The authors have no acknowledgements.

1. Preparação de EOB-DTPA e Ga [EOB-DTPA] Cuidado: Por favor, consulte todas as folhas de dados de segurança pertinentes (MSDS) dos utilizados solventes orgânicos, ácidos e alcalinos antes do uso. Execute todas as etapas em um exaustor e usar equipamentos de proteção individual (óculos de segurança, luvas, jaleco). <ol><li> Isolamento de EOB-DTPA a partir de ácido gadoxético <ol><li> Coloque 3 ml de solução injectável gadoxético 0,25 M de ácido para um balão. Adicionar 500 mg (5,6 mmol) de ácido oxálico à solução agitada. </li><li> Depois de se agitar durante 1 hora, filtrar a suspensão através de uma frita utilizando pressão reduzida. Lavar o resíduo três vezes com 3 ml de água, respectivamente. </li><li> Combinar os filtrados aquosos e equipar a solução com um eléctrodo de pH. Adiciona-se ácido clorídrico 12 M para o filtrado até que o pH é de cerca de -0,1. </li><li> Remover o solvente in vácuo para se obter um resíduo incolor. Armazenar sob gás inerte. </li><li> Lavar o resíduo cuidadosamente (pelo menos trêsvezes) com acetato de etilo para remover o excesso de ácido oxálico. Secar o resíduo em vácuo. </li><li> Redissolve-se o resíduo em 2 ml de água à temperatura ambiente e depois arrefece-se a solução num banho de gelo. Sem remover o banho de gelo, adicionar 0,5 M de hidróxido de sódio aquoso a solução gota a gota, até que a formação de um sólido incolor é observado pegajosa. </li><li> Remover a água por decantação. Lavar os sólidos mais duas vezes com 1 ml de água fria. Seca-se o sólido in vácuo para se obter a primeira fracção do produto. </li><li> Isolar uma segunda fracção de produto a partir das fracções combinadas de água decantada por meio de cromatografia em coluna (sílica, metanol / água 01/04). 24 Remover o solvente em vácuo. </li><li> Se o sólido assim obtido não é puro branco, dissolvê-la em 1 ml de água, adicionar 10 ml de etanol e subsequentemente 10 ml de éter dietílico para precipitar o produto. Filtra-se através de um filtro poroso utilizando pressão reduzida e seca in vácuo. </li><li> Combinarambas as frações sólidas de EOB-DTPA e realizar espectroscopia de RMN, 25 de espectrometria de massa 26 e elementares 27 análises. </li></ol></li><li> Síntese de Ga [EOB-DTPA] CUIDADO: Loja cloreto de sólido Ga (III) sob uma atmosfera inerte seca, uma vez que ao entrar em contato com o ar, humidade ou a decomposição da graxa ocorre, resultando em vapores corrosivos e formação de impurezas amarelos, castanhos ou pretos. <ol><li> Prepara-se uma solução de estoque de 0,11 M por dissolução de 1,94 g (11,0 mmol) de Ga (III) cloreto em 100 ml de água. Dilui-se 1 ml de solução de amoníaco aquoso a 25% com 4 ml de água. </li><li> Dissolve-se 80 mg (0,15 mmol) de EOB-DTPA num balão de 10 ml de água. Se necessário, aquecer o solvente para se conseguir a dissolução completa. </li><li> Adicionar 1,4 ml (0,15 mmol) da solução de cloreto de Ga (III). Equipar o frasco com um agitador e pH-eletrodo. Adicionar gota a gota uma solução de amoníaco diluído aquoso até que o pH da solução é de aproximadamente 4,1. Agita-se à rotemperatura om durante 30 minutos. </li><li> Remover o solvente em vácuo. Colocar o resíduo num balão, equipado com um stillhead com uma tubuladura lateral central e paralela. Equipar a central do pescoço com um dedo de arrefecimento e do pescoço lado com uma saída da bomba de vácuo </li><li> Aquece-se o resíduo sob pressão reduzida (125 ° C, 0,6 mbar). Periodicamente remover o cloreto de amónio sublimado (visível como revestimento branco da superfície de vidro) a partir do dedo de refrigeração e ainda cabeça, bem como a partir das partes superiores do frasco com um pano ligeiramente molhado. Continuar o processo até que não há formação visível de novo sublimado. </li><li> Para remover os vestígios finais de cloreto de amónio lavar o resíduo três vezes com 0,5 ml de metanol quente, respectivamente. Seca-se o resíduo incolor em vácuo. Execute NMR espectroscópica, 25 de massa por espectrometria de 26 e elementares 27 análises. </li></ol></li></ol> 2. Procedimento Geral Labeling ATENÇÃO: Todos os exexperi- incluindo contato direto ou indireto com substâncias radioactivas devem ser realizadas apenas por pessoal treinado. Por favor, use equipamento de proteção adequado. Recolher quaisquer resíduos radioactivos separadamente e armazenar e descartar de acordo com os regulamentos válidos. <ol><li> A eluição do gerador Nota: A 40 mCi 68 Ge / 68Ga gerador com o nuclido mãe ligado como óxido sobre sílica dodecil-3,4,5-trihydroxybenzoate foi usada. A eluição e a purificação pode ser realizada manualmente ou, como foi o caso no presente processo, tal como um processo automatizado combinada utilizando uma bomba peristáltica e unidade de distribuição. <ol><li> Preparar soluções de 5,5 M, 1,0 M e ácido clorídrico 0,05 M. Prepara-se uma solução de cloreto de sódio 5,0 M contendo 25 uL de ácido clorídrico 5,5 M por ml. Prepara-se uma solução tampão de pH 4,6 através da combinação de 4,1 g de acetato de sódio, 1 mL de HCl (30%) e 2,5 ml de ácido acético glacial e diluindo a mistura com água até 50 ml. </li><li> precondition o PS-H + cartucho enxaguando-o devagar com 1 ml de ácido clorídrico 1,0 M e, subsequentemente, 5 ml de água. </li><li> Elui-se a coluna de sílica do gerador com 4 ml de 0,05 M de HCl. 12 Carregar o 68Ga eluato para o PS-H + cartucho. </li><li> Passar o cartucho com 5 ml de água e subsequentemente secá-lo com 5 ml de ar. Eluir a 68 Ga a partir do cartucho com 1 ml de 5,0 M de solução de cloreto de sódio acidificada. 28 </li></ol></li><li> Etiquetagem de EOB-DTPA com 68Ga <ol><li> Dissolve-se 1 mg (1,9 umol) de EOB-DTPA em 1 ml de água. A partir desta solução ter 100 uL (0,19 nmol) e diluí-los com 9,9 ml de água para preparar um 19 uM (10 ug / ml) da solução de EOB-DTPA. </li><li> Remover 50 pi (equivalentes a 22-29 MBq) da solução contendo 68 Ga e colocado num frasco. Adicionam-se 50 ul (0,5 ug) de uma solução de estoque 19 mM de EOB-DTPA e 300 ul óf tampão para elevar o pH a 4,0. Agitar rapidamente e incubar a solução à temperatura ambiente durante 5 min. Retirar uma alíquota de 1-5 ul e colocar a HPLC ou análise TLC. </li><li> Realizar a análise por HPLC de rádio em um de fase inversa (RP) C18 29 Uso da seguinte fase móvel:. A - água ácido trifluoroacético / (99,9% / 0,1%), B - acetonitrilo / ácido trif luoroacético (99,9% / 0,1%), gradiente : 06 min 80% de A → 0% de A (0,5 ml / min), 610 min 0% de A (0,5 ml / min). </li><li> Determinar as intensidades dos picos dos sinais de rádio HPLC, como área sob a curva. Calcular o rendimento da marcação de pureza radioquímica (RCP) do traçador como se segue: RCP = A Ga-EOB-DTPA / (A Ga + A Ga-EOB-DTPA) ∙ 100% A Ga-EOB-DTPA: área sob a curva de 68 Ga [EOB-DTPA] A Ga: área sob a curva de livre 68 Ga </li></ol></li></ol> Eficiência 3. Rotulagem <ol><li> Realizar procedimentos de rotulagem como descreverd na seção 2. Use uma gama consistente de iniciar a atividade de 68 Ga fluido, por exemplo, 22-29 MBq (40-140 ul, dependendo da frescura do eluato). </li><li> Adicionar a quantidade necessária de solução tampão para ajustar o pH a 3,8-4,0 (40-190 ul, dependendo do volume de fluido 68 Ga). Adicionar a quantidade necessária de solução de reserva de ligando (10-70 ul de uma solução a 19 mM). </li><li> Adicionar as quantidades necessárias de água para ajustar o volume global de cada sonda rotulagem para 1,75 ml. Misturar completamente e deixar a amostra repousar durante 5 min à temperatura ambiente. Realizar análise HPLC como descrito na seção 2 para determinar o rendimento de marcação. </li><li> Realizar procedimentos de rotulagem com quantidades de ligante entre 0,1 mg e 0,7 mg em intervalos de 0,1 g. Realizar experiências em triplicado para cada concentração de ligando. Calcule o rendimento de média e desvio padrão. </li></ol> 4. Vitro estabilidade na <ol><li> p geralROCEDIMENTO e preparações <ol><li> Dissolve-se um comprimido de tampão fosfato salino (PBS) em 200 ml de água desionizada para se preparar uma solução stock de PBS com uma concentração de fosfato de 10 mM. </li><li> Realizar etiquetagem de 22-29 MBq 68Ga com 0,5 ml de solução de estoque EOB-DTPA, como descrito na secção 2. Dependendo do volume do eluato 68Ga, ajustar a quantidade de tampão, como descrito na secção 3. Retirar amostras de solução de rotulagem contendo 6-12 MBq de traçador para realizar medições de estabilidade. </li><li> Realizar a análise TLC rádio sobre gel de sílica placas de alumínio revestidas de 80 mm utilizando citrato de sódio 0,1 M aquoso como eluente e analisar as placas com um leitor de radioactividade TLC. 30 Determinar as intensidades dos sinais de TLC como a área sob a curva. Calcula-se a RCP do traçador como se segue: RCP = A Ga-EOB-DTPA / (A Ga-livre + A Ga-EOB-DTPA + A Ga-coloidal) ∙ 100% A Ga-EOB-DTPA: área sob a curva de 68 Ga [EOB-DTPA] A Ga-livre: área sob a curva de livre 68 Ga A Ga-coloidal: área sob a curva de coloidal 68 Ga </li><li> Calcule RCP t / RCP 0 para cada ponto de tempo. Traçar a RCP assim padronizado vs. diferença de tempo desde o ponto de partida t = 0 min. RCP t = RCP de 68 Ga [EOB-DTPA] no ponto de tempo t. RCP 0 = RCP de 68 Ga [EOB-DTPA] em t = 0 min. </li></ol></li><li> Estabilidade em tampão fosfato salino (A) <ol><li> A 65 ul de solução de etiquetagem adicionar 150 ul de solução de reserva de PBS e 60 ul de solução de hidróxido de sódio (0,1 M) para elevar o pH para 7,4. Homogeneizar. </li><li> Retirar uma alíquota de 1-5 ul para realizar a análise TLC ( &#39;ponto de partida&#39;). armazenar imediatamente a solução numa incubadora a 37 ° C e remover aliquotas para realizar a análise de cromatografia em camada fina representamAtivE pontos de tempo ao longo de 3 h. </li></ol></li><li> Estabilidade no sentido excesso de apo -transferrin em PBS (B) <ol><li> A 120 ul de solução de etiquetagem adicionar 50 ul de solução de reserva de PBS e 430 ul de uma solução de hidróxido de sódio (0,1 M) para elevar o pH para 7,4. Adicionar 40 ul de uma solução de Apo -transferrin (25 mg / ml). Homogeneizar. </li><li> Retirar uma alíquota de 1-5 ul para realizar a análise TLC ( &#39;ponto de partida&#39;). armazenar imediatamente a solução numa incubadora a 37 ° C e remover aliquotas para realizar a análise de TLC em pontos temporais representativos ao longo de 3 h. </li></ol></li><li> Estabilidade no soro humano (C) <ol><li> A 500 ul de soro humano adicionar 25 ul de solução de etiquetagem e 45 ul de solução de hidróxido de sódio (0,1 M) para elevar o pH para 7,4. Homogeneizar. </li><li> Retirar uma alíquota de 1-5 ul para realizar a análise TLC ( &#39;ponto de partida&#39;). armazenar imediatamente a solução em uma incuBator a 37 ° C e remover aliquotas para realizar a análise de TLC em pontos temporais representativos ao longo de 3 h. </li></ol></li></ol> 5. Determinação do coeficiente de distribuição LoGD <ol><li> Executar procedimentos de marcação, tal como descrito na secção 2. 50 ul de solução de etiquetagem adicionar 20 ul de solução de reserva de PBS e 170 ul de uma solução de hidróxido de sódio (0,1 M) para elevar o pH para 7,4. </li><li> Retirar 200 ul a partir dessa solução e colocá-la em um plástico V-frasco. Adicionar 200 ul de n-octanol. Fechar o frasco e agitar com vortex durante 2 min. Em seguida centrifugar a amostra a 1600 xg durante 5 min. </li><li> Remover triplicatas de 40 ul da fase n -octanol e a fase aquosa cada um e colocá-los em V-frascos separados. Tenha cuidado para não misturar as camadas. </li><li> Medir a actividade de cada uma das amostras num contador gama bem durante 30 segundos. Para cada amostra imediatamente repetir a medição e duas vezes da mesma calcular a actividade Ᾱ t significativo </sub&gt; em contagens por minuto (cpm). Listar o, assim, ganhou Ᾱ t, W1, Ᾱ t, W2 e Ᾱ t, W3 (atividades em amostras aquosas) e Ᾱ t, O1, Ᾱ t, O2, Ᾱ t, O3 (atividades em n- octanol), juntamente com o respectivo ponto de tempo t de sua determinação. </li><li> Definir o ponto de tempo da medição da última amostra, tal como t 0. Determinar e listar Dt em min calculando Dt = tt 0. Realizar correcção de decaimento Ᾱ t, usando a seguinte fórmula: Ᾱ 0 = Ᾱ T · 2 (Dt / 68 min). </li><li> Calcular Ᾱ 0, W como a média de Ᾱ 0, W1, Ᾱ 0, W2 e Ᾱ 0, W3, bem como Ᾱ 0, O como a média de Ᾱ 0, O1, Ᾱ 0, O2 e Ᾱ 0, O3. Calcular logD usando a seguinte fórmula: logD = log [(Ᾱ <sub&gt; 0, S · 40 ug) / (Ᾱ 0, W · 33 ug)]. </li><li> Executar toda a experiência em triplicado e calcular a média de logD, juntamente com o seu desvio padrão. </li></ol>

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W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Journal of Chromatography Library. 22A, A137-A160 (1983).</li><li>Reichenbaecher, M., Popp, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Strukturanalytik organischer und anorganischer Verbindungen. , (2007).</li><li>Gross, J. H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Mass Spectrometry: A Textbook. , (2004).</li><li>Ma, T. S., Rittner, R. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Modern Organic Elemental Analysis. , (1979).</li><li>Mueller, D., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Simplified+NaCl+Based+68Ga+Concentration+and+Labeling+Procedure+for+Rapid+Synthesis+of+68Ga+Radiopharmaceuticals+in+High+Radiochemical+Purity.">Simplified NaCl Based 68Ga Concentration and Labeling Procedure for Rapid Synthesis of 68Ga Radiopharmaceuticals in High Radiochemical Purity.</a> Bioconjugate Chem. 23, 1712-1717 (2012).</li><li>Roberts, T. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Radio-column+chromatography.">Radio-column chromatography.</a> Journal of Chromatography Library. 14, 103-132 (1978).</li><li>Roberts, T. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Radio-thin-layer+chromatography.">Radio-thin-layer chromatography.</a> Journal of Chromatography Library. 14, 45-83 (1978).</li><li>Green, M. A., Welch, M. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Gallium+radiopharmaceutical+chemistry.">Gallium radiopharmaceutical chemistry.</a> Nucl. Med. Biol. 16, 435-448 (1989).</li><li>Notni, J., Plutnar, J., Wester, H. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Bone-seeking+TRAP+conjugates:+surprising+observations+and+their+implications+on+the+development+of+gallium-68-labeled+bisphosphonates.">Bone-seeking TRAP conjugates: surprising observations and their implications on the development of gallium-68-labeled bisphosphonates.</a> EJNMMI Res. 2, 13 (2012).</li><li>Schmitt-Willich, H., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+and+Physicochemical+Characterization+of+a+New+Gadolinium+Chelate:+The+Liver-Specific+Magnetic+Resonance+Imaging+Contrast+Agent+Gd-EOB-DTPA.">Synthesis and Physicochemical Characterization of a New Gadolinium Chelate: The Liver-Specific Magnetic Resonance Imaging Contrast Agent Gd-EOB-DTPA.</a> Inorg. Chem. 38, 1134-1144 (1999).</li><li>Zhernosekov, K., Nikula, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=68Ga+generator+for+positron+emission+tomography.">68Ga generator for positron emission tomography.</a> , (2012).</li><li>Simecek, J., Hermann, P., Wester, H. J., Notni, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=How+is+68Ga+Labeling+of+Macrocyclic+Chelators+Influenced+by+Metal+Ion+Contaminants+in+68Ge/68Ga+Generator+Eluates?.">How is 68Ga Labeling of Macrocyclic Chelators Influenced by Metal Ion Contaminants in 68Ge/68Ga Generator Eluates?.</a> ChemMedChem. 8, 95-103 (2013).</li><li>Baur, B., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis,+Radiolabelling+and+In+Vitro+Characterization+of+the+Gallium-68-,+Yttrium-90-+and+Lutetium-177-Labelled+PSMA+Ligand,+CHX-A''-DTPA-DUPA-Pep.">Synthesis, Radiolabelling and In Vitro Characterization of the Gallium-68-, Yttrium-90- and Lutetium-177-Labelled PSMA Ligand, CHX-A''-DTPA-DUPA-Pep.</a> Pharmaceuticals (Basel). 7, 517-529 (2014).</li><li>Boros, E., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=RGD+conjugates+of+the+H2dedpa+scaffold:+synthesis,+labeling+and+imaging+with+68Ga.">RGD conjugates of the H2dedpa scaffold: synthesis, labeling and imaging with 68Ga.</a> Nucl. Med. Biol. 39, 785-794 (2012).</li><li>Beck, W. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Hematology. , (1998).</li><li>Patel, V., Morrissey, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Practical and Professional Clinical Skills. , (2001).</li><li>Bartke, A., Constanti, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Basic Endocrinology. , (1998).</li><li>Bernstein, L. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Mechanisms+of+Therapeutic+Activity+for+Gallium.">Mechanisms of Therapeutic Activity for Gallium.</a> Pharmacol. 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The authors have nothing to disclose.

EOB-DTPA é acessível através de uma síntese de múltiplos passos 33, mas pode muito bem ser isolado a partir de agentes de contraste que contêm ácido disponíveis gadoxético. Para este propósito, o ião central, Gd (III) pode ser precipitado com um excesso de ácido oxálico. Depois de remover o oxalato Gd (III) e ácido oxálico o ligando pode ser isolado por precipitação em água fria a um pH de 1,5. No entanto, a fim de aumentar os rendimentos de cromatografia em coluna do filtrado pode ser reali...

Ácido gadoxético, um nome comum para o complexo de Gd (III) do ligando EOB-DTPA 1, é um agente de contraste utilizado em imagiologia hepatobiliar frequência de ressonância magnética (MRI). 2,3 Devido à sua absorção específica do fígado por hepatócitos e elevada percentagem de excreção hepatobiliar que permite a localização das lesões focais e tumores hepáticos. 2-5 no entanto, certas limitações da técnica de ressonância magnética (por exemplo, a toxicidade dos agentes de contraste, aplicabilidade limitada em pacientes com implantes claustrophobia ou de metal) para chamar uma ferramenta de diagnóstico alternativa . A tomografia de emissão de positrões (PET) é um método de imagiologia molecular, em que uma pequena quantidade de uma substância radioactiva (traçador) é administrado, em que a sua distribuição no corpo é registado por um aparelho de PET. 6 O PET é um método dinâmico que permite alta a resolução espacial e temporal das imagens, bem como a quantificação dos resultados, sem ter delidar com os efeitos colaterais dos agentes de contraste de MRI. O valor informativo das informações metabólica obtida pode ser ainda aumentada pela combinação com dados anatômicos recebidos dos métodos de imagem adicionais, como mais comumente atingida por imagem híbrido com tomografia computadorizada (TC) em scanners de PET / CT. A estrutura química de um marcador adequado para o PET deve incluir um isótopo radioactivo serve como emissor de positrões. Pósitrons têm um curto período de vida, uma vez que aniquilar quase imediatamente com os elétrons das conchas átomo de tecido circundante. Por aniquilação dois fotões gama 511 keV com direcção oposta de movimento são emitidos, que são registados pelo aparelho de PET 7,8. Para formar um traçador, nuclidos animal de estimação pode ser ligado covalentemente a uma molécula, como é o caso em 2-desoxi- 2- [18F] fluoroglucose (FDG), o marcador PET mais amplamente utilizado. 7 no entanto, um nuclídeo também podem formar ligações coordenativas a um ou vários ligantes (por exemplo,, [68 Ga] -DOTATOC 9,10) ou ser aplicado na forma de sais inorgânicos dissolvidos (por exemplo, [18F] fluoreto de sódio 11). No seu conjunto, a estrutura do marcador é crucial, uma vez que determina o seu comportamento biodistribuição, metabolismo e excreção. Um nuclido PET adequado deve combinar as características favoráveis ​​de energia de positrões como conveniente e disponibilidade, bem como uma meia-vida adequadas para a investigação pretendida. O 68Ga nuclídeo tornou-se uma força essencial no domínio do PET ao longo das últimas duas décadas. 12,13 Isto é principalmente devido à sua disponibilidade através de um sistema de gerador, que permite rotulagem no local, independentemente, a partir da vizinhança de um ciclotrão. Em um gerador, o nuclido mãe 68 Ge é absorvido numa coluna de onde o nuclídeo filha 68Ga é eluída e, subsequentemente, rotulados com um agente quelante adequado. 6,14 Uma vez que o 68Ga nuclídeo existe como um TrivalPendientesent catião tal como Gd (III) 10,13, quelantes EOB-DTPA com 68Ga vez iria produzir um complexo com a mesma carga global negativa como ácido gadoxético. Assim, que 68 Ga traçador pode combinar uma especificidade hepática característica semelhante com a aptidão para a imagem PET. Embora o ácido gadoxético é comprado e administrado como sal de sódio, no seguinte contexto vamos nos referir a ele como Gd [EOB-DTPA] e para o complexo não-radioativo Ga (III) como Ga [EOB-DTPA], ou 68 Ga [ EOB-DTPA] no caso de o componente marcado radioactivamente por uma questão de conveniência. Para avaliar a sua aplicabilidade como marcadores para PET, complexos de metais radioactivos têm de ser examinadas extensivamente in vitro, in vivo ou ex experiências in vivo em primeiro lugar. Para determinar a aptidão para o respectivo problema médico, várias características tracer como comportamento biodistribuição e perfil de apuramento, a estabilidade, a especificidade do órgão e célula ou tissue captação precisam ser investigadas. Devido ao seu caráter não-invasivo, in vitro determinações são muitas vezes realizados antes de experimentos in vivo. É geralmente reconhecido que o DTPA e os seus derivados são de aptidão limitada como quelantes para 68Ga, devido a estes complexos de falta inércia cinética, resultando em decomposição comparativamente rápido, quando administrado in vivo. 14-20 Isto é causado principalmente pela apo- transferrina actua como um concorrente por 68 Ga no plasma. No entanto, nós investigamos este novo marcador relativa à sua eventual aplicação em imagiologia hepatobiliar, em que as informações de diagnóstico podem ser fornecidas dentro de minutos após a injecção 3,4,21-23, assim, que não implica necessariamente a estabilidade traçador de longo prazo. Para este efeito foram isoladas EOB-DTPA a partir de ácido gadoxético e inicialmente realizado a complexação com Ga naturais (III), que existe como uma mistura de dois isótopos estáveis, 69 Ga e 71 </sup&gt; Ga. O complexo assim obtido serviu como padrão não radioactivo para o seguinte quelação de 68 Ga. Usamos métodos estabelecidos e, simultaneamente, avaliada sua adequação para determinar a eficiência 68 Galabeling de EOB-DTPA e investigar a lipofilicidade do novo 68 Ga traçador e sua estabilidade em diferentes mídias.

<table border="0" cellpadding="0" cellspacing="0" width="682">
	<colgroup>
		<col />
		<col />
		<col />
		<col />
	</colgroup>
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">primovist</td>
			<td style="width:180px;">Bayer</td>
			<td style="width:119px;">-</td>
			<td style="width:167px;">0.25 M</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">gallium(III) chloride</td>
			<td style="width:180px;">Sigma-Aldrich Co.</td>
			<td style="width:119px;">450898</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">water (deionized)</td>
			<td style="width:180px;">-</td>
			<td style="width:119px;">-</td>
			<td>&#160;tap water deionizing equipment by Auma-Tec GmbH</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">hydrochloric acid 12 M</td>
			<td style="width:180px;">VWR</td>
			<td style="width:119px;">20252.29</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">sodium hydroxide</td>
			<td style="width:180px;">Polskie Odczynniki Chemiczne S.A.</td>
			<td style="width:119px;">810925429</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">oxalic acid</td>
			<td style="width:180px;">Sigma-Aldrich Co.</td>
			<td style="width:119px;">75688</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">ethyl acetate</td>
			<td style="width:180px;">Brenntag GmbH</td>
			<td style="width:119px;">10010447</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">silica gel</td>
			<td style="width:180px;">Merck KGaA</td>
			<td style="width:119px;">1.10832.9025</td>
			<td>Geduran Si 60 0,063-0,2 mm</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">TLC silica gel 60 F254</td>
			<td style="width:180px;">Merck KGaA</td>
			<td style="width:119px;">1.16834.0001</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">methanol</td>
			<td style="width:180px;">VWR</td>
			<td style="width:119px;">20903.55</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">ethanol</td>
			<td style="width:180px;">Brenntag GmbH</td>
			<td style="width:119px;">10018366</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">eiethylether</td>
			<td style="width:180px;">VWR</td>
			<td style="width:119px;">23807.468</td>
			<td>stored over KOH plates</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">ammonia solution (25 %)</td>
			<td style="width:180px;">VWR</td>
			<td style="width:119px;">1133.1</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">pH electrode</td>
			<td style="width:180px;">VWR</td>
			<td style="width:119px;">662-1657</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">stirring and heating unit</td>
			<td style="width:180px;">Heidolph</td>
			<td style="width:119px;">505-20000-00</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">pump</td>
			<td style="width:180px;">Ilmvac GmbH</td>
			<td style="width:119px;">322002</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">frit</td>
			<td style="width:180px;">-</td>
			<td style="width:119px;">custom design</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">NMR spectrometer</td>
			<td style="width:180px;">Bruker Coorporation</td>
			<td style="width:119px;">-</td>
			<td>Ultra Shield 400</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">mass spectrometer</td>
			<td style="width:180px;">Thermo Fisher Scientific Inc.</td>
			<td style="width:119px;">-</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">elemental analyser</td>
			<td>Hekatech GmbH Analysentechnik</td>
			<td style="width:119px;">-</td>
			<td>EuroVector EA 3000 CHNS</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:216px;">deuterated water D2O</td>
			<td style="width:180px;">euriso-top</td>
			<td style="width:119px;">D214</td>
			<td>99,90 % D</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Name</td>
			<td style="width:180px;">Company</td>
			<td style="width:119px;">Catalog Number</td>
			<td>Comments</td>
		</tr>
		<tr height="21">
			<td colspan="4" height="21" style="height:21px;width:681px;">Material/Equipment required for labeling procedures</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">68Ge/68Ga generator</td>
			<td style="width:180px;">ITG Isotope Technologies Garching GmbH</td>
			<td style="width:119px;">A150</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">pump and dispenser system</td>
			<td style="width:180px;">Scintomics GmbH</td>
			<td style="width:119px;">-</td>
			<td>Variosystem</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">hydrochloric acid 30 % (suprapur)</td>
			<td style="width:180px;">Merck KGaA</td>
			<td style="width:119px;">1.00318.1000</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">water (ultrapur)</td>
			<td style="width:180px;">Merck KGaA</td>
			<td style="width:119px;">1.01262.1000</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">sodium chloride (suprapur)</td>
			<td style="width:180px;">Merck KGaA</td>
			<td style="width:119px;">1.06406.0500</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">sodium acetate (suprapur)</td>
			<td style="width:180px;">Merck KGaA</td>
			<td style="width:119px;">1.06264.0050</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">glacial acetic acid (suprapur)</td>
			<td style="width:180px;">Merck KGaA</td>
			<td style="width:119px;">1.00066.0250</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">sodium citrate dihydrate</td>
			<td style="width:180px;">VEB Laborchemie Apolda</td>
			<td style="width:119px;">10782</td>
			<td>&#62;98.5%</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">PS-H+ Cartridge (S)</td>
			<td style="width:180px;">Macherey-Nagel</td>
			<td style="width:119px;">731867</td>
			<td>Chromafix</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">apo-Transferrin</td>
			<td style="width:180px;">Sigma-Aldrich Co.</td>
			<td style="width:119px;">T2036</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">PBS&#160; buffer (tablets)</td>
			<td style="width:180px;">Sigma-Aldrich Co.</td>
			<td style="width:119px;">79382</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">human serum</td>
			<td style="width:180px;">Sigma-Aldrich Co.</td>
			<td style="width:119px;">H4522</td>
			<td>from human male AB plasma</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">flasks, columns etc.</td>
			<td style="width:180px;"></td>
			<td style="width:119px;">custom design</td>
			<td></td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;width:216px;">pH electrode</td>
			<td style="width:180px;">Knick Elektronische Messger&#228;te GmbH &#38; Co. KG</td>
			<td style="width:119px;">765-Set</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">binary pump (HPLC)</td>
			<td style="width:180px;">Hewlett-Packard</td>
			<td style="width:119px;">G1312A (HP 1100)</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">UV Vis detector (HPLC)</td>
			<td style="width:180px;">Hewlett-Packard</td>
			<td style="width:119px;">G1315A (HP 1100)</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">radioactive detector (HPLC)</td>
			<td style="width:180px;">EGRC Berthold</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;width:216px;">HPLC C-18-PFP column</td>
			<td style="width:180px;">Advanced Chromatography Technologies Ltd.</td>
			<td style="width:119px;">ACE-1110-1503/A100528</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">HPLC glass vials</td>
			<td style="width:180px;">GTG Glastechnik Graefenroda GmbH</td>
			<td style="width:119px;">8004-HP-H/i3&#181;</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">pipette</td>
			<td style="width:180px;">Eppendorf</td>
			<td style="width:119px;">-</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">plastic vials</td>
			<td style="width:180px;">Sarstedt AG &#38; Co.</td>
			<td style="width:119px;">6542.007</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">plastic vials</td>
			<td style="width:180px;">Greiner Bio-One International GmbH</td>
			<td style="width:119px;">717201</td>
			<td></td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;width:216px;">activimeter</td>
			<td style="width:180px;">MED Nuklear-Medizintechnik Dresden GmbH</td>
			<td style="width:119px;">-</td>
			<td>Isomed 2010</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">tweezers</td>
			<td style="width:180px;"></td>
			<td style="width:119px;">custom design</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">incubator</td>
			<td style="width:180px;">Heraeus Instruments GmbH</td>
			<td style="width:119px;">51008815</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">vortex mixer</td>
			<td style="width:180px;">Fisons</td>
			<td style="width:119px;">-</td>
			<td>Whirlimixer</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">centrifuge</td>
			<td style="width:180px;">Heraeus Instruments GmbH</td>
			<td style="width:119px;">75003360</td>
			<td></td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;width:216px;">gamma well counter</td>
			<td style="width:180px;">MED Nuklear-Medizintechnik Dresden GmbH</td>
			<td style="width:119px;">-</td>
			<td>Isomed 2100</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">water for chromatography</td>
			<td style="width:180px;">Merck KGaA</td>
			<td style="width:119px;">1.15333.2500</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">acetonitrile for chromatography</td>
			<td style="width:180px;">Merck KGaA</td>
			<td style="width:119px;">1.00030.2500</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">trifluoroacetic acid</td>
			<td style="width:180px;">Sigma-Aldrich</td>
			<td style="width:119px;">91707</td>
			<td></td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;width:216px;">TLC radioactivity scanner</td>
			<td style="width:180px;">raytest Isotopenmessger&#228;te GmbH</td>
			<td style="width:119px;">B00003875</td>
			<td>equipped with beta plastic detector</td>
		</tr>
	</tbody>
</table>

investigations on the ga(iii) complex of eob-dtpa and its 68ga radiolabeled analogue

Nós demonstramos um método para o isolamento de EOB-DTPA (3,6,9-triaza-f 3,6,9-tris (carboximetil) -4- (etoxibenzil) ácido -undecanedioic) a partir da sua Gd (III) e os protocolos para a preparação do seu novo não-radioactivos, isto é, singular Ga (III), bem como radioactivos 68Ga complexo. O ligando, bem como o Ga (III) foram caracterizados por espectroscopia de ressonância magnética nuclear (RMN), espectrometria de massa e análise elementar. 68Ga foi obtido por um método de eluição a partir de um padrão / 68Ga gerador 68 Ge. Experimentos para avaliar a eficiência de 68 Ga-rotulagem de EOB-DTPA em pH 3,8-4,0 foram realizadas. técnicas de análise de rádio estabelecida TLC (cromatografia de camada fina) e HPLC de rádio (cromatografia líquida de alta eficiência) foram usadas para determinar a pureza radioquímica do traçador. Como uma primeira investigação de lipofilicidade dos 68 Ga traçadores o n- octanol / água DISTRIBUTION coeficiente de Ga 68 espécies presentes em uma solução de pH 7,4 foi determinada por um método de extracção. medições in vitro de estabilidade do marcador em vários meios a pH fisiológico foram realizadas, revelando diferentes taxas de decomposição.

O ligando EOB-DTPA e o Ga não radioactivo (III) foram analisados ​​por meio de 1 H e 13 C {1 H} espectroscopia de RMN, espectrometria de massa e análise elementar. Os resultados listados na Tabela 1 e ilustrados nas Figuras 1-6 verificar a pureza das substâncias. A eluição da Ga gerador de 68 Ge / 68 produziu soluções d...

Watch this Scientific Journal Video about Investigations on the GaIII Complex of EOB-DTPA and Its 68Ga Radiolabeled Analogue at JoVE.com

Investigations on the GaIII Complex of EOB-DTPA and Its 68Ga Radiolabeled Analogue

Um procedimento para o isolamento de EOB-DTPA e complexação subsequente com Ga naturais (III) e 68 Ga é aqui apresentado, bem como uma análise aprofundada de todos os compostos e investigações sobre a eficiência rotulagem, a estabilidade in vitro e o octanol / água coeficiente de distribuição do complexo marcado radioactivamente.

As investigações sobre o Complexo Ga (III) de EOB-DTPA e sua<sup&gt; 68</sup&gt; Ga Radiolabeled Analogue

We demonstrate a method for the isolation of EOB-DTPA (3,6,9-triaza-3,6,9-tris(carboxymethyl)-4-(ethoxybenzyl)-undecanedioic acid) from its Gd(III) ...

investigations-on-ga-iii-complex-eob-dtpa-its-68ga-radiolabeled

Research

JoVE Journal

Chemistry

Investigations on the Ga(III) Complex of EOB-DTPA and Its 68Ga Radiolabeled Analogue

9.9K visualizações.  University Hospital Jena.  Um procedimento para o isolamento de EOB-DTPA e complexação subsequente com Ga naturais (III) e 68 Ga é aqui apresentado, bem como uma análise aprofundada de todos os compostos e investigações sobre a eficiência rotulagem, a estabilidade in vitro e o octanol / água coeficiente de distribuição do complexo marcado radioactivamente. 

Vídeo: Investigations on the GaIII Complex of EOB-DTPA and Its 68Ga Radiolabeled Analogue

LabVIEW-operated Novel Nanoliter Osmometer for Ice Binding Protein Investigations

Ice-binding proteins (IBPs), including antifreeze proteins, ice structuring proteins, thermal hysteresis proteins, and ice recrystallization inhibition proteins, are found in cold-adapted organisms and protect them from freeze injuries by interacting with ice crystals. IBPs are found in a variety of organism, including fish1, plants2, 3, arthropods4, 5, fungi6, and bacteria7. IBPs adsorb to the surfaces of ice crystals and prevent water molecules from joining the ice lattice at the IBP adsorption location. Ice that grows on the crystal surface between the adsorbed IBPs develops a high curvature that lowers the temperature at which the ice crystals grow, a phenomenon referred to as the Gibbs-Thomson effect. This depression creates a gap (thermal hysteresis, TH) between the melting point and the nonequilibrium freezing point, within which ice growth is arrested8-10, see Figure 1. One of the main tools used in IBP research is the nanoliter osmometer, which facilitates measurements of the TH activities of IBP solutions. Nanoliter osmometers, such as the Clifton instrument (Clifton Technical Physics, Hartford, NY,) and Otago instrument (Otago Osmometers, Dunedin, New Zealand), were designed to measure the osmolarity of a solution by measuring the melting point depression of droplets with nanoliter volumes. These devices were used to measure the osmolarities of biological samples, such as tears11, and were found to be useful in IBP research. Manual control over these nanoliter osmometers limited the experimental possibilities. Temperature rate changes could not be controlled reliably, the temperature range of the Clifton instrument was limited to 4,000 mOsmol (about -7.5 &deg;C), and temperature recordings as a function of time were not an available option for these instruments.
We designed a custom-made computer-controlled nanoliter osmometer system using a LabVIEW platform (National Instruments). The cold stage, described previously9, 10, contains a metal block through which water circulates, thereby functioning as a heat sink, see Figure 2. Attached to this block are thermoelectric coolers that may be driven using a commercial temperature controller that can be controlled via LabVIEW modules, see Figure 3. Further details are provided below. The major advantage of this system is its sensitive temperature control, see Figure 4. Automated temperature control permits the coordination of a fixed temperature ramp with a video microscopy output containing additional experimental details.
To study the time dependence of the TH activity, we tested a 58 kDa hyperactive IBP from the Antarctic bacterium Marinomonas primoryensis (MpIBP)12. This protein was tagged with enhanced green fluorescence proteins (eGFP) in a construct developed by Peter Davies' group (Queens University)10. We showed that the temperature change profile affected the TH activity. Excellent control over the temperature profile in these experiments significantly improved the TH measurements. The nanoliter osmometer additionally allowed us to test the recrystallization inhibition of IBPs5, 13. In general, recrystallization is a phenomenon in which large crystals grow larger at the expense of small crystals. IBPs efficiently inhibit recrystallization, even at low concentrations14, 15. We used our LabVIEW-controlled osmometer to quantitatively follow the recrystallization of ice and to enforce a constant ice fraction using simultaneous real-time video analysis of the images and temperature feedback from the sample chamber13. The real-time calculations offer additional control options during an experimental procedure. A stage for an inverted microscope was developed to accommodate temperature-controlled microfluidic devices, which will be described elsewhere16.
The Cold Stage System
The cold stage assembly (Figure 2) consists of a set of thermoelectric coolers that cool a copper plate. Heat is removed from the stage by flowing cold water through a closed compartment under the thermoelectric coolers. A 4 mm diameter hole in the middle of the copper plate serves as a viewing window. A 1 mm diameter in-plane hole was drilled to fit the thermistor. A custom-made copper disc (7 mm in diameter) with several holes (500 &mu;m in diameter) was placed on the copper plate and aligned with the viewing window. Air was pumped at a flow rate of 35 ml/sec and dried using Drierite (W.A. Hammond). The dry air was used to ensure a dry environment at the cooling stage. The stage was connected via a 9 pin connection outlet to a temperature controller (Model 3040 or 3150, Newport Corporation, Irvine, California, US). The temperature controller was connected via a cable to a computer GPIB-PCI card (National instruments, Austin, Texas, USA).

Ice binding proteins (IBPs), also known as antifreeze proteins, inhibit ice growth and are a promising additive for use in the cryopreservation of tissues. The main tool used to investigate IBPs is the nanoliter osmometer. We developed a home-designed cooling stage mounted on an optical microscope and controlled using a custom-built LabVIEW routine. The nanoliter osmometer described here manipulated the sample temperature in an ultra-sensitive manner.

LabVIEW operado Osmometer nanolitro Novel de Investigações de gelo ligação às proteínas

Ice-binding proteins (IBPs), including antifreeze proteins, ice structuring proteins, thermal hysteresis proteins, and ice recrystallization inhibition ...

Química

Reductive Electropolymerization of a Vinyl-containing Poly-pyridyl Complex on Glassy Carbon and Fluorine-doped Tin Oxide Electrodes

Controllable electrode surface modification is important in a number of fields, especially those with solar fuels applications. Electropolymerization is one surface modification technique that electrodeposits a polymeric film at the surface of an electrode by utilizing an applied potential to initiate the polymerization of substrates in the Helmholtz layer. This useful technique was first established by a Murray-Meyer collaboration at the University of North Carolina at Chapel Hill in the early 1980s and utilized to study numerous physical phenomena of films containing inorganic complexes as the monomeric substrate. Here, we highlight a procedure for coating electrodes with an inorganic complex by performing reductive electropolymerization of the vinyl-containing poly-pyridyl complex onto glassy carbon and fluorine doped tin oxide coated electrodes. Recommendations on electrochemical cell configurations and troubleshooting procedures are included. Although not explicitly described here, oxidative electropolymerization of pyrrole-containing compounds follows similar procedures to vinyl-based reductive electropolymerization but are far less sensitive to oxygen and water.

A procedure for performing reductive electropolymerization of vinyl-containing compounds onto glassy carbon and fluorine doped tin-oxide coated electrodes is presented. Recommendations on electrochemical cell configurations and troubleshooting procedures are included. Although not explicitly described here, oxidative electropolymerization of pyrrole-containing compounds follows similar procedures to vinyl-based reductive electropolymerization.

Electropolimerização redutiva de um complexo poli-piridil-vinil no Glassy contendo carbono e flúor-dopado com óxido de estanho Eléctrodos

Controllable electrode surface modification is important in a number of fields, especially those with solar fuels applications. Electropolymerization is ...

Photochemical Oxidative Growth of Iridium Oxide Nanoparticles on CdSe@CdS Nanorods

We demonstrate a procedure for the photochemical oxidative growth of iridium oxide catalysts on the surface of seeded cadmium selenide-cadmium sulfide (CdSe@CdS) nanorod photocatalysts. Seeded rods are grown using a colloidal hot-injection method and then moved to an aqueous medium by ligand exchange. CdSe@CdS nanorods, an iridium precursor and other salts are mixed and illuminated. The deposition process is initiated by absorption of photons by the semiconductor particle, which results with formation of charge carriers that are used to promote redox reactions. To insure photochemical oxidative growth we used an electron scavenger. The photogenerated holes oxidize the iridium precursor, apparently in a mediated oxidative pathway. This results in the growth of high quality crystalline iridium oxide particles, ranging from 0.5 nm to about 3 nm, along the surface of the rod. Iridium oxide grown on CdSe@CdS heterostructures was studied by a variety of characterization methods, in order to evaluate its characteristics and quality. We explored means for control over particle size, crystallinity, deposition location on the CdS rod, and composition. Illumination time and excitation wavelength were found to be key parameters for such control. The influence of different growth conditions and the characterization of these heterostructures are described alongside a detailed description of their synthesis. Of significance is the fact that the addition of iridium oxide afforded the rods astounding photochemical stability under prolonged illumination in pure water (alleviating the requirement for hole scavengers).

A protocol for the photochemical oxidative growth of small crystalline iridium oxide nanoparticles on the surface of CdSe@CdS seeded rod nanoparticles is presented.

Fotoquímica Crescimento oxidativo da Iridium nanopartículas de óxido de CdSe @ CdS nanobastões

We demonstrate a procedure for the photochemical oxidative growth of iridium oxide catalysts on the surface of seeded cadmium selenide-cadmium sulfide ...

Synthesis and Characterization of Supramolecular Colloids

Control over colloidal assembly is of utmost importance for the development of functional colloidal materials with tailored structural and mechanical properties for applications in photonics, drug delivery and coating technology. Here we present a new family of colloidal building blocks, coined supramolecular colloids, whose self-assembly is controlled through surface-functionalization with a benzene-1,3,5-tricarboxamide (BTA) derived supramolecular moiety. Such BTAs interact via directional, strong, yet reversible hydrogen-bonds with other identical BTAs. Herein, a protocol is presented that describes how to couple these BTAs to colloids and how to quantify the number of coupling sites, which determines the multivalency of the supramolecular colloids. Light scattering measurements show that the refractive index of the colloids is almost matched with that of the solvent, which strongly reduces the van der Waals forces between the colloids. Before photo-activation, the colloids remain well dispersed, as the BTAs are equipped with a photo-labile group that blocks the formation of hydrogen-bonds. Controlled deprotection with UV-light activates the short-range hydrogen-bonds between the BTAs, which triggers the colloidal self-assembly. The evolution from the dispersed state to the clustered state is monitored by confocal microscopy. These results are further quantified by image analysis with simple routines using ImageJ and Matlab. This merger of supramolecular chemistry and colloidal science offers a direct route towards light- and thermo-responsive colloidal assembly encoded in the surface-grafted monolayer.

A protocol for the synthesis and characterization of colloids coated with supramolecular moieties is described. These supramolecular colloids undergo self-assembly upon the activation of the hydrogen-bonds between the surface-anchored molecules by UV-light.

Síntese e Caracterização de Supramoleculares Colloids

Control over colloidal assembly is of utmost importance for the development of functional colloidal materials with tailored structural and mechanical ...

On-line Analysis of Nitrogen Containing Compounds in Complex Hydrocarbon Matrixes

The shift to heavy crude oils and the use of alternative fossil resources such as shale oil are a challenge for the petrochemical industry. The composition of heavy crude oils and shale oils varies substantially depending on the origin of the mixture. In particular they contain an increased amount of nitrogen containing compounds compared to the conventionally used sweet crude oils. As nitrogen compounds have an influence on the operation of thermal processes occurring in coker units and steam crackers, and as some species are considered as environmentally hazardous, a detailed analysis of the reactions involving nitrogen containing compounds under pyrolysis conditions provides valuable information. Therefore a novel method has been developed and validated with a feedstock containing a high nitrogen content, i.e., a shale oil. First, the feed was characterized offline by comprehensive two-dimensional gas chromatography (GC &#215; GC) coupled with a nitrogen chemiluminescence detector (NCD). In a second step the on-line analysis method was developed and tested on a steam cracking pilot plant by feeding pyridine dissolved in heptane. The former being a representative compound for one of the most abundant classes of compounds present in shale oil. The composition of the reactor effluent was determined via an in-house developed automated sampling system followed by immediate injection of the sample on a GC &#215; GC coupled with a time-of-flight mass spectrometer (TOF-MS), flame ionization detector (FID) and NCD. A novel method for quantitative analysis of nitrogen containing compounds using NCD and 2-chloropyridine as an internal standard has been developed and demonstrated.

A method combining comprehensive two-dimensional gas chromatography with nitrogen chemiluminescence detection has been developed and applied to on-line analysis of nitrogen containing compounds in a complex hydrocarbon matrix.

Análise on-line de compostos contendo azoto em matrizes de hidrocarbonetos complexos

The shift to heavy crude oils and the use of alternative fossil resources such as shale oil are a challenge for the petrochemical industry. The ...

Preparation of Chitosan-based Injectable Hydrogels and Its Application in 3D Cell Culture

The protocol presents a facile, efficient, and versatile method to prepare chitosan-based hydrogels using dynamic imine chemistry. The hydrogel is prepared by mixing solutions of glycol chitosan with a synthesized benzaldehyde terminated polymer gelator, and hydrogels are efficiently obtained in several minutes at room temperature. By varying ratios between glycol chitosan, polymer gelator, and water contents, versatile hydrogels with different gelation times and stiffness are obtained. When damaged, the hydrogel can recover its appearances and modulus, due to the reversibility of the dynamic imine bonds as crosslinkages. This self-healable property enables the hydrogel to be injectable since it can be self-healed from squeezed pieces to an integral bulk hydrogel after the injection process. The hydrogel is also multi-responsive to many bio-active stimuli due to different equilibration statuses of the dynamic imine bonds. This hydrogel was confirmed as bio-compatible, and L929 mouse fibroblast cells were embedded following standard procedures and the cell proliferation was easily assessed by a 3D cell cultivation process. The hydrogel can offer an adjustable platform for different research where a physiological mimic of a 3D environment for cells is profited. Along with its multi-responsive, self-healable, and injectable properties, the hydrogels can potentially be applied as multiple carriers for drugs and cells in future bio-medical applications.

Here we describe a facile preparation of chitosan-based injectable hydrogels using dynamic imine chemistry. Methods to adjust the hydrogel&#8217;s mechanical strength and its application in 3D cell culture are presented.

Preparação do hidrogel injetável à base de quitosana e sua aplicação em cultura de células 3D

The protocol presents a facile, efficient, and versatile method to prepare chitosan-based hydrogels using dynamic imine chemistry. The hydrogel is ...

Molten-Salt Synthesis of Complex Metal Oxide Nanoparticles

The development of feasible synthesis methods is critical for the successful exploration of novel properties and potential applications of nanomaterials. Here, we introduce the molten-salt synthesis (MSS) method for making metal oxide nanomaterials. Advantages over other methods include its simplicity, greenness, reliability, scalability, and generalizability. Using pyrochlore lanthanum hafnium oxide (La2Hf2O7) as a representative, we describe the MSS protocol for the successful synthesis of complex metal oxide nanoparticles (NPs). Furthermore, this method has the unique ability to produce NPs with different material features by changing various synthesis parameters such as pH, temperature, duration, and post-annealing. By fine-tuning these parameters, we are able to synthesize highly uniform, non-agglomerated, and highly crystalline NPs. As a specific example, we vary the particle size of the La2Hf2O7&#160;NPs by changing the concentration of the ammonium hydroxide solution used in the MSS process, which allows us to further explore the effect of particle size on various properties. It is expected that the MSS method will become a more popular synthesis method for nanomaterials and more widely employed in the nanoscience and nanotechnology community in the upcoming years.

Here, we demonstrate a unique, relatively low-temperature, molten-salt synthesis method for preparing uniform complex metal oxide lanthanum hafnate nanoparticles.

Sal fundido síntese de nanopartículas de óxido metálico complexo

The development of feasible synthesis methods is critical for the successful exploration of novel properties and potential applications of nanomaterials. ...

Extraction of Lignin with High &#946;-O-4 Content by Mild Ethanol Extraction and Its Effect on the Depolymerization Yield

Lignin valorization strategies are a key factor for achieving more economically competitive biorefineries based on lignocellulosic biomass. Most of the emerging elegant procedures to obtain specific aromatic products rely on the lignin substrate having a high content of the readily cleavable &#946;-O-4 linkage as present in the native lignin structure. This provides a miss-match with typical technical lignins that are highly degraded and therefore are low in &#946;-O-4 linkages. Therefore, the extraction yields, and the quality of the obtained lignin are of utmost importance to access new lignin valorization pathways. In this manuscript, a simple protocol is presented to obtain lignins with high &#946;-O-4 content by relatively mild ethanol extraction that can be applied to different lignocellulose sources. Furthermore, analysis procedures to determine the quality of the lignins are presented together with a depolymerization protocol that yields specific phenolic 2-arylmethyl-1,3-dioxolanes, which can be used to evaluate the obtained lignins. The presented results demonstrate the link between lignin quality and potential for the lignins to be depolymerized into specific monomeric aromatic chemicals. Overall, the extraction and depolymerization demonstrates a trade-off between the lignin extraction yield and the retention of the native aryl-ether structure and thus the potential of the lignin to be used as the substrate for the production of chemicals for higher-value applications.

Here, we present a protocol to perform ethanol extraction of lignin from several biomass sources. The effect of the extraction conditions on the lignin yield and &#946;-O-4 content are presented. Selective depolymerization is performed on the obtained lignins to obtain high aromatic monomer products.

Extração da lignina com alto teor de β-O-4 por extração de etanol suave e seu efeito sobre o rendimento de despolimerização

Lignin valorization strategies are a key factor for achieving more economically competitive biorefineries based on lignocellulosic biomass. Most of the ...

Analysis of Complex Molecules and Their Reactions on Surfaces by Means of Cluster-Induced Desorption/Ionization Mass Spectrometry

Desorption/Ionization Induced by Neutral SO2 Clusters (DINeC) is employed as a very soft and efficient desorption/ionization technique for mass spectrometry (MS) of complex molecules and their reactions on surfaces. DINeC is based on a beam of SO2 clusters impacting on the sample surface at low cluster energy. During cluster-surface impact, some of the surface molecules are desorbed and ionized via dissolvation in the impacting cluster; as a result of this dissolvation-mediated desorption mechanism, low cluster energy is sufficient and the desorption process is extremely soft. Both surface adsorbates and molecules of which the surface is composed of can be analyzed. Clear and fragmentation-free spectra from complex molecules such as peptides and proteins are obtained. DINeC does not require any special sample preparation, in particular no matrix has to be applied. The method yields quantitative information on the composition of the samples; molecules at a surface coverage as low as 0.1 % of a monolayer can be detected. Surface reactions such as H/D exchange or thermal decomposition can be observed in real-time and the kinetics of the reactions can be deduced. Using a pulsed nozzle for cluster beam generation, DINeC can be efficiently combined with ion trap mass spectrometry. The matrix-free and soft nature of the DINeC process in combination with the MSn capabilities of the ion trap allows for very detailed and unambiguous analysis of the chemical composition of complex organic samples and organic adsorbates on surfaces.

Neutral SO2 clusters of low kinetic energy (&#60; 0.8 eV/constituent) are used to desorb complex surface molecules such as peptides or lipids for further analysis by means of mass spectrometry using an ion trap mass spectrometer. No special sample preparation is required, and real-time observation of reactions is possible.

Análise de Moléculas Complexas e Suas Reações em Superfícies por meio da espectrometria de desormetria/desonização induzida por cluster

Desorption/Ionization Induced by Neutral SO2 Clusters (DINeC) is employed as a very soft and efficient desorption/ionization technique for mass ...

Synthesis of Functionalized Magnetic Nanoparticles, Their Conjugation with the Siderophore Feroxamine and its Evaluation for Bacteria Detection

In the present work, the synthesis of magnetic nanoparticles, its coating with SiO2, followed by its amine functionalization with (3-aminopropyl)triethoxysilane (APTES) and its conjugation with deferoxamine, a siderophore recognized by Yersinia enterocolitica, using a succinyl moiety as a linker are described.
Magnetic nanoparticles (MNP) of magnetite (Fe3O4) were prepared by solvothermal method and coated with SiO2 (MNP@SiO2) using the St&#246;ber process followed by functionalization with APTES (MNP@SiO2@NH2). Then, feroxamine was conjugated with the MNP@SiO2@NH2 by carbodiimide coupling to give MNP@SiO2@NH2@Fa. The morphology and properties of the conjugate and intermediates were examined by eight different methods including powder X-Ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM) and energy dispersive X-Ray (EDX) mapping. This exhaustive characterization confirmed the formation of the conjugate. Finally, in order to evaluate the capacity and specificity of the nanoparticles, they were tested in a capture bacteria assay using Yersinia enterocolitica.

This work describes protocols for the preparation of magnetic nanoparticles, its coating with SiO2, followed by its amine functionalization with (3-aminopropyl)triethoxysilane (APTES) and its conjugation with deferoxamine using a succinyl moiety as a linker. A deep structural characterization description and a capture bacteria assay using Y. enterocolitica for all the intermediate nanoparticles and the final conjugate are also described in detail.

As investigações sobre o Complexo Ga (III) de EOB-DTPA e sua

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