Among the sorbents evaluated, the PIL-based capillary, [VC16IM][Br]/[(VIM)2C10]2 [Br] presented the best performance with a sorption capacity of 37,311 ng cm-3 and 48,307 ng cm-3 for AEA and 2 A G, respectively. This capillary was reused more than ninety times without significant changes in extraction efficiency. The in-tube SPME-UHPLC-MS/MS method presented a linear range from 0.1 ng mL-1 to 100 ng mL-1 for AEA, and from 0.05 ng mL-1 to 100 ng mL-1 for 2 A G, with coefficients of determination higher than 0.99, p-value for Lack-of-fit test higher than 0.05 (α of 0.05), precision with coefficient of variation (CV) values ranging from 1.6 to 14.0% and accuracy with relative standard deviation (RSD) values from -19.6% to 13.2%. This method was successfully applied to determine AEA and 2 A G in plasma patients with Parkinson's disease. The concentrations in these plasma samples ranged from 0.14 to 0.46 ng mL-1 for AEA and from <0.05 ng mL-1 to 0.51 ng mL-1 for 2-AG.

Recent development of chromatographic methods to determine parabens in breast milk samples: A review.

Parabens have been widely used as antimicrobial preservatives in food, drugs, and cosmetics for over 60 years. These endocrine disruptors can alter both the wildlife and the human hormone function. Determining these compounds in human milk is important because breast milk plays an important role in infant growth and in neurocognitive development. This article summarizes the current state-of-the-art of chromatographic methods to determine parabens in breast milk samples. Apart from the conventional and modern microextraction sample preparation techniques described herein, the authors discuss the chromatographic systems, primarily LC-MS/MS, and the concentration ranges at which parabens have been detected in milk samples obtained from lactating women over the past few years.

Avaliação de risco relativo ao uso de agrotóxicos na agricultura familiar / Risk assessment related to the use of pesticides in family farming

Objetivos ­ Identificar os agrotóxicos utilizados pelos agricultores familiares do povoado Passagem do Sargento, Juazeiro-BA e verificar os riscos à saúde do agricultor relacionados com o método de uso e a exposição a esses produtos. Métodos ­ Foram entrevistados quatro agricultores familiares e por meio de pesquisas na literatura, bulas dos agrotóxicos e consultas às fichas de informações de segurança de produtos químicos, foram identificados os possíveis efeitos dos agrotóxicos sobre a saúde e se os produtos químicos estão sendo utilizados de acordo com a praga e cultura às quais se destinam. Resultados ­ Verificou-se que os agricultores não seguem as indicações dos fabricantes contidas nos rótulos, seja em relação a frequência de seu uso, seja em relação à indicação da planta alvo. Além disso, um terço dos agrotóxicos utilizados por eles são classificados como extremamente tóxicos para a saúde humana, o que evidencia o potencial de danos de grande magnitude para os trabalhadores que os manuseiam, sobretudo por não seguirem as indicações contidas nas bulas. Conclusão ­ Diante dos riscos identificados, é necessária a atuação do poder público no fornecimento de assistência técnica, no sentido de fornecer informações adequadas para os agricultores familiares, buscando proteger esses trabalhadores dos efeitos nocivos dos agrotóxicos e viabilizar o processo produtivo.

Trends and association of BMI between sociodemographic and living conditions variables in the Brazilian elderly: 2002/03-2008/09. / Evolução e associação do IMC entre variáveis sociodemográficas e de condições de vida em idosos do Brasil: 2002/03-2008/09.

This study aimed to describe BMI's short-term trends and analyze the association between the Body Mass Index (BMI) and the sociodemographic variables and variables of family perception of the sufficiency and type of food consumed by Brazilian elderly of both sexes. The authors used data from the Household Budget Surveys (HBS) collected by the Brazilian Institute of Geography and Statistics (IBGE) in 2002/03 and 2008/09. The prevalence of overweight and obesity increased, whereas normal and low weight decreased. Multinomial regression models were used for 2008/09 to analyze the association between BMI and sociodemographic variables and variables of family perception of the sufficiency and type of food intake. Income and age were more associated with BMI. We suggest that health and nutrition prevention and monitoring measures be implemented through public policies, considering multifactorial overweight in the Brazilian elderly.

O objetivo foi descrever a evolução de curto prazo do índice de massa corporal (IMC) e analisar a associação entre este e variáveis sociodemográficas e de percepção familiar sobre a suficiência e o tipo dos alimentos consumidos em idosos brasileiros de ambos os sexos. Utilizaram-se dados das Pesquisas de Orçamentos Familiares (POF) coletados pelo Instituto Brasileiro de Geografia e Estatística (IBGE), em 2002/03 e em 2008/09. As prevalências de sobrepeso e obesidade aumentaram, e as de peso adequado e baixo peso diminuíram. Utilizaram-se modelos de regressão multinomial para 2008/09, a fim de analisar a associação entre o IMC e as características sociodemográficas e de percepção familiar sobre a suficiência e o tipo dos alimentos consumidos. Renda e idade se apresentaram mais associadas ao IMC. Sugere-se medidas de prevenção e monitoramento de saúde e nutrição por meio de políticas públicas, considerando a multifatorialidade do excesso de peso em idosos brasileiros.