Otimização e validação do método para análise de microcontaminantes de preocupação emergente por cromatografia gasosa acoplada à espectrometria de massas utilizando derivatização online

Nas últimas décadas uma classe de contaminantes tem despertado interesse na comunidade científica, os microcontaminantes de preocupação emergente, em função dos seus possíveis efeitos adversos a humanos e ao meio ambiente. Dentro desse grupo, se destacam fármacos, antibióticos, produtos de higiene pessoal e desreguladores endócrinos. Como a remoção destes compostos em estações de tratamento de esgotos é geralmente ineficaz, eles chegam a corpos receptores, trazendo consequências à biota e aos seres humanos. Dentre os efeitos reportados, se destacam a preocupação com o aumento da resistência bacteriana, desregulação endócrina, distúrbios motores em animais aquáticos, dentre outros. Baseado nessas constatações, o presente trabalho envolve a validação e otimização, pelo planejamento de experimentos por superfície de respostas, do método de derivatização online, para determinação de 12 microcontaminantes de preocupação emergente por cromatografia em fase gasosa acoplada a espectrometria de massas. Foram avaliados 5 fármacos (ibuprofeno, diclofenaco, naproxeno, paracetamol e genfibrozila), compostos fenólicos, hormônios naturais e sintéticos de comprovada atividade estrogênica (4-nonilfenol, 4-octilfenol e bisfenol A, estrona, estradiol, etinilestradiol e estriol). No pré-tratamento da amostra foi utilizada extração em fase sólida (SPE), utilizando cartuchos Strata X e Strata SAX cujas recuperações variaram entre 70,8 a 109,3%. A otimização do método de derivatização online utilizou BSTFA e piridina. Os parâmetros investigados na otimização por superfície de respostas foram temperatura do injetor; pressão e volume de reagente derivatizante obtendo-se como condição ótima de análise 326,4 ºC de temperatura do injetor, 140 kPa de pressão do injetor e 1 μL de reagente derivatizante. Os limites de detecção e quantificação do método analítico variaram entre 0,8 a 20,6 ng.L-1 e 2,6 a 68,5 ng.L-1, respectivamente. O procedimento validado foi utilizado para analisar amostras de esgoto obtidas no Centro de Pesquisa e Treinamento em Saneamento UFMG/COPASA – CePTS, localizado na Estação de Tratamento de Esgoto Arrudas, em Belo Horizonte, Minas Gerais, Brasil. Nas amostras foram encontrados apenas bisfenol A (22,5 ng.L-1) e 4-octilfenol (13,0 ng.L-1).In recent decades a class of contaminants has attracted interest in the scientific community, microcontaminants of emerging concern, due to their possible adverse effects on humans and the environment. Within this group, there are drugs, antibiotics, personal care products and endocrine disrupters. As the removal of these compounds at sewage treatment plants is generally ineffective, they reach recipient bodies, bringing consequences to biota and humans. Among the reported effects, it is highlighted the concern with the increase of bacterial resistance, endocrine disruption, motor disorders in aquatic animals, among others. Based on these findings, the present work involves the method validation and optimization, by the response surface experimental design, to online derivatization, for the determination of 12 microcontaminants of emerging concern by gas chromatography coupled to mass spectrometry. Five drugs (ibuprofen, diclofenac, naproxen, paracetamol and genfibrozil), phenolic compounds, natural and synthetic hormones of proven estrogenic activity (4-nonylphenol, 4-octylphenol and bisphenol A, estrone, estradiol, ethinyl estradiol and estriol) were evaluated. In the pre-treatment of the sample solid phase extraction (SPE) was used, using Strata X and Strata SAX cartridges whose recoveries ranged from 70.8 to 109.3%. The optimization of the online derivatization method used BSTFA and pyridine. The parameters investigated in the response surface experimental design were (i) injector temperature; (2) injector pressure and (3) volume of derivatizing reagent. The optimal analysis condition obtained were 326.4 ºC of injector temperature, 140 kPa of injector pressure and 1 μL of derivatizing reagent. The limits of detection and quantification of the analytical method ranged from 0.8 to 20.6 ng.L-1 and 2.6 to 68.5 ng.L-1, respectively. The validated procedure was used to analyze sewage samples obtained at the UFMG / COPASA - CePTS Sanitation Research and Training Center, located at the Sewage Treatment Plant of Arrudas, in Belo Horizonte, Minas Gerais, Brazil. Only bisphenol A (22.5 ng.L-1) and 4-octylphenol (13.0 ng.L-1) were found in the samples

Otimiza??o e valida??o do m?todo para an?lise de microcontaminantes de preocupa??o emergente por cromatografia gasosa acoplada ? espectrometria de massas utilizando derivatiza??o online.

Programa de P?s-Gradua??o em Qu?mica. Departamento de Qu?mica, Instituto de Ci?ncias Exatas e Biol?gicas, Universidade Federal de Ouro Preto.Nas ?ltimas d?cadas uma classe de contaminantes tem despertado interesse na comunidade cient?fica, os microcontaminantes de preocupa??o emergente, em fun??o dos seus poss?veis efeitos adversos a humanos e ao meio ambiente. Dentro desse grupo, se destacam f?rmacos, antibi?ticos, produtos de higiene pessoal e desreguladores end?crinos. Como a remo??o destes compostos em esta??es de tratamento de esgotos ? geralmente ineficaz, eles chegam a corpos receptores, trazendo consequ?ncias ? biota e aos seres humanos. Dentre os efeitos reportados, se destacam a preocupa??o com o aumento da resist?ncia bacteriana, desregula??o end?crina, dist?rbios motores em animais aqu?ticos, dentre outros. Baseado nessas constata??es, o presente trabalho envolve a valida??o e otimiza??o, pelo planejamento de experimentos por superf?cie de respostas, do m?todo de derivatiza??o online, para determina??o de 12 microcontaminantes de preocupa??o emergente por cromatografia em fase gasosa acoplada a espectrometria de massas. Foram avaliados 5 f?rmacos (ibuprofeno, diclofenaco, naproxeno, paracetamol e genfibrozila), compostos fen?licos, horm?nios naturais e sint?ticos de comprovada atividade estrog?nica (4-nonilfenol, 4-octilfenol e bisfenol A, estrona, estradiol, etinilestradiol e estriol). No pr?-tratamento da amostra foi utilizada extra??o em fase s?lida (SPE), utilizando cartuchos Strata X e Strata SAX cujas recupera??es variaram entre 70,8 a 109,3%. A otimiza??o do m?todo de derivatiza??o online utilizou BSTFA e piridina. Os par?metros investigados na otimiza??o por superf?cie de respostas foram temperatura do injetor; press?o e volume de reagente derivatizante obtendo-se como condi??o ?tima de an?lise 326,4 ?C de temperatura do injetor, 140 kPa de press?o do injetor e 1 ?L de reagente derivatizante. Os limites de detec??o e quantifica??o do m?todo anal?tico variaram entre 0,8 a 20,6 ng.L-1 e 2,6 a 68,5 ng.L-1, respectivamente. O procedimento validado foi utilizado para analisar amostras de esgoto obtidas no Centro de Pesquisa e Treinamento em Saneamento UFMG/COPASA ? CePTS, localizado na Esta??o de Tratamento de Esgoto Arrudas, em Belo Horizonte, Minas Gerais, Brasil. Nas amostras foram encontrados apenas bisfenol A (22,5 ng.L-1) e 4-octilfenol (13,0 ng.L-1).In recent decades a class of contaminants has attracted interest in the scientific community, microcontaminants of emerging concern, due to their possible adverse effects on humans and the environment. Within this group, there are drugs, antibiotics, personal care products and endocrine disrupters. As the removal of these compounds at sewage treatment plants is generally ineffective, they reach recipient bodies, bringing consequences to biota and humans. Among the reported effects, it is highlighted the concern with the increase of bacterial resistance, endocrine disruption, motor disorders in aquatic animals, among others. Based on these findings, the present work involves the method validation and optimization, by the response surface experimental design, to online derivatization, for the determination of 12 microcontaminants of emerging concern by gas chromatography coupled to mass spectrometry. Five drugs (ibuprofen, diclofenac, naproxen, paracetamol and genfibrozil), phenolic compounds, natural and synthetic hormones of proven estrogenic activity (4-nonylphenol, 4-octylphenol and bisphenol A, estrone, estradiol, ethinyl estradiol and estriol) were evaluated. In the pre-treatment of the sample solid phase extraction (SPE) was used, using Strata X and Strata SAX cartridges whose recoveries ranged from 70.8 to 109.3%. The optimization of the online derivatization method used BSTFA and pyridine. The parameters investigated in the response surface experimental design were (i) injector temperature; (2) injector pressure and (3) volume of derivatizing reagent. The optimal analysis condition obtained were 326.4 ?C of injector temperature, 140 kPa of injector pressure and 1 ?L of derivatizing reagent. The limits of detection and quantification of the analytical method ranged from 0.8 to 20.6 ng.L-1 and 2.6 to 68.5 ng.L-1, respectively. The validated procedure was used to analyze sewage samples obtained at the UFMG / COPASA - CePTS Sanitation Research and Training Center, located at the Sewage Treatment Plant of Arrudas, in Belo Horizonte, Minas Gerais, Brazil. Only bisphenol A (22.5 ng.L-1) and 4-octylphenol (13.0 ng.L-1) were found in the samples

Behavior of micropollutants in polishing units that combine sorption and biodegradation mechanisms to improve the quality of activated sludge effluent.

The current study evaluated the removal of six micropollutants (estrone (E1); 17?-estradiol (E2); 17?-ethynylestradiol (EE2); ibuprofen (IBP), diclofenac (DCF), and paracetamol (PCT)) from the final effluent of an activated sludge domestic sewage treatment plant using polishing filters. Four polishing filters were assembled as columns and filled with a mixture of sand and vermiculite, sand and charcoal, sand and granulated activated carbon (9:1 by volume), and sand only. The column filters were placed near the outlet of a full-scale activated sludge treatment plant and were fed with a treated effluent containing from 4.71 to 28.93 ng L-1 of the target compounds at a hydraulic loading rate (HLR) of 50 m3 m?2 day?1. Samples were collected periodically from the influent (biologically treated sewage) and effluent of the four columns and analyzed for estrogens, anti-inflammatories, and analgesic compounds. Liquid samples were submitted to a solid phase extraction (SPE) and analyzed by gas chromatography coupled with mass spectrometry after their derivatization. Among the compounds found, diclofenac was distinguished by the high occurrence of detection in the samples (85%) and higher mean concentration (~?17 ng L?1). High removal efficiency (>?90%) of the estrogens was observed in the polishing systems studied, while for the other targets, the removal efficiency varied from 10 to 30%. The concentration values of some compounds were low, probably due to rainfall during the sampling period

AMAZONIA CAMTRAP: A data set of mammal, bird, and reptile species recorded with camera traps in the Amazon forest

The Amazon forest has the highest biodiversity on Earth. However, information on Amazonian vertebrate diversity is still deficient and scattered across the published, peer-reviewed, and gray literature and in unpublished raw data. Camera traps are an effective non-invasive method of surveying vertebrates, applicable to different scales of time and space. In this study, we organized and standardized camera trap records from different Amazon regions to compile the most extensive data set of inventories of mammal, bird, and reptile species ever assembled for the area. The complete data set comprises 154,123 records of 317 species (185 birds, 119 mammals, and 13 reptiles) gathered from surveys from the Amazonian portion of eight countries (Brazil, Bolivia, Colombia, Ecuador, French Guiana, Peru, Suriname, and Venezuela). The most frequently recorded species per taxa were: mammals: Cuniculus paca (11,907 records); birds: Pauxi tuberosa (3713 records); and reptiles: Tupinambis teguixin (716 records). The information detailed in this data paper opens up opportunities for new ecological studies at different spatial and temporal scales, allowing for a more accurate evaluation of the effects of habitat loss, fragmentation, climate change, and other human-mediated defaunation processes in one of the most important and threatened tropical environments in the world. The data set is not copyright restricted; please cite this data paper when using its data in publications and we also request that researchers and educators inform us of how they are using these data

Guidelines for the use and interpretation of assays for monitoring autophagy (4th edition)

In 2008, we published the first set of guidelines for standardizing research in autophagy. Since then, this topic has received increasing attention, and many scientists have entered the field. Our knowledge base and relevant new technologies have also been expanding. Thus, it is important to formulate on a regular basis updated guidelines for monitoring autophagy in different organisms. Despite numerous reviews, there continues to be confusion regarding acceptable methods to evaluate autophagy, especially in multicellular eukaryotes. Here, we present a set of guidelines for investigators to select and interpret methods to examine autophagy and related processes, and for reviewers to provide realistic and reasonable critiques of reports that are focused on these processes. These guidelines are not meant to be a dogmatic set of rules, because the appropriateness of any assay largely depends on the question being asked and the system being used. Moreover, no individual assay is perfect for every situation, calling for the use of multiple techniques to properly monitor autophagy in each experimental setting. Finally, several core components of the autophagy machinery have been implicated in distinct autophagic processes (canonical and noncanonical autophagy), implying that genetic approaches to block autophagy should rely on targeting two or more autophagy-related genes that ideally participate in distinct steps of the pathway. Along similar lines, because multiple proteins involved in autophagy also regulate other cellular pathways including apoptosis, not all of them can be used as a specific marker for bona fide autophagic responses. Here, we critically discuss current methods of assessing autophagy and the information they can, or cannot, provide. Our ultimate goal is to encourage intellectual and technical innovation in the field