COMPOSIÇÃO QUÍMICA E AVALIAÇÃO DA ATIVIDADE CARRAPATICIDA DO ÓLEO ESSENCIAL DE Cinnamomun zeylanicum NO CONTROLE DE Rhipicephalus microplus

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ILDENICE NOGUEIRA MONTEIRO

2013-01-01

Os constituintes do óleo de Cinnamomum zeylanicum foram identificados por cromatografia gasosa acoplada à espectrometria de massas (CG-EM). Também foi avaliada a atividade deste óleo essencial contra larvas e fêmeas de Rhipicephalus microplus (carrapato bovino). O óleo das folhas mostrou um rendimento de 1,03% e seus principais constituintes foram Benzoato de Benzila (65,39%), Linalol (5,37%), E-Cinamaldeido (3,97%), α-Pineno (3,95%), β-Felandreno (3,42%), Eugenol (3,36%) e Benzalde...

Produção de biodiesel por transesterificação enzimática in situ em solvente orgânico a partir da biomassa de Desmodesmus sp.

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Danielle Kochenborger John

2017-07-01

Full Text Available Um dos materiais alternativos mais investigados atualmente para a produção de biodiesel são as microalgas. O presente trabalho teve como objetivo a avaliação do método de transesterificação enzimática in situ da microalga Desmodesmus sp. em solvente orgânico, acompanhando a reação através do monitoramento on-line com sonda de infravermelho e cromatografia gasosa. Dois ensaios foram realizados em condições distintas para efeito comparativo. Baseado nos resultados obtidos por espectroscopia e cromatografia, bem como nas propriedades calculadas a partir do perfil cromatográfico, pode-se concluir que é possível a produção de biodiesel in situ a partir de biomassa de microalgas, reduzindo a etapa de extração de óleo.

Identificação e quantificação de voláteis de café através de cromatografia gasosa de alta resolução / espectrometria de massas empregando um amostrador automático de "headspace" Identification and quantification of coffee volatile components through high resolution gas chromatoghaph/mass spectrometer using a headspace automatic sampler

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Leonardo César AMSTALDEN

2001-01-01

Full Text Available Usando um amostrador automático, os "headspaces" de três marcas comerciais de café torrado e moído foram analisados qualitativa e quantitativamente quanto a composição dos voláteis responsáveis pelo aroma através da técnica de cromatografia gasosa/espectrometria de massas. Uma vez que a metodologia não envolveu isolamento ou concentração dos aromas, suas proporções naturais foram mantidas, além de simplificar o preparo das amostras. O emprego do amostrador automático permitiu também boa resolução dos picos cromatográficos sem o emprego de criogenia, contribuindo para redução no tempo de análise. Noventa e um componentes puderam ser identificados, sendo que alguns compostos conhecidos como presentes em café como o dimetilsulfeto, metional e furfuril mercaptana não foram detectados. Os voláteis presentes em maior concentração puderam ser quantificados com o auxílio de dois padrões internos. A técnica se provou viável, tanto para caracterização como para quantificação de voláteis de café.Employing an automatic headspace sampler, the headspaces of three commercial brands of ground roasted coffee were qualitatively and quantitatively analyzed by gas chromatography / mass spectrometry. Since the methodology did not involve aroma isolation or concentration, their natural proportions were maintained, providing a more accurate composition of the flavors, and simplifying sample preparation. The automatic sampler allowed good resolution of the chromatographic peaks without cryofocusing the samples at the head of the column during injection, reducing analysis time. Ninety one compounds were identified and some known coffee volatiles, such as dimethyl sulphide, methional and furfuryl mercaptan were not detected. The more concentrated volatiles could be identified using two internal standards. The technique proved viable, for both characterization and for quantification of coffee volatiles.

EVALUATION OF THE CONTAMINATION FROM GUANABARA BAY MANGROVES USING CRABS UCIDES CORDATUS AS INDICATORS OF OIL POLLUTANTS AND DEVELOPMENT OF ANALYSIS

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ADRIANA HADDAD NUDI

2005-01-01

O principal objetivo deste estudo foi validar o caranguejo da espécie Ucides cordatus como organismo indicador de poluição por óleo em áreas de manguezais da Baía de Guanabara. Para isto foram realizadas as seguintes etapas: (1) análises químicas de hidrocarbonetos policíclicos aromáticos (HPAs) em amostras de hepatopâncreas e sedimento por cromatografia gasosa acoplada ao espectrômetro de massas (CG/EM); (2) bioensaios com experimentos de exp...

Estudo da degradação do fármaco Nabumetona por fotólise direta Study of Nabumetone degradation through direct photolysis

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Florangela Maionchi

2002-03-01

Full Text Available O presente trabalho teve por objetivo estudar a degradação do fármaco Nabumetona por fotólise direta. Soluções etanólicas de amostras (20 mg/mL foram preparadas e divididas em cubetas de quartzo com tampas de teflon. Estas foram colocadas em uma câmara de fotólise à temperatura de 35ºC. As quantificações das fotodegradações foram analisadas por Cromatografia Líquida de Alta Eficiência (CLAE; após 47 dias de fotólise, a degradação da amostra foi de 67%, após 73 dias 88,5% e após 111 dias 89,5%. Determinações espectrofotométricas (240 a 360 nm foram realizadas após 28, 47 e 73 dias de fotólise. Os fotoprodutos foram separados por CLAE e analisados por Cromatografia Gasosa Acoplada ao Espectro de Massa de Baixa Resolução (CG-EM. A análise em CG-EM da Nabumetona fotolisada durante 111 dias permitiu a sugestão de duas substâncias.The present work aims to study the degradation of Nabumetone through direct photolysis. Solutions of Nabumetone in ethanol (20 mg/mL were prepared and divided in quartz cuvettes with teflon lids. These were placed in the photolysis cabinet at 35ºC. The photodegradation quantifications were analyzed in High Performance Liquid Cromatography (HPLC; after 47 days of photolysis the sample degradation was 67%, after 73 days 88.5% and after 111 days 89.5%. Spectrophotometers determinations (240 to 360 nm were accomplished after 28, 47 and 73 days of photolysis. The photoproducts were separate for HPLC and analyzed by Gas Cromatograph coupled to Mass Spectrometer (GC-MS. The analysis in GC-MS of the Nabumetona photolyseded for 111 days allowed the suggestion of two substances.

Antibacterial activity and chemical composition of essential oil of Lippia microphylla Cham =Atividade antibacteriana e composição química do óleo essencial de Lippia microphylla Cham

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Fabiola Fernandes Galvão Rodrigues

2011-04-01

Full Text Available The essential oil from the fresh leaves of Lippia microphylla Cham. was obtained by hydrodistillation and characterized by gas chromatography-mass spectrometry (GC-MS. Major constituents of the oil were 1.8-cineole (18.12%, ƒÒ-ocimene (15.20%, bicyclogermacrene (11.63% and caryophyllene oxide (8.32%. Antimicrobial activity of the oil against Gram-positive and Gram-negative bacteria was determined by gel diffusion method. The oil showed good antibacterial activity against Shigella flexneri, Escherichia coli and Streptococcus pyogenes and very good antibacterial activity against Staphylococcus aureus.O oleo essencial das folhas frescas de Lippia microphylla Cham. foi obtido por hidrodestilacao e caracterizado por cromatografia gasosa acoplada a espectrometria de massas (CG-EM. O constituinte majoritario do oleo foi 1.8-cineol (18,12%, ƒÒ-ocimeno (15,20%, bicyclogermacreno (11,63% e oxido de caryophylleno (8,32%. A atividade antimicrobiana do oleo frente as bacterias Gram-positivas e Gramnegativas foi determinada pelo metodo de difusao em gel. O oleo apresentou uma boa atividade antibacteriana frente a Shigella flexneri, Escherichia coli e Streptococcus pyogenes sendo o melhor resultado frente a Staphylococcus aureus.

COMPARAÇÃO DOS MÉTODOS OFICIAIS DE ANÁLISE E CROMATOGRÁFICOS PARA A DETERMINAÇÃO DOS TEORES DE ALDEÍDOS E ÁCIDOS EM BEBIDAS ALCOÓLICAS

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NASCIMENTO Ronaldo F.

1998-01-01

Full Text Available É apresentado um estudo comparativo entre os métodos oficiais e cromatográficos para a análise de aldeídos e de ácidos em bebidas alcoólicas. Foram analisadas trinta e cinco amostras de destilados alcoólicos. Com respeito a determinação dos teores totais de aldeídos e de ácidos. Os métodos oficiais e cromatográficos apresentam similar exatidão e reprodutibilidade. Entretanto, apenas os métodos cromatográficos permitem identificar e quantificar os componentes de cada série homologa. As metodologias propostas utilizando as técnicas de cromatografia gasosa e cromatografia líquida são simples, rápidas e apresentam maior sensibilidade que os métodos oficiais sendo aplicáveis também a amostras coloridas.

Embolia gasosa venosa inadvertida durante cesariana: bolsas retráteis ​​para líquidos intravenosos sem saídas autovedantes oferecem riscos. Relato de caso

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Mefkur Bakan

2013-08-01

Full Text Available O anestesiologista deve estar ciente das causas, do diagnóstico e do tratamento de embolia venosa e adotar padrões de prática para prevenir sua ocorrência. Embora a embolia gasosa seja uma complicação conhecida da cesariana, descrevemos um caso raro de desatenção que causou embolia gasosa iatrogênica quase fatal durante uma cesariana sob raquianestesia. uma das razões para o uso de bolsas autorretráteis para infusão em vez dos frascos convencionais de vidro ou plástico é a precaução contra embolia gasosa. Também demonstramos o risco de embolia venosa com o uso de dois tipos de bolsas plásticas retráteis (à base de cloreto de polivinil [PVC] e de polipropileno para líquidos intravenosos. As bolsas para líquidos sem saídas autovedantes apresentam risco de embolia gasosa se o sistema de fechamento estiver quebrado, enquanto a flexibilidade da bolsa limita a quantidade de entrada de ar. bolsas à base de pvc, que têm mais flexibilidade, apresentam risco significativamente menor de entrada de ar quando o equipo de administração intravenosa (IV é desconectado da saída. usar uma bolsa pressurizada para infusão rápida sem verificar e esvaziar todo o ar da bolsa IV pode ser perigoso.

Crescimento e trocas gasosas de genótipos de feijão-caupi sob estratégias de cultivo

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Aldemir da Silva

2016-06-01

Full Text Available O feijão-caupi tem grande importância econômica, alimentar e social. No Nordeste brasileiro, notadamente nas regiões semiáridas, sua produção é limitada pelo déficit hídrico, sendo necessário identificar genótipos tolerantes atrelados ao uso de tecnologias em seu cultivo. Com isto, objetivou-se avaliar o rendimento de fitomassa e as trocas gasosas de genótipos de feijão-caupi cultivados em diferentes técnicas de conservação de água. O experimento foi realizado em campo, no município de Pombal, na Paraíba, estudando-se quatro técnicas de retenção de água in situ (camalhão, sulco, bacia e sistema convencional e seis genótipos de feijão-caupi (1. Costela de Vaca, 2. BRS Itaim, 3. BRS Guariba, 4. BR-17 Gurguéia, 5. BRS Potengi e 6. BRS Aracé semeados no espaçamento de 0,5 m x 0,5 m, usando o delineamento experimental de blocos ao acaso, com quatro repetições. Os dados das estimativas do rendimento de fitomassa seca e das trocas gasosas das plantas foram submetidos à análise de variância, ao teste F, seguido de testes de comparação de médias, teste de Tukey. O cultivo em sulcos e em camalhão deram melhor resultados do que o sistema convencional de plantio e em bacia. As variedades BRS - Potengi, BRS - Aracé e BRS - Guariba tiveram melhor crescimento e trocas gasosas das plantas.

Estudo comparativo dos óleos voláteis de algumas espécies de Piperaceae

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J.M.O. Mesquita

Full Text Available O presente trabalho teve por objetivo a análise comparativa dos óleos voláteis de espécies da família Piperaceae. As espécies estudadas foram as seguintes: Piper aduncum, P. amalago, P. arboreum, P. cernuum, P. hispidum, P. regnelii, P. submarginalum, P. vicosanum e Pothomorphe umbellata. A análise dos óleos voláteis foi efetuada pela combinação de técnicas de Cromatografia de Fase Gasosa (CG e de Cromatografia de Fase Gasosa acoplada a Espectrometria de Massa (CG/EM. A porcentagem de identificação dos constituintes nas análises dos óleos voláteis de Piper aduncum, P. amalago, P. vicosanum, P. submarginalum e Pothomorphe umbellata, atingiu valores superiores a 80%. Houve predominância de compostos de natureza sesquiterpênica nas composições químicas das espécies analisadas, com exceção de P. hispidum, P. submarginalum e P. vicosanum onde a predominância na composição foi de monoterpenos. Pelos dados apresentados observou-se que, dentre os compostos majoritários, os mais freqüentes, nas 9 espécies estudadas, foram beta-pineno (9/9 e espatulenol (9/9, seguidos por E-cariofileno (8/9, óxido de cariofileno (8/9, germacreno D (7/9, alfa-pineno (7/9 e limoneno (6/9. Pela primeira vez se relata a composição dos óleos voláteis de P. submarginalum e P vicosanum.

Perfil lipídico tecidual de ratos alimentados com diferentes fontes lipídicas

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Almeida,Martha Elisa Ferreira de; Queiroz,José Humberto de; Queiroz,Maria Eliana Lopes Ribeiro de; Costa,Neuza Maria Brunoro; Matta,Sérgio Luis Pinto

2009-01-01

OBJETIVO:Determinar se fontes lipídicas com diferentes razões de ácidos graxos insaturados e saturados (PUFA+MUFA)/SFA na dieta altera o perfil lipídico tecidual, a concentração de lipídios (mg/g) dos tecidos hepáticos e mesentérico e a digestibilidade lipídica. MÉTODOS: Foi realizada cromatografia gasosa para determinar o perfil de ácidos graxos nos tecidos hepático e adiposo de ratos alimentados com diferentes fontes lipídicas. O coeficiente de digestibilidade foi determinado a partir da re...

Lipid profile of dehydrated eggs with emphasis on the contents of trans fatty acids

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Guassi, Silce Adeline Danelon; Salgado, Jocelem Mastrodi; Lanna, Dante Pazzanese Duarte

2008-01-01

O presente trabalho objetivou a determinação do perfil lipídico de ovos integrais desidratados, bem como de gemas desidratadas, a fim de enfatizar seu conteúdo de ácidos graxos de configuração trans. A fração lipídica das amostras foi extraída com hexano/isopropanol e, a seguir, metilada. Os ácidos graxos foram identificados via cromatografia gasosa. Constatou-se que a natureza lipídica dos ovos tem caráter predominantemente insaturado: 63,65% dos lipídios totais nos ovos integrais e 62,63% n...

Perfil lipídico de ovos desidratados com ênfase no seu teor de gorduras trans

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Guassi,Silce Adeline Danelon; Salgado,Jocelem Mastrodi; Lanna,Dante Pazzanese Duarte

2008-01-01

O presente trabalho objetivou a determinação do perfil lipídico de ovos integrais desidratados, bem como de gemas desidratadas, a fim de enfatizar seu conteúdo de ácidos graxos de configuração trans. A fração lipídica das amostras foi extraída com hexano/isopropanol e, a seguir, metilada. Os ácidos graxos foram identificados via cromatografia gasosa. Constatou-se que a natureza lipídica dos ovos tem caráter predominantemente insaturado: 63,65% dos lipídios totais nos ovos integrais e 62,63% n...

Conversion of hydroxycinnamic acids into volatile phenols in a synthetic medium and in red wine by Dekkera bruxellensis Transformação de ácidos hidroxicinâmicos em fenóis voláteis em meio sintético e em vinho tinto por Dekkera bruxellensis

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Maria João Cabrita

2012-03-01

Full Text Available The conversion of p-coumaric acid, ferulic acid, and caffeic acid into 4-ethylphenol, 4-ethylguaiacol and 4-ethylcatechol was studied in Dekkera bruxellensis ISA 1791 under defined conditions in a synthetic medium and in a red wine. Liquid chromatography (HPLC-DAD was used to quantify the phenolic acids, and gas chromatography (GC coupled to a FID detector was used to quantify volatile phenols using a novel analytical methodology that does not require sample derivatization. Identification was achieved by gas chromatography-mass detection (GC-MS. The results show that phenolic acids concentration decreases while volatile phenols concentration increases. The proportion of caffeic acid taken up by Dekkera bruxellensis is lower than that for p-coumaric or ferulic acid; therefore less 4-ethylcatechol is formed. More important, 4-ethylcathecol synthesis by Dekkera bruxellensis in wine has never been demonstrated so far. These results contribute decisively to a better understanding of the origin of the volatile phenols in wines. The accumulation of these compounds in wine is nowadays regarded as one of the key factors of quality control.A transformação do ácido p-cumárico, ácido ferúlico e ácido cafeico em 4-etilfenol, 4-etilguaiacol e 4-etilcatecol foi estudada na presença de Dekkera bruxelensis ISA 1791, sob condições controladas, em meio sintético e em vinho tinto. Os compostos fenólicos foram doseados por cromatografia em fase líquida (HPLC-DAD e os fenóis voláteis foram doseados por cromatografia em fase gasosa (GC com detector de ionização de chama (FID, recorrendo a uma metodologia que não requer prévia derivatização da amostra. A identificação dos compostos foi comprovada por espectrometria de massa (GC-MS. Os resultados demonstram que os teores em ácidos fenólicos diminuem enquanto se observa um aumento dos teores em fenóis voláteis. O ácido cafeico é dos três ácidos em estudo, o menos utilizado pela levedura, da

Quality of cocaine seized in 1997 in the street-drug market of São Paulo city, Brazil Qualidade da cocaína traficada em 1997 na cidade de São Paulo, Brasil

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Débora Gonçalves de Carvalho

2003-03-01

carbonates and bicarbonates (19.2%; silicates (13.8%, sugars (9.59%; starch (5.6%, borate (3.8% and sulphates(2.8%. Contaminants (secondary products originated from coca paste refining or decomposition processes were not analysed.Teores de cocaína e adulterantes bem como vários diluentes foram determinados em 389 amostras de pó branco apreendidas na cidade de São Paulo, no ano de 1997. Cocaína e seus adulterantes foram analisados por cromatografia em camada delgada, cromatografia em fase gasosa (detetor de ionização de chama e cromatografia em fase gasosa acoplado a espectrometria de massa (CG/MS. Diluentes foram analisados através de "spot tests" e da cromatografia em camada delgada. Foram obtidos os seguintes resultados: em 4,4% das amostras não foram detectados cocaína e adulterantes; de todas as amostras positivas para cocaína, 14% não continham mais que 200 mg/g de pó; em 70% a pureza da cocaína variou de 201 a 550 mg/g e em 16% não foi maior que 700 mg/g. Os anestésicos locais lidocaína e procaína foram detectados em 19 amostras em concentrações que variaram de 10 a 602 mg/g de pó. Cafeína foi encontrada em duas amostras. Os principais diluentes detectados foram: carbonatos e bicarbonatos, silicatos, açúcares, amido, borato e sulfatos. Contaminantes (produtos secundários originários do refino da pasta de coca ou de processos de decomposição não foram analisados.

Gc protein (vitamin D-binding protein): Gc genotyping and GcMAF precursor activity.

Science.gov (United States)

Nagasawa, Hideko; Uto, Yoshihiro; Sasaki, Hideyuki; Okamura, Natsuko; Murakami, Aya; Kubo, Shinichi; Kirk, Kenneth L; Hori, Hitoshi

2005-01-01

The Gc protein (human group-specific component (Gc), a vitamin D-binding protein or Gc globulin), has important physiological functions that include involvement in vitamin D transport and storage, scavenging of extracellular G-actin, enhancement of the chemotactic activity of C5a for neutrophils in inflammation and macrophage activation (mediated by a GalNAc-modified Gc protein (GcMAF)). In this review, the structure and function of the Gc protein is focused on especially with regard to Gc genotyping and GcMAF precursor activity. A discussion of the research strategy "GcMAF as a target for drug discovery" is included, based on our own research.

Fatty acids trans profile of oil and hidrogenated soy fat in frying process

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Sanibal, Elaine Abrão Assef; Mancini Filho, Jorge

2004-01-01

O objetivo desse estudo foi avaliar as alterações dos ácidos graxos e a formação de isômeros trans, durante o aquecimento de óleo de soja (OS) e gordura parcialmente hidrogenada de soja (GPHS) no processo de fritura de batata por 100 horas com reposição lipídica. O perfil de ácidos graxos foi avaliado através de cromatografia gasosa em coluna capilar de 100m. Os ácidos graxos monoinsaturados trans foram os predominantes entre os isômeros trans. A partir de 10 horas de fritura, o OS formou 2,1...

Aspectos analíticos do controle da dopagem de agentes anabolizantes em urina de atletas: avaliação de critérios de positividade Positiviness criteria for analysis of anabolic steroids by GC/MS in the urine of athletes

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Eliane Granuzzio Castilho

2003-03-01

Full Text Available O abuso dos esteróides anabólicos androgênicos (EAA está em constante ascensão, tanto nos esportes profissionais como nos esportes praticados nas academias. Essas substâncias são banidas pelo Comitê Olímpico Internacional (COI, sendo que este comitê recomenda que a metodologia usada na detecção e quantificação desses compostos em amostras biológicas dos atletas seja a cromatografia em fase gasosa acoplada a espectrometria de massa (GC/MS. Nesse trabalho foram avaliados, por técnica de extração líquido/líquido e posterior identificação em GC/MS-SIM, 15 EAA, dos quais três foram quantificados. Os critérios de correlação entre os íons mais característicos dos EAA analisados foram definidos como segue: os de intensidade relativa maior que 20% podem apresentar uma variação de até 30%; os de intensidade relativa entre 10 e 20% podem apresentar uma variação de até 50% e os de intensidade relativa menor que 10% podem apresentar uma variação de até 90%. Com a aplicação dos critérios anteriores, foi possível confirmar os resultados obtidos em oito amostras de urina de atletas, nos quais foi constatado o uso dos EAA, ficando evidenciada a importância da aplicação desses critérios de positividade na comprovação inequívoca da presença de tais substâncias em amostras biológicas.The use of anabolic androgenic steroids (AAS in sports is in a constant increase among professionals athlets and amateurs. These substances were banned by the International Olimpic Committee and the doping control of this steroids are to be performed analysing biological samples taken from this athletes using gas cromatography coupled with mass spectrometry (GC/MS. This paper evaluates 15 AAS by means of liquid extration and subsequent GC/MS identification. Three of these AAS were also quantified. Correlation criteria among the AAS most characteristic ions were stablished for the evidence of positive samples: when comparing these ions

Identificação de compostos voláteis da cúrcuma empregando microextração por fase sólida e cromatografia gasosa acoplada à espectrometria de massas Identification of volatile compounds of turmeric using solid phase microextraction and gas chromatography coupled to mass spectrometry

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Adriana R. Mata

2004-03-01

Full Text Available Compostos voláteis da cúrcuma (Curcuma longa L. cultivada no Brasil foram isolados por microextração por fase sólida. Os rizomas foram cozidos em solução de bicarbonato de sódio 0,1%, fatiados, secos e triturados. Visando estabelecer o sistema ideal para a microextração, fibras de polidimetilsiloxano de 100µm de espessura foram expostas ao headspace de frascos de 10mL. Estudou-se a influência das seguintes variáveis sobre o rendimento dos compostos voláteis obtidos: amostras em pó (0,1 a 1,0g e em solução (40mg/L, diferentes temperaturas (40 a 70ºC e tempos (2 a 20min de partição. O efeito da temperatura (210 a 240ºC e do tempo (3 e 5min de dessorção também foi avaliado. As melhores condições para a partição dos compostos voláteis foram 0,1g do pó, 70ºC e 5min. A temperatura de 220ºC e o tempo de 5 minutos foram os de maior eficiência para a dessorção. A cromatografia gasosa foi conduzida em coluna capilar, detecção por ionização de chama e identificação por espectrometria de massas. A análise dos espectros de massas obtidos para os nove compostos voláteis predominantes indicou a presença de ar-curcúmeno, ar-turmerona, zingibereno, beta-sesquifelandreno, sabineno, 1,8-cineol e 1,4-terpineol.Volatile compounds from turmeric (Curcuma longa L. cultived in Brazil were isolated by solid phase microextraction. The rhizomes were cooked in 0.1% sodium bicarbonate solution, sliced, dried and ground. Polydimethyldiloxanes fibers (100 mm diameter were exposed to the headspace of 10 mL flasks with the aim of establishing an ideal microextraction system. The influence of the following parameters on the volatile substances obtained was studied: powder samples (0.1 to 1.0 g and dissolved samples (40 mg/L, different temperatures (40 to 70ºC and partition periods (2 to 20 min. The effect of temperature (210 to 240ºC and time (3 to 5 min on desorption efficiency was also evaluated. Optimum conditions for the

Concentrações plasmáticas de triptamina, tiramina e feniletilamina em eqüinos sob efeitos de sobrecarga de carboidratos e antiinflamatórios não esteroidais Plasmatic concentrations of tryptamine, tyramine end phenylethylamine in horses under the effect of carbohydrate overload and non-steroid antinflammatory compounds

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Paulo Tarso L. Botteon

2008-06-01

Full Text Available As concentrações plasmáticas das aminas triptamina (TRP, tyramina (TYR e pheniletilamina (PEA foram determinadas por cromatografia gasosa (CG de 20 eqüinos sob efeito de sobrecarga por carboidratos (SC. Após 36h da SC os animais foram aleatoriamente divididos em quatro grupos (n=5 e receberam a cada 12h por via iv: solução salina 10mL (GC, ketoprofeno 2,2mg/kg (GK, fenilbutazona 4,4mg/kg (GF e flunixin meglumine 1,1mg/kg (GFM. As concentrações das aminas TYR e PEA variaram de 0,18 a 164,2mg/L, com diferenças nos tempos avaliados, mas não entre os tratamentos (pThe concentrations of the bioactives amines tryptamine (TRP, tyramine (TYR and phenylethylamine (PEA were determined by gas chromatography in plasma samples of 20 horses submitted to carbohydrate overload. Thirty hours after the overload, the horses were randomly distributed in four groups (n=5 and were submitted to four IV treatments every 12 hours: 10ml of saline (GC, ketoprofen 2.2mg/kg (GK, phenylbutazone 4.4mg/kg (GF, and flunixin meglumine 1.1mg/kg (GFM. Blood samples were collected at various times after the overload (0-72 h. Plasma TYR and PEA concentrations ranged from 0.18 to 164.2mg/L, and differed significantly with time (p<0.01, but did not differ in the treatments. Plasma concentrations of TRP differed between times and treatments. The GC was significantly major than other treatments at 48h and 60h after the overload, and the plasma concentration of TRP in groups GK and GFM was significantly lower than in groups GF and GC at 72 h (p=0.0012. We concluded that the anti-inflammatory drugs evaluated do not interfere in the plasma concentration of TYP and PEA. For TRP, ketoprofen and flunixin meglumine was effective to reduce de plasmatic concentration of this amine.

Analysis of volatile compounds of Ilex paraguariensis A. St. - Hil. and its main adulterating species Ilex theizans Mart. ex Reissek and Ilex dumosa Reissek Análise de compostos voláteis de Ilex paraguariensis A. St. - Hil. e suas principais espécies adulterantes Ilex theizans Mart. ex Reissek e Ilex dumosa Reissek

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Rogério Marcos Dallago

2011-12-01

Full Text Available The adulteration of the product Ilex paraguariensis with other Ilex species is a mAjor problem for maté tea producers. In this work, three species of Ilex were evaluated for their volatile composition by headspace solid phase microextraction coupled to gas chromatography and mass spectrum detector (HS-SPME/GC-MS. The adulterating species I. dumnosa and I. theizans Mart. ex Reissek presented a different profile of volatile organic compounds when compared to I. paraguariensis. Aldehydes methyl-butanal, pentanal, hexanal, heptanal and nonanal were detected only in the adulterating species. This result suggests that such compounds are potential chemical markers for identification of adulteration and quality analysis of products based on Ilex paraguariensis.A adulteração do produto Ilex paraguariensis com outras espécies de Ilex é um dos principais problemas dos produtores de erva-mate. Neste trabalho, três espécies de Ilex foram avaliadas quanto à sua composição volátil por microextração em fase sólida acoplada à cromatografia gasosa e detector de espectro de massas (HS-SPME/GC-MS. As espécies adulterantes I. dumnosa e I. theizans Mart. ex Reissek apresentaram um perfil diferente de compostos orgânicos voláteis, quando comparadas com a I. paraguariensis. Os aldeídos metil-butanal, pentanal, hexanal, heptanal e nonanal foram detectados apenas nas espécies adulterantes. Esse resultado sugere que esses compostos químicos são marcadores potenciais para a identificação de adulteração e análise da qualidade dos produtos à base de Ilex paraguariensis.

Determinación de aminas aromaticas por cromatografia liquida de alta resolución.

OpenAIRE

Gutiérrez Bouzán, Mª Carmen; Crespi Rosell, Martí

1989-01-01

Este trabajo consiste en la puesta a punto del metodo analítico para la determinación por cromatografia liquida de alta resolución (HPLC) de las aminas aromáticas empleadas más frecuentemente en la fabricación de colorantes sulfurosos: m-tolilendiamina, p-fenilendiamina, o-toluidina, p-toluidina, anilina, p-aminofenol, difenilamina, y p-hidroxidifenilamina. La longitud de onda de detección es de 260 nm. El principal objetivo del presente estudio es la consecución de un método de análisis p...

Detecção de capsaicina em extratos dos frutos verdes e maduros de Capsicum baccatum L. pelas metodologias de cromatografia em camada delgada e histoquímica

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Tamires de Souza RODRIGUES

2015-01-01

Full Text Available A pimenta dedo-de-moça (Capsicum baccatum L. é uma espécie utilizada no mundo inteiro pelo seu sabor picante e por possuir inúmeras atividades medicinais. Essas atividades farmacológicas são proporcionadas por um grupo de substâncias presentes, os capsaicinoides, além de taninos, flavonoides, vitamina C, entre outros. Dos capsaicinoides presentes, a capsaicina possui especial importância. O objetivo do presente trabalho foi avaliar a presença da capsaicina nos extratos dos frutos verdes e maduros de Capsicum baccatum L. pelas metodologias de cromatografia em camada delgada e histoquímica. Os extratos foram preparados com acetona. A cromatografia foi realizada com placas de sílica gel G4, eluída com hexano:acetato de etila (60:40 e reveladas com reagente de Dragendorff. A capsaicina pode ser detectada somente no estágio imaturo (verde dos frutos de Capsicum baccatum L. pela metodologia de cromatografia em camada delgada e pelo teste histoquímico.

NOVAS APLICAÇÕES DE SISTEMAS SFE "HOME MADE".: I. PLANTAS MEDICINAIS BRASILEIRAS

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Fernando M. LANÇAS

1997-12-01

Full Text Available Neste trabalho, apresenta-se uma visão geral da evolução do uso da SFE (extração com fluido supercrítico na análise de plantas medicinais brasileiras dentro das pesquisas desenvolvidas pelo Laboratório de Cromatografia do IQSC-USP. Utilizou-se como fluido extrator o CO2, puro ou modificado com solventes de polaridade baixa a alta (pentano, solventes halogenados, álcoois, água, para a extração seletiva de princípios ativos de Maytenus aquifolium ("espinheira santa" e Mikania glomerata ("guaco", respectivamente contendo triterpenos e cumarina. Os extratos obtidos por SFE foram analisados por CGAR (cromatografia gasosa de alta resolução, CLAE-DAD (cromatografia líquida de alta eficiência com detector" photodiodearray" ou CCD (cromatografia de camada delgada. A SFE forneceu resultados similares ou melhores do que os obtidos com métodos convencionais de extração (Soxhlet, maceração, etc, indicando o potencial uso da SFE para análise e/ou produção de preparações contendo estas plantas medicinais.Further applications of "home made" SFE systems. I. Brazilian medicinal plants. In this paper, an overview on the evolution of the utilization of SFE for the analysis of Brazilian medicinal plants in the research developed by the Laboratório de Cromatografia, IQSC-USP, is presented. CO2, pure or with modifiers from low to high polarity (pentane, halogenated solvents, alcohols, water were used for the selective extraction of active compounds. Maytenus aquifolium (known popularly in Brazil as" espinheira santa", and Mikania glomerata ("guaco", containing respectively triterpenes and coumarin, were studied. The extracts obtained by SFE showed similar or better results than of those extracts obtained by conventional extraction methods (Soxhlet, maceration, etc., which indicates the potential of SFE technique in the analysis and/or production of phytomedicines.

Analysis of Alkaloids from Physalis peruviana by Capillary GC, Capillary GC-MS, and GC-FTIR.

Science.gov (United States)

Kubwabo, C; Rollmann, B; Tilquin, B

1993-04-01

The alkaloid composition of the aerial parts and roots of PHYSALIS PERUVIANA was analysed by capillary GC (GC (2)), GC (2)-MS and GC (2)-FTIR. Eight alkaloids were identified, three of those alkaloids are 3beta-acetoxytropane and two N-methylpyrrolidinylhygrine isomers, which were not previously found in the genus PHYSALIS. A reproduction of the identification of alkaloids detected in the plant by the use of retention indices has been proposed.

NOVAS APLICAÇÕES DE SISTEMAS SFE "HOME MADE": III. ENERGIA QUÍMICA E ELÉTRICA

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Fernando M. LANÇAS

1997-12-01

Full Text Available Este trabalho apresenta três aplicações da SFE com diferentes fluídos supercríticos, matrizes e sistemas de extração. Um sistema estático "home made" foi utilizado na pesquisa de fontes alternativas de insumos químicos e energéticos tais como o bagaço de cana-de-açucar e o carvão mineral. Foram usados, respectivamente, o etanol (sem e com catalisador e o tolueno como fluídos extratores e hidrogênio como gás de pressurização. Na extração dos contaminantes do óleo mineral adsorvidos em bauxita, foi utilizado o dióxido de carbono como fluído extrator em um sistema "home made"/dinâmico. Estudos visando a maximização do rendimento de alguns dos processos também foram realizados, utilizando o planejamento fatorial e a metodologia da superfície de resposta. Os produtos de maior interesse neste trabalho (fração de resinas, obtidos do processo de extração do bagaço de cana-de-açucar e aqueles contaminantes do óleo isolante adsorvidos em bauxita extraídos com fluídos supercríticos foram caracterizados usando cromatografia gasosa de alta resolução com detector de ionização de chama (CGAR - DIC e cromatografia gasosa de alta resolução com detector seletivo de massas (CGAR - EM após fracionamento por cromatografia líquida preparativa em 8 frações distintas.This work presents three aplications of SFE with different supercritical fluids, samples and extraction systems. A home made static system was utilized in the search for alternative chemicals and energetics resources such as sugar cane bagasse and mineral coal. Ethanol (with and without catalyst and toluene were used, respectively ,as extraction fluids and hydrogen as pressurization gas. The adsorbed contaminants of mineral oil in bauxite were also extracted with carbon dioxide as extractor fluid in a home made dinamical system. Maximization of yields in some processes was studied using factorial design and response surface methodologies. The products

Cromatografia em camada delgada acoplada a voltametrias cíclica e de pulso diferencial na análise de ácido rosmarínico de Rosmarinus officinalis Linné (Alecrim)

OpenAIRE

GONÇALVES, Darlene

2010-01-01

Esse estudo apresenta um método eletroanalítico em estado sólido para identificação e quantificação do ácido rosmarínico (AR), um fitoantioxidante de grande interesse pelas vantagens terapêuticas e aplicabilidade nas áreas alimentícia, cosmética e farmacêutica; após isolamento do mesmo de amostras de Rosmarinus officinalis Linné (alecrim), através de cromatografia em camada delgada (CCD), onde utilizou-se a sílica contendo o analito isolado (mancha da cromatografia) raspada da cromatoplaca, p...

Trocas gasosas de mudas de videira, obtidas por dois porta-enxertos, submetidos à deficiência hídrica.

OpenAIRE

SOUZA, C.R. de; SOARES, A.M.; REGINA, M. de A.

2001-01-01

Este trabalho teve como objetivo avaliar o efeito da deficiência hídrica e de dois porta-enxertos nas trocas gasosas de mudas de videira cultivadas em vasos, nas condições de casa de vegetação. Utilizou-se como copa a 'Niágara Rosada' (Vitis labrusca), e como porta-enxertos, o 101-14 (V. riparia) e o 1103 Paulsen (V. rupestris x V. berlandieri). Doze dias após a suspensão da rega, o potencial hídrico foliar da combinação 'Niágara Rosada'/101-14 apresentou os menores valores (-2,80 MPa) em rel...

Lipídios em sedimentos arqueológicos: resultados preliminares do sítio arqueológico Rio do Meio, Ilha de Santa Catarina (SC Lipids in archaeological sediments: preliminary results of the archaeological site Rio do Meio, Santa Catarina Island (SC, Brazil

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Fabrício Augusto Hansel

2008-02-01

Full Text Available Este trabalho foi realizado com o objetivo de avaliar a distribuição de lipídios em sedimentos arqueológicos do sítio Rio do Meio, Ilha de Santa Catarina. Nos extratos totais de lipídios, analisados por cromatografia gasosa e espectrometria de massas (CG e CG-EM, predominaram os compostos ácidos e álcoois saturados. Foram detectados pelo menos dois tipos de matéria orgânica: uma antiga e outra comparativamente recente. Na primeira, o extrato total de lipídios foi dominado por ácidos graxos de cadeias curtas ( Ac20:0 e Al20:0. Em contraste, na deposição classificada como recente, foram identificados em maiores teores os ácidos e álcoois de cadeias longas (> Ac20:0 e Al20:0. Neste estudo, foi possível observar a incorporação de material orgânico procedente de fontes de origem vegetal, bacteriana e, possivelmente, animal (gorduras nos sedimentos arqueológicos analisados.In this study the distribution of lipid compounds was evaluated in sediment samples of an archaeological site Rio do Meio, Santa Catarina Island, Brazil. In the total lipid extracts, analyzed by gas chromatography and mass spectrometry (GC and GC-MS, saturated fatty acids and alcohols were predominant. At least two sources of organic matter were detected, an older and a more recent one. In the old deposit, the most abundant lipids were short-chain fatty acids ( Ac20:0 and Al20:0. In contrast, the fresh deposit was dominated by long-chain fatty acids and alcohols (> Ac20:0 and Al20:0. This paper described the incorporation of vegetal, bacterial and possible animal (fat sources into the archaeological sediments analyzed.

AVALIAÇÃO DA FORÇA DE RETENÇÃO DE COMPOSTOS ORGÂNICOS (COV EM NANOESTRUTURAS DE CARBONO “CUP STACKED”

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Waldir Nagel Schirmer

2009-01-01

Full Text Available Adsorventes carbonados estão entre as melhores opções na remoção de compostos orgânicos voláteis (COV de correntes gasosas, pela boa afinidade que apresentam com compostos dessa natureza, além de baixo custo e disponibilidade. O presente trabalho avalia o desempenho do ciclo adsorção/dessorção de dois compostos orgânicos voláteis (fenol e tolueno em nanotubos de carbono (NTC comparativamente a um carbono grafitizado de aplicação tipicamente analítica (Carbotrap. As metodologias de amostragem e análise empregadas compreendem a coleta de gases por bombeamento (amostragem ativa em cartuchos (tubos, contendo o material adsorvente com posterior análise por cromatografia gasosa e espectrometria de massa (CG/EM, de acordo com o Método TO-17 da USEPA. Em relação ao desempenho dos adsorventes, o nanotubo obteve clara vantagem em relação ao Carbotrap, conseguindo reter mais adsorbato por massa de adsorvente. Além disso, não foi verificada interação diferenciada do fenol e tolueno com os dois adsorventes, tanto na etapa de adsorção quanto na de dessorção.

AVALIAÇÃO DA FORÇA DE RETENÇÃO DE COMPOSTOS ORGÂNICOS (COV EM NANOESTRUTURAS DE CARBONO “CUP STACKED”

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Waldir Nagel Schirmer

2008-12-01

Full Text Available Adsorventes carbonados estão entre as melhores opções na remoção de compostos orgânicos voláteis (COV de correntes gasosas,pela boa afinidade que apresentam com compostos dessa natureza, além de baixo custo e disponibilidade. O presente trabalhoavalia o desempenho do ciclo adsorção/dessorção de dois compostos orgânicos voláteis (fenol e tolueno em nanotubos de carbono(NTC comparativamente a um carbono grafitizado de aplicação tipicamente analítica (Carbotrap. As metodologias deamostragem e análise empregadas compreendem a coleta de gases por bombeamento (amostragem ativa em cartuchos (tubos,contendo o material adsorvente com posterior análise por cromatografia gasosa e espectrometria de massa (CG/EM, de acordocom o Método TO-17 da USEPA. Em relação ao desempenho dos adsorventes, o nanotubo obteve clara vantagem em relação aoCarbotrap, conseguindo reter mais adsorbato por massa de adsorvente. Além disso, não foi verificada interação diferenciada dofenol e tolueno com os dois adsorventes, tanto na etapa de adsorção quanto na de dessorção.

Gc protein-derived macrophage activating factor (GcMAF): isoelectric focusing pattern and tumoricidal activity.

Science.gov (United States)

Mohamad, Saharuddin Bin; Nagasawa, Hideko; Sasaki, Hideyuki; Uto, Yoshihiro; Nakagawa, Yoshinori; Kawashima, Ken; Hori, Hitoshi

2003-01-01

Gc protein is the precursor for Gc protein-derived macrophage activating factor (GcMAF), with three phenotypes: Gc1f, Gc1s and Gc2, based on its electrophoretic mobility. The difference in electrophoretic mobility is because of the difference in its posttranslational sugar moiety composition. We compared the difference between Gc protein and GcMAF electrophoretic mobility using the isoelectric focusing (IEF) method. The tumoricidal activity of GcMAF-treated macrophage was evaluated after coculture with L-929 cell. The tumoricidal mechanism was investigated using TNF bioassay and nitric oxide (NO) release. The difference in Gc protein and GcMAF electrophoretic mobility was detected. The tumoricidal activity of GcMAF-treated macrophage was detected, but no release of TNF and NO was detected. The difference of isoelectric focusing mobility in Gc protein and GcMAF would be useful to develop a GcMAF detection method. GcMAF increased macrophage tumoricidal activity but TNF and NO release were not involved in the mechanism.

Análise de pesticidas organoclorados em água usando a microextração em fase sólida por headspace com cromatografia gasosa e espectrometria de massas

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Crislaine Batista Prates

2011-01-01

Full Text Available A method based on headspace - solid phase microextraction coupled with gas chromatography - mass spectrometry was validated for the quantitative determination of 18 organochlorine pesticides in water. For the extraction conditioning some parameters as the best type of coating fiber, time and temperature of extraction, pH and ionic strength were evaluated. The method HS-SPME/GC-MS/MS showed linear coefficient above 0.9948. The repeatability of the measurements were lower than 7.6%. Relative recoveries were between 88 and 110%. Limits of detection from 0.5 x 10-3 to 1.0 mg L-1 were obtained. A total of 31 samples were analyzed and 16 presented from 1 to 5 pesticides.

Trocas gasosas e fluorescência da clorofila em plantas de berinjela sob lâminas de irrigação

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Flaviana G. da Silva

2015-10-01

Full Text Available RESUMOA berinjela tem grande importância nutricional e socioeconômica, sendo cultivada e comercializada em vários países, principalmente em ambiente protegido; sua produção, assim como a de inúmeros cultivos agrícolas, é dependente de fatores como água, nutrientes e luz; propôs-se, assim, com este trabalho, avaliar as trocas gasosas, fluorescência da clorofila a e temperatura foliar de berinjela cultivada em ambiente protegido em diferentes lâminas de irrigação. O estudo foi realizado em casa de vegetação utilizando-se delineamento inteiramente casualizado, com 5 tratamentos e oito repetições, totalizando 40 unidades experimentais. Os tratamentos constaram de cinco lâminas de irrigação: 33, 66, 100, 133 e 166% da ETc, as quais corresponderam a 133, 266, 403, 536, 669 mm planta-1 ciclo-1, respectivamente. A taxa fotossintética das plantas de berinjela aumenta com o acréscimo da reposição hídrica. Os valores mais expressivos de trocas gasosas (A, E, gs, Ci, EiUA e EiC nas plantas de berinjela, de forma geral, foram observados quando se utilizaram, na irrigação, lâminas estimadas entre 123,52 e 166% da ETc. A fluorescência da clorofila aumentou com o aumento das lâminas de irrigação e a temperatura foliar diminuiu em função do aumento da água.

TROCAS GASOSAS E EFICIÊNCIA DO FOTOSSISTEMA II EM PLANTAS ADULTAS DE SEIS ESPÉCIES FLORESTAIS EM FUNÇÃO DO SUPRIMENTO DE ÁGUA NO SOLO1

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David de Holanda Campelo

2015-10-01

Full Text Available RESUMO A redução da disponibilidade hídrica causa efeitos sobre a fotossíntese e o desenvolvimento de espécies arbóreas. O objetivo deste trabalho foi avaliar as trocas gasosas e a eficiência fotoquímica do fotossistema II em plantas adultas de gonçalo-alves (Astronium fraxinifolium Schott., guanandi (Calophyllum brasiliense Cambess., ipê-amarelo (Handroanthus serratifolius (Vahl., ipê-rosa (Handroanthus impetiginosa (Mart. Matos, marupá (Simarouba amara Aubl. e mogno (Swietenia macrophylla King. cultivadas em condições de sequeiro e irrigadas, no Perímetro Irrigado do Baixo Acaraú, Ceará. O delineamento experimental adotado foi o de medidas repetidas no tempo, num esquema de parcelas subsubdivididas (6 x 2 x 3, sendo a parcela principal composta por seis espécies, a subparcela por dois regimes hídricos (irrigado e sequeiro e a subsubparcela pelas épocas de avaliação. As análises das trocas gasosas foram realizadas em 22/11/2012 (estação seca, 07/02/2013 (data que antecedeu o período chuvoso e 17/05/2013 (estação chuvosa. As espécies mogno, guanandi e ipê-amarelo mostraram-se mais sensíveis ao déficit hídrico, em comparação com as outras espécies, o que foi evidenciado pelas maiores reduções nas trocas gasosas e na eficiência fotoquímica do fotossistema II. O ipê-rosa, o marupá e o gonçalo-alves mostraram-se mais adaptados às condições de baixa disponibilidade hídrica do solo.

Solvents orgànics en electroforesi capil·lar i cromatografia de líquids

OpenAIRE

Subirats i Vila, Xavier

2007-01-01

La cromatografia de líquids d'alta eficàcia (HPLC) és la tècnica de separació més àmpliament utilitzada, degut a la seva sensibilitat, exactitud de les determinacions quantitatives i aplicabilitat a anàlits no volàtils o termolàbils d'interès científic i industrial. L'electroforesi capil·lar juga un paper fonamental en bioquímica. Aquesta tècnica permet obtenir anàlisis ràpides amb una elevada resolució i un baix consum de reactius auxiliars, fet que minimitza la generació de residus. L'objec...

Protein chemical characterization of Gc globulin (vitamin D-binding protein) isoforms; Gc-1f, Gc-1s and Gc-2

DEFF Research Database (Denmark)

Christiansen, Maja; Jørgensen, Charlotte S; Laursen, Inga

2007-01-01

-survival of patients with fulminant hepatic failure and trauma. Here, we characterize the dominant isoforms of plasma-derived Gc globulin from Cohn fraction IV paste with respect to amino acid sequence and posttranslational modifications. Gc globulin was purified in large scale and the isoforms separated by ion...

Theoretical study of GC+/GC base pair derivatives

International Nuclear Information System (INIS)

Meng Fancui; Wang Huanjie; Xu Weiren; Liu Chengbu

2005-01-01

The geometries of R (R=CH 3 , CH 3 O, F, NO 2 ) substituted GC base pair derivatives and their cations have been optimized at B3LYP/6-31G* level and the substituent effects on the neutral and cationic geometric structures and energies have been discussed. The inner reorganization energies of various base pair derivatives and the native GC base pair have been calculated to discuss the substituent effects on the reorganization energy. NBO (natural bond orbital) analysis has been carried out on both the neutral and the cationic systems to investigate the differences of the charge distributions and the electronic structures. The outcomes indicate that 8-CH 3 O-G:C has the greatest reorganization energy and 8-NO 2 -G:C has the least, while the other substituted base pairs have a reorganization energy close to that of G:C. The one charge is mostly localized on guanine part after ionization and as high as 0.95e. The bond distances of N1-N3'andN2-O2' in the cationic base pair derivatives shortened and that of O6-N4' elongated as compared with the corresponding bond distances of the neutral GC base pair derivatives

Determinação de isotiocianato de benzila em Carica papaya utilizando cromatografia gasosa com detectores seletivos Determination of benzyl isothiocyanate in Carica papaya using gas chromatography with selectives detectors

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Izabela Miranda de Castro

2008-01-01

Full Text Available In the present work, a method was developed and validated for the quantification of benzyl isothiocyanate (BITC in the fruits of Carica papaya. The quantification of this compound was carried out by gas chromatography (GC with selective detectors - nitrogen phosphorus detector (NPD and flame photometric detector (FPD. The performance of these detectors showed a higher sensitivity of the NPD with a broader linear range of detection. The LOD/LOQ were 0.038/0.100 µg/mL for NPD and 5.78/19.29 µg/mL for FPD. The recovery of the method for BITC was 90,64%. An average value of BITC concentration in all the analyzed samples was 16,23 µg BITC/g.

Immunotherapy for Prostate Cancer with Gc Protein-Derived Macrophage-Activating Factor, GcMAF.

Science.gov (United States)

Yamamoto, Nobuto; Suyama, Hirofumi; Yamamoto, Nobuyuki

2008-07-01

Serum Gc protein (known as vitamin D(3)-binding protein) is the precursor for the principal macrophage-activating factor (MAF). The MAF precursor activity of serum Gc protein of prostate cancer patients was lost or reduced because Gc protein was deglycosylated by serum alpha-N-acetylgalactosaminidase (Nagalase) secreted from cancerous cells. Therefore, macrophages of prostate cancer patients having deglycosylated Gc protein cannot be activated, leading to immunosuppression. Stepwise treatment of purified Gc protein with immobilized beta-galactosidase and sialidase generated the most potent MAF (termed GcMAF) ever discovered, which produces no adverse effect in humans. Macrophages activated by GcMAF develop a considerable variation of receptors that recognize the abnormality in malignant cell surface and are highly tumoricidal. Sixteen nonanemic prostate cancer patients received weekly administration of 100 ng of GcMAF. As the MAF precursor activity increased, their serum Nagalase activity decreased. Because serum Nagalase activity is proportional to tumor burden, the entire time course analysis for GcMAF therapy was monitored by measuring the serum Nagalase activity. After 14 to 25 weekly administrations of GcMAF (100 ng/week), all 16 patients had very low serum Nagalase levels equivalent to those of healthy control values, indicating that these patients are tumor-free. No recurrence occurred for 7 years.

Analysis of Biogenic Amines by GC/FID and GC/MS

OpenAIRE

Nakovich, Laura

2003-01-01

Low levels of biogenic amines occur naturally, but high levels (FDA sets 50 ppm of histamine in fish as the maximum allowable level) can lead to scombroid poisoning. Amines in general are difficult to analyze by Gas Chromatography (GC) due to their lack of volatility and their interaction with the GC column, often leading to significant tailing and poor reproducibility. Biogenic amines need to be derivatized before both GC and HPLC analyses. The objective of this research was to devel...

Quantitative chemical analysis for the standardization of copaiba oil by high resolution gas chromatography; Analise quimica quantitativa para a padronizacao do oleo de copaiba por cromatografia em fase gasosa de alta resolucao

Energy Technology Data Exchange (ETDEWEB)

Tappin, Marcelo R.R.; Pereira, Jislaine F.G.; Lima, Lucilene A.; Siani, Antonio C. [Farmanguinhos - Inst. de Tecnologia em Farmacos, Rio de Janeiro, RJ (Brazil)]. E-mail: siani@far.fiocruz.br; Mazzei, Jose L. [Universidade Federal, Rio de Janeiro, RJ (Brazil). Escola de Quimica; Ramos, Monica F.S. [Universidade Federal, Rio de Janeiro, RJ (Brazil). Faculdade de Farmacia. Dept. de Medicamentos

2004-04-01

Quantitative GC-FID was evaluated for analysis of methylated copaiba oils, using trans-(-)-caryophyllene or methyl copalate as external standards. Analytical curves showed good linearity and reproducibility in terms of correlation coefficients (0.9992 and 0.996, respectively) and relative standard deviation (< 3%). Quantification of sesquiterpenes and diterpenic acids were performed with each standard, separately. When compared with the integrator response normalization, the standardization was statistically similar for the case of methyl copalate, but the response of trans-(-)-caryophyllene was statistically (P < 0.05) different. This method showed to be suitable for classification and quality control of commercial samples of the oils. (author)

Immunotherapy for Prostate Cancer with Gc Protein-Derived Macrophage-Activating Factor, GcMAF1

Science.gov (United States)

Yamamoto, Nobuto; Suyama, Hirofumi; Yamamoto, Nobuyuki

2008-01-01

Serum Gc protein (known as vitamin D3-binding protein) is the precursor for the principal macrophage-activating factor (MAF). The MAF precursor activity of serum Gc protein of prostate cancer patients was lost or reduced because Gc protein was deglycosylated by serum α-N-acetylgalactosaminidase (Nagalase) secreted from cancerous cells. Therefore, macrophages of prostate cancer patients having deglycosylated Gc protein cannot be activated, leading to immunosuppression. Stepwise treatment of purified Gc protein with immobilized β-galactosidase and sialidase generated the most potent MAF (termed GcMAF) ever discovered, which produces no adverse effect in humans. Macrophages activated by GcMAF develop a considerable variation of receptors that recognize the abnormality in malignant cell surface and are highly tumoricidal. Sixteen nonanemic prostate cancer patients received weekly administration of 100 ng of GcMAF. As the MAF precursor activity increased, their serum Nagalase activity decreased. Because serum Nagalase activity is proportional to tumor burden, the entire time course analysis for GcMAF therapy was monitored by measuring the serum Nagalase activity. After 14 to 25 weekly administrations of GcMAF (100 ng/week), all 16 patients had very low serum Nagalase levels equivalent to those of healthy control values, indicating that these patients are tumor-free. No recurrence occurred for 7 years. PMID:18633461

Caracterização química do óleo essencial de Hypericum brasiliense Choisy

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E.S. Carvalho

Full Text Available Hypericum brasiliense Choisy, planta da família Guttiferae, ocorre principalmente nas regiões Sudeste e Sul do Brasil. Em trabalhos anteriores foram isolados e identificados nesta espécie, dentre outras classes de compostos, xantonas, floroglucinóis e flavonóides. Apesar da presença de óleos essenciais ser uma característica do gênero, ainda não há registros na literatura da composição química do óleo essencial desta espécie. Neste trabalho foi realizado o estudo químico da fração volátil de H. brasiliense visando identificar e quantificar as substâncias químicas presentes através da cromatografia em fase gasosa acoplada a espectrômetro de massas equipado com banco de dados.

Preparation of Gc protein-derived macrophage activating factor (GcMAF) and its structural characterization and biological activities.

Science.gov (United States)

Mohamad, Saharuddin Bin; Nagasawa, Hideko; Uto, Yoshihiro; Hori, Hitoshi

2002-01-01

Gc protein has been reported to be a precursor of Gc protein-derived macrophage activation factor (GcMAF) in the inflammation-primed macrophage activation cascade. An inducible beta-galactosidase of B cells and neuraminidase of T cells convert Gc protein to GcMAF. Gc protein from human serum was purified using 25(OH)D3 affinity column chromatography and modified to GcMAF using immobilized glycosidases (beta-galactosidase and neuraminidase) The sugar moiety structure of GcMAF was characterized by lectin blotting by Helix pomatia agglutinin. The biological activities of GcMAF were evaluated by a superoxide generation assay and a phagocytosis assay. We successfully purified Gc protein from human serum. GcMAF was detected by lectin blotting and showed a high biological activity. Our results support the importance of the terminal N-acetylgalactosamine moiety in the GcMAF-mediated macrophage activation cascade, and the existence of constitutive GcMAF in human serum. These preliminary data are important for designing small molecular GcMAF mimics.

Variabilidade sazonal dos constituintes da própolis vermelha e bioatividade em Artermia salina

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Lívio César Cunha Nunes

Full Text Available A própolis é uma substância resinosa coletada pelas abelhas de diversas partes das plantas. Sua composição depende da época, vegetação e local de coleta. Apresenta diversas atividades biológicas como antimicrobiana, antioxidante, antitumoral, dentre outras. Foi realizado estudo da variabilidade sazonal, nos meses de fevereiro, junho e outubro de 2006, dos constituintes voláteis da própolis vermelha de Pernambuco através da extração por headspace dinâmico e identificação por cromatografia gasosa acoplada com espectrometria de massas (CG-EM. Foram identificados 34 constituintes voláteis, sendo monoterpenos e monoterpenóides, sesquiterpenos e sesquiterpenóides, fenilpropanóides, aldeídos, cetonas e η-alcanos. Os constituintes majoritários foram o trans-anetol, α-copaeno e o metil cis-isoeugenol. Também foi realizado o perfil fitoquímico por cromatografia em camada delgada (CCD, através da qual os constituintes fenólicos foram identificados como majoritários. Com o extrato bruto metanólico da própolis, realizou-se o ensaio de letalidade em Artemia salina, que demonstrou DL50 de 18,9 µg/mL, sugerindo uma possível atividade antitumoral.

Purification of equine Gc-globulin

DEFF Research Database (Denmark)

Houen, Gunnar; Pihl, Tina Holberg; Andersen, Pia Haubro

Objectives With the aim of producing antibodies for an equine Group specific component (Gc)-globulin assay, the protein was purified from normal equine plasma. Methods Equine Gc-globulin was purified from healthy horse plasma using ion exchange chromatography (Q-Sepharose, CM......-Sepharose) and preparative PAGE. Results Equine Gc-globulin has successfully been purified from healthy horse plasma and rabbits and mice are being immunized to produce specific antibodies. Conclusions Purification of equine Gc-globulin and the production of specific antibodies will make it possible to develop an assay...... to be a sensitive marker of acute tissue injury and fatal outcome in humans. Patients with a low plasma concentration of Gc-globulin due to severe tissue injury might potentially benefit from infusions with purified Gc-globulin [1]. With an equine Gc-globulin assay, future studies will investigate the concentration...

Immunotherapy for Prostate Cancer with Gc Protein-Derived Macrophage-Activating Factor, GcMAF1

OpenAIRE

Yamamoto, Nobuto; Suyama, Hirofumi; Yamamoto, Nobuyuki

2008-01-01

Serum Gc protein (known as vitamin D3-binding protein) is the precursor for the principal macrophage-activating factor (MAF). The MAF precursor activity of serum Gc protein of prostate cancer patients was lost or reduced because Gc protein was deglycosylated by serum α-N-acetylgalactosaminidase (Nagalase) secreted from cancerous cells. Therefore, macrophages of prostate cancer patients having deglycosylated Gc protein cannot be activated, leading to immunosuppression. Stepwise treatment of pu...

Deficiência hídrica, trocas gasosas e crescimento de raízes em laranjeira ‘Valência’ sobre dois tipos de porta-enxertos

OpenAIRE

Magalhães Filho,José Rodrigues; Amaral,Lucas Rios do; Machado,Daniela Fávero São Pedro; Medina,Camilo Lázaro; Machado,Eduardo Caruso

2008-01-01

O crescimento e a distribuição do sistema radicular afetam as respostas das plantas à ocorrência de deficiência hídrica. Este trabalho teve como objetivo avaliar em mudas de laranjeira 'Valência' enxertada sobre limoeiro 'Cravo' ou Poncirus trifoliata ('Trifoliata') o crescimento de raízes, as trocas gasosas (CO2 e H2O), o potencial da água na folha e a distribuição de carboidratos nos diversos órgãos, em plantas submetidas à deficiência hídrica. As mudas foram transplantadas para 32 rizotron...

Caracterização eletrofisiológica em girassol: cinética, rotas de propagação, trocas gasosas e fluorescência da clorofila

OpenAIRE

Diogo Capelin

2016-01-01

Esta tese refere-se a pesquisa cujo o principal objetivo foi estudar os efeitos da sinalização elétrica sobre parâmetros fisiológicos de trocas gasosas e fluorescência da clorofila, bem como caracterizar e identificar rotas de propagação de sinais elétricos desencadeados por estímulos de queima em plantas de girassol. Os resultados obtidos a partir deste estudo demonstram que os sinais elétricos desencadeados por estímulo de queima podem ser classificados como potenciais de variação (PV). Est...

Recent developments in comprehensive two-dimensional gas chromatography (GC X GC) I. Introduction and instrumental set-up

NARCIS (Netherlands)

Adahchour, M.; Beens, J.; Vreuls, R.J.J.; Brinkman, U.A.T.

2006-01-01

We review the literature on comprehensive two-dimensional gas chromatography (GC × GC), emphasizing developments in the period 2003-2005. The review opens with a general introduction, the principles of the technique and the set-up of GC × GC systems. It also discusses theoretical aspects, trends in

Immunotherapy of HIV-infected patients with Gc protein-derived macrophage activating factor (GcMAF).

Science.gov (United States)

Yamamoto, Nobuto; Ushijima, Naofumi; Koga, Yoshihiko

2009-01-01

Serum Gc protein (known as vitamin D3-binding protein) is the precursor for the principal macrophage activating factor (MAF). The MAF precursor activity of serum Gc protein of HIV-infected patients was lost or reduced because Gc protein is deglycosylated by alpha-N-acetylgalactosaminidase (Nagalase) secreted from HIV-infected cells. Therefore, macrophages of HIV-infected patients having deglycosylated Gc protein cannot be activated, leading to immunosuppression. Since Nagalase is the intrinsic component of the envelope protein gp120, serum Nagalase activity is the sum of enzyme activities carried by both HIV virions and envelope proteins. These Nagalase carriers were already complexed with anti-HIV immunoglobulin G (IgG) but retained Nagalase activity that is required for infectivity. Stepwise treatment of purified Gc protein with immobilized beta-galactosidase and sialidase generated the most potent macrophage activating factor (termed GcMAF), which produces no side effects in humans. Macrophages activated by administration of 100 ng GcMAF develop a large amount of Fc-receptors as well as an enormous variation of receptors that recognize IgG-bound and unbound HIV virions. Since latently HIV-infected cells are unstable and constantly release HIV virions, the activated macrophages rapidly intercept the released HIV virions to prevent reinfection resulting in exhaustion of infected cells. After less than 18 weekly administrations of 100 ng GcMAF for nonanemic patients, they exhibited low serum Nagalase activities equivalent to healthy controls, indicating eradication of HIV-infection, which was also confirmed by no infectious center formation by provirus inducing agent-treated patient PBMCs. No recurrence occurred and their healthy CD + cell counts were maintained for 7 years.

Effect of the Gc-derived macrophage-activating factor precursor (preGcMAF) on phagocytic activation of mouse peritoneal macrophages.

Science.gov (United States)

Uto, Yoshihiro; Yamamoto, Syota; Takeuchi, Ryota; Nakagawa, Yoshinori; Hirota, Keiji; Terada, Hiroshi; Onizuka, Shinya; Nakata, Eiji; Hori, Hitoshi

2011-07-01

The 1f1f subtype of the Gc protein (Gc(1f1f) protein) was converted into Gc-derived macrophage-activating factor (GcMAF) by enzymatic processing in the presence of β-galactosidase of an activated B-cell and sialidase of a T-cell. We hypothesized that preGc(1f1f)MAF, the only Gc(1f1f) protein lacking galactose, can be converted to GcMAF in vivo because sialic acid is cleaved by residual sialidase. Hence, we investigated the effect of preGc(1f1f)MAF on the phagocytic activation of mouse peritoneal macrophages. We examined the sugar moiety of preGc(1f1f)MAF with a Western blot using peanut agglutinin (PNA) and Helix pomatia agglutinin (HPA) lectin. We also found that preGc(1f1f)MAF significantly enhanced phagocytic activity in mouse peritoneal macrophages but only in the presence of the mouse peritoneal fluid; the level of phagocytic activity was the same as that observed for GcMAF. PreGc(1f1f)MAF can be used as an effective macrophage activator in vivo.

Degradação de poliolefinas utilizando catalisadores zeolíticos Degradation of polyolefins using zeolitic catalysts

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Maria Letícia M. Valle

2004-03-01

Full Text Available Neste trabalho foi estudada a degradação de alguns dos principais constituintes dos rejeitos plásticos (polietileno de alta densidade (HDPE, polietileno de baixa densidade (LDPE e polipropileno (PP, empregando-se um catalisador exausto de unidades de craqueamento de fluidos (FCC e um catalisador zeolítico (ADZ3 sintetizado em laboratório. Utilizando técnicas de termogravimetria (TG-DTG e cromatografia gasosa (CG, foi possível avaliar os produtos gerados no craqueamento destas poliolefinas. Na degradação catalítica de poliolefinas com catalisadores zeolíticos, verificou-se a obtenção preferencial de gasolina, GLP e diesel, produtos importantes na matriz energética brasileira. O catalisador de FCC exausto foi mais seletivo para a produção de gasolina e GLP, enquanto que a produção de diesel foi mais favorecida com o catalisador ADZ3.In this work the degradation of some of the main plastics responsible for waste, viz. high density polyethylene (HDPE, low density polyethylene (LDPE and polypropylene (PP, was studied using a spent FCC catalyst (fluid cracking catalyst and a zeolitic catalyst (ADZ3 synthesized in laboratory. Using thermogravimetry (TG-DTG and gas chromatography (GC techniques, it was possible to evaluate the products from these polyolefins cracking. The catalytic degradation of polyolefins led to a preferential production of LPG, diesel and gasoline, which are important products of the Brazilian energetic matrix. The spent FCC catalyst was more selective for production of LPG and gasoline, whereas the diesel production was more favored with the ADZ3 catalyst.

Yield and chemical composition of essential oil of the chamomile [Chamomilla recutita (L. Raeuchert] extracted for steam distillation/ Rendimento e composição química do óleo essencial da camomila [Chamomilla recutita (L. Rauschert] extraído por arraste de vapor d’água, em escala comercial

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Edmilson Cezar Paglia

2008-08-01

Full Text Available The distillation process was periodically monitored, on Campo Largo-PR, in “CHAMEL Ind. e Com. De Produtos Naturais LTDA.”, in the 2005 harvest. The hydrodistillation and GC-MS analyses were done in the UFPR Laboratories. The obtained data indicate that the chamomile essential oil extracted through the distiller model used presented low quality. Great part of the essential oil, besides their main components, it was being lost with the hidrolato. In the distillation process the periodic evaluation of quality and efficiency indicators is indispensable to establish appropriate operational conditions.Com o objetivo de avaliar o rendimento e a composição química do óleo essencial de camomila submetida a um sistema de extração por arraste de vapor, em escala comercial, monitorou-se periodicamente o processo realizado, no município de Campo Largo – PR, num modelo utilizado pela “CHAMEL Ind. E Com. de Produtos Naturais Ltda.”, na safra de 2005. As determinações analíticas foram realizadas em laboratórios da UFPR, por meio da hidrodestilação e cromatografia gasosa acoplada à espectrometria de massas. Os dados obtidos indicam que o óleo essencial da camomila extraído por meio do modelo de destilador utilizado apresentou qualidade aquém das expectativas. Grande parte do óleo essencial, inclusive seus principais componentes, estava sendo perdida junto ao hidrolato. No processo de destilação o monitoramento periódico de indicadores de qualidade e de eficiência é imprescindível para estabelecer condições adequadas de operacionalização.

Intra-genomic GC heterogeneity in sauropsids: evolutionary insights from cDNA mapping and GC3 profiling in snake

Science.gov (United States)

2012-01-01

Background Extant sauropsids (reptiles and birds) are divided into two major lineages, the lineage of Testudines (turtles) and Archosauria (crocodilians and birds) and the lineage of Lepidosauria (tuatara, lizards, worm lizards and snakes). Karyotypes of these sauropsidan groups generally consist of macrochromosomes and microchromosomes. In chicken, microchromosomes exhibit a higher GC-content than macrochromosomes. To examine the pattern of intra-genomic GC heterogeneity in lepidosaurian genomes, we constructed a cytogenetic map of the Japanese four-striped rat snake (Elaphe quadrivirgata) with 183 cDNA clones by fluorescence in situ hybridization, and examined the correlation between the GC-content of exonic third codon positions (GC3) of the genes and the size of chromosomes on which the genes were localized. Results Although GC3 distribution of snake genes was relatively homogeneous compared with those of the other amniotes, microchromosomal genes showed significantly higher GC3 than macrochromosomal genes as in chicken. Our snake cytogenetic map also identified several conserved segments between the snake macrochromosomes and the chicken microchromosomes. Cross-species comparisons revealed that GC3 of most snake orthologs in such macrochromosomal segments were GC-poor (GC3 < 50%) whereas those of chicken orthologs in microchromosomes were relatively GC-rich (GC3 ≥ 50%). Conclusion Our results suggest that the chromosome size-dependent GC heterogeneity had already occurred before the lepidosaur-archosaur split, 275 million years ago. This character was probably present in the common ancestor of lepidosaurs and but lost in the lineage leading to Anolis during the diversification of lepidosaurs. We also identified several genes whose GC-content might have been influenced by the size of the chromosomes on which they were harbored over the course of sauropsid evolution. PMID:23140509

Trocas gasosas e conteúdo de carboidratos e compostos nitrogenados em pinhão-manso irrigado com águas residuária e salina

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Antonio Evami Cavalcante Sousa

2012-10-01

Full Text Available O objetivo deste trabalho foi avaliar alterações nas trocas gasosas e nos conteúdos de carboidratos e compostos nitrogenados, em pinhão-manso (Jatropha curcas irrigado com águas residuária e salina. Empregou-se o delineamento em blocos ao acaso, com quatro tratamentos e quatro repetições: irrigação plena com água de abastecimento a 0,6 dS m-1 (controle; irrigação plena com água salinizada a 2,4 dS m-1 (SAL; e irrigação com água residuária de esgoto, plena (R100 e a 50% da capacidade de campo (R50. O tratamento R50 reduziu fortemente as trocas gasosas e a área foliar, comparado ao controle, seguido pelos tratamentos SAL e R100. A redução na fotossíntese diminuiu o nível de sacarose nas folhas, nos quatro tratamentos. Os teores de açúcares solúveis aumentaram nos tratamentos R50, SAL e R100, enquanto o conteúdo de amido permaneceu praticamente inalterado. Os conteúdos de prolina e glicina betaína aumentaram nos três tratamentos, mas a última foi mais importante, em termos quantitativos, como protetor celular e osmótico. A irrigação plena com água residuária induz efeitos similares aos causados pela irrigação com água salina. A irrigação limitada com água residuária causa estresse agudo às plantas, provavelmente pela combinação de deficiência hídrica e acúmulo de solutos no solo.

Identificação de δ tocotrienol e de ácidos graxos no óleo fixo de urucum (Bixa orellana Linné

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C.K. Costa

2013-01-01

Full Text Available Bixa orellana é uma planta nativa do Brasil, conhecida popularmente como urucum. O objetivo desse estudo foi extrair o óleo das sementes de B. orellana e, a partir dele, isolar e identificar o tocotrienol e quantificar seus ácidos graxos. A extração do óleo realizou-se em aparelho Soxhlet utilizando hexano como solvente extrator. O tocotrienol foi isolado por meio de métodos cromatográficos e identificado por espectrometria de ressonância magnética nuclear RMN ¹H e RMN 13C. Os ácidos graxos foram quantificados por cromatografia gasosa acoplada ao espectrômetro de massa. Os resultados demonstraram a presença de δ -tocotrienol e, dentre os ácidos graxos, a ocorrência do ácido aracdônico, que até o presente momento não havia sido relatada na espécie em estudo.

Análise dos óleos essenciais de três espécies de Piper coletadas na região do Distrito Federal (Cerrado e comparação com óleos de plantas procedentes da região de Paraty, RJ (Mata Atlântica

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Miriam Cristina Leone Potzernheim

Full Text Available Foi determinada a composição química dos óleos essenciais de 3 espécies do gênero Piper coletadas em Matas de Galeria no Cerrado, e comparada com composição dos óleos das mesmas espécies oriundas da Mata Atlântica. A composição química do óleo de Piper arboreum subsp arboreum, P. dilatatum e P. hispidum foi determinada por cromatografia gasosa em coluna capilar HP-5 e espectrometria de massas. As três espécies do Cerrado apresentaram predominância de sesquiterpenos. Piper arboreum subsp arboreum apresentou como constituintes majoritários biciclogermacreno (12,1%, 10-epi-g-eudesmol (11,6% e óxido de cariofileno (10,1%. Em P. dilatatum os constituintes em maior quantidade foram cis-b-ocimeno (19,6% e b-cariofileno (11,3% e em P. hispidum foram b-pineno (19,7%, a-pineno (9,0%.

Pirólise de resíduos poliméricos gerados por atividades offshore Pyrolysis of offshore solid wastes

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Mara L. de Oliveira

2009-01-01

Full Text Available Resíduos plásticos gerados pelas atividades offshore da indústria de exploração e produção de óleo e gás, após caracterização por ensaio de identificação das classes poliméricas e análise térmica, foram pirolisados em atmosfera inerte a 450 °C. Os óleos pirolíticos foram caracterizados por espectrofotometria de infravermelho por transformada de Fourier (FTIR e cromatografia em fase gasosa acoplada à espectrometria de massas (CG/EM, indicando a composição de parafinas, olefinas e aromáticos.Solid wastes from oil and gas offshore exploration and production activities, after characterization of polymeric classes and thermal identification analysis tests, were pyrolysed under an inert atmosphere at 450 °C. The pyrolysis oil was characterized by Fourier Transform Infrared Spectroscopy (FTIR gas chromatography mass spectrometry (CG/EM, indicating high generation of paraffin, olefines and aromatics.

Media components and amino acid supplements influencing the production of fruity aroma by Geotrichum candidum Influência da composição do meio de cultivo e da suplementação com aminoácidos na produção de aroma frutal por Geotrichum candidum

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T. Pinotti

2006-12-01

Full Text Available The ability of Geotrichum candidum to produce fruity aroma in food grade sucrose, molasses, corn steep liquor and peptone based culture media was tested by sensory evaluation and analyzed by gas chromatography mass spectrometry. A strong and sweet fruity aroma was produced from molasses, with peptone or corn steep liquor stimulating aroma production. Molasses with peptone supplemented with leucine, valine, or alanine yielded better fruity aroma production and the presence of many esters was consistent with the fruity aroma production.Geotrichum candidum foi cultivado em diversos meios de cultura contendo sacarose ou melaço e milhocina ou peptona e a produção de aroma frutal foi verificada através de avaliação sensorial e cromatografia gasosa acoplada a espectrometria de massas. Os meios contendo melaço, peptona e leucina, valina ou alanina apresentaram os melhores resultados e a presença de diversos ésteres foi consistente com a formação de aroma frutal.

Constituintes químicos voláteis e não-voláteis de Moringa oleifera Lam., Moringaceae

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Milena B. Barreto

Full Text Available O estudo fitoquímico do extrato etanólico das folhas de Moringa oleifera Lam., Moringaceae, resultou no isolamento dos derivados benzilnitrilas niazirina, niazirinina e 4-hidroxifenil-acetonitrila, enquanto que das cascas dos frutos somente o octacosano foi obtido. Os óleos essenciais das folhas, flores e frutos foram analisados por cromatografia gasosa acoplada a espectrometria de massa. Os constituintes principais identificados foram: fitol (21,6% e timol (9,6% nas folhas, octadecano (27,4% e ácido hexadecanóico (18,4% nas flores e docosano (32,7% e tetracosano (24,0% nos frutos. As estruturas dos compostos isolados foram identificadas a partir de técnicas espectroscópicas (RMN, IV e EM. A 4-hidroxifenil-acetonitrila está sendo citada pela primeira vez para o gênero Moringa e os óleos essenciais das flores e frutos estão sendo citados pela primeira vez para a espécie M. oleifera.

Mutational Biases and GC-Biased Gene Conversion Affect GC Content in the Plastomes of Dendrobium Genus

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Zhitao Niu

2017-11-01

Full Text Available The variation of GC content is a key genome feature because it is associated with fundamental elements of genome organization. However, the reason for this variation is still an open question. Different kinds of hypotheses have been proposed to explain the variation of GC content during genome evolution. However, these hypotheses have not been explicitly investigated in whole plastome sequences. Dendrobium is one of the largest genera in the orchid species. Evolutionary studies of the plastomic organization and base composition are limited in this genus. In this study, we obtained the high-quality plastome sequences of D. loddigesii and D. devonianum. The comparison results showed a nearly identical organization in Dendrobium plastomes, indicating that the plastomic organization is highly conserved in Dendrobium genus. Furthermore, the impact of three evolutionary forces—selection, mutational biases, and GC-biased gene conversion (gBGC—on the variation of GC content in Dendrobium plastomes was evaluated. Our results revealed: (1 consistent GC content evolution trends and mutational biases in single-copy (SC and inverted repeats (IRs regions; and (2 that gBGC has influenced the plastome-wide GC content evolution. These results suggest that both mutational biases and gBGC affect GC content in the plastomes of Dendrobium genus.

Mutational Biases and GC-Biased Gene Conversion Affect GC Content in the Plastomes of Dendrobium Genus

Science.gov (United States)

Niu, Zhitao; Xue, Qingyun; Wang, Hui; Xie, Xuezhu; Zhu, Shuying; Liu, Wei; Ding, Xiaoyu

2017-01-01

The variation of GC content is a key genome feature because it is associated with fundamental elements of genome organization. However, the reason for this variation is still an open question. Different kinds of hypotheses have been proposed to explain the variation of GC content during genome evolution. However, these hypotheses have not been explicitly investigated in whole plastome sequences. Dendrobium is one of the largest genera in the orchid species. Evolutionary studies of the plastomic organization and base composition are limited in this genus. In this study, we obtained the high-quality plastome sequences of D. loddigesii and D. devonianum. The comparison results showed a nearly identical organization in Dendrobium plastomes, indicating that the plastomic organization is highly conserved in Dendrobium genus. Furthermore, the impact of three evolutionary forces—selection, mutational biases, and GC-biased gene conversion (gBGC)—on the variation of GC content in Dendrobium plastomes was evaluated. Our results revealed: (1) consistent GC content evolution trends and mutational biases in single-copy (SC) and inverted repeats (IRs) regions; and (2) that gBGC has influenced the plastome-wide GC content evolution. These results suggest that both mutational biases and gBGC affect GC content in the plastomes of Dendrobium genus. PMID:29099062

β-Galactosidase treatment is a common first-stage modification of the three major subtypes of Gc protein to GcMAF.

Science.gov (United States)

Uto, Yoshihiro; Yamamoto, Syota; Mukai, Hirotaka; Ishiyama, Noriko; Takeuchi, Ryota; Nakagawa, Yoshinori; Hirota, Keiji; Terada, Hiroshi; Onizuka, Shinya; Hori, Hitoshi

2012-06-01

The 1f1f subtype of the group-specific component (Gc) protein is converted into Gc protein-derived macrophage-activating factor (GcMAF) by enzymatic processing with β-galactosidase and sialidase. We previously demonstrated that preGc(1f1f)MAF, a full Gc(1f1f) protein otherwise lacking a galactosyl moiety, can be converted to GcMAF by treatment with mouse peritoneal fluid. Here, we investigated the effects of the β-galactosidase-treated 1s1s and 22 subtypes of Gc protein (preGc(1s1s)MAF and preGc₂₂MAF) on the phagocytic activation of mouse peritoneal macrophages. We demonstrated the presence of Gal-GalNAc disaccharide sugar structures in the Gc(1s1s) protein by western blotting using peanut agglutinin and Helix pomatia agglutinin lectin. We also found that preGc(1s1s)MAF and preGc₂₂MAF significantly enhanced the phagocytic activity of mouse peritoneal macrophages in the presence and absence of mouse peritoneal fluid. We demonstrate that preGc(1s1s)MAF and preGc₂₂MAF proteins can be used as effective macrophage activators.

Admission levels of serum Gc-globulin

DEFF Research Database (Denmark)

Schiødt, F V; Bondesen, S; Petersen, I

1996-01-01

Gc-globulin scavenges actin released from necrotic hepatocytes to the extracellular space. In 77 patients with fulminant hepatic failure (FHF) (excluding patients treated with liver transplantation), admission levels of serum Gc-globulin and degree of complexing with monomeric actin (complex ratio...... in the same range as the KCH criteria. An advantage of Gc-globulin is that it gives an estimate of the outcome already on admission. Acute liver transplantation should be considered in FHF patients with Gc-globulin less than 100 mg/L....

Separation of fatty acid methyl esters by GC-online hydrogenation × GC.

Science.gov (United States)

Delmonte, Pierluigi; Fardin-Kia, Ali Reza; Rader, Jeanne I

2013-02-05

The separation of fatty acid methyl esters (FAME) provided by a 200 m × 0.25 mm SLB-IL111 capillary column is enhanced by adding a second dimension of separation ((2)D) in a GC × GC design. Rather than employing two GC columns of different polarities or using different elution temperatures, the separation in the two-dimensional space is achieved by altering the chemical structure of selected analytes between the two dimensions of separation. A capillary tube coated with palladium is added between the first dimension of separation ((1)D) column and the cryogenic modulator, providing the reduction of unsaturated FAMEs to their fully saturated forms. The (2)D separation is achieved using a 2.5 m × 0.10 mm SLB-IL111 capillary column and separates FAMEs based solely on their carbon skeleton. The two-dimensional separation can be easily interpreted based on the principle that all the saturated FAMEs lie on a straight diagonal line bisecting the separation plane, while the FAMEs with the same carbon skeleton but differing in the number, geometric configuration or position of double bonds lie on lines parallel to the (1)D time axis. This technique allows the separation of trans fatty acids (FAs) and polyunsaturated FAs (PUFAs) in a single experiment and eliminates the overlap between PUFAs with different chain lengths. To our knowledge, this the first example of GC × GC in which a chemical change is instituted between the two dimensions to alter the relative retentions of components and identify unsaturated FAMEs.

Resíduos de anabolizantes na produção animal: importância e métodos de detecção Anabolic residues in livestock prodution: relevancy and detection methods

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Keila Maria Roncato Duarte

2002-08-01

Full Text Available Com o desenvolvimento da indústria farmacêutica e o conseqüente surgimento de novas substâncias promotoras do crescimento animal, o setor agropecuário necessita de tecnologias cada vez mais eficientes e sensíveis para detectar possíveis resíduos deixados por este vasto número de substâncias anabolizantes, principalmente esteróides com atividades estrogênicas, androgênicas e progestogênicas. Tais substâncias, quando presentes na carne, gordura, ovos, entre outros, podem ser detectadas e quantificadas por uma série de métodos, dentre os quais, descrevemos os cromatográficos, baseados principalmente em cromatografia gasosa acoplada à espectrometria de massa (CG-EM, cromatografia líquida de alta eficiência (CLAE, cromatografia em camada delgada de alta eficiência (CCDAE e os métodos imunológicos, como radioomunoensaio (RIA e ensaio imunoenzimático (ELISA. Estes métodos têm como vantagens o elevado número de amostras que podem ser analisadas por período de tempo, aliadas à alta sensibilidade na detecção de resíduos.With the development of the pharmaceutical industry, and consequently appearance of new substances which promote animal growth, the agricultural sector needs technologies more and more efficient and sensitive to detect possible residues left by this vast number of anabolic substances, mainly steroids with estrogenic, androgenic and progesterogenics activities. Such substances, when present in meat, fat, and eggs among others, can be detected and quantified by a series of methods, among the ones which we described the chromatographic methods, based mainly on gaseous chromatography coupled to the mass espectrometry (CG-MS, high performance liquid chromatography (HPLC, thin layer chromatography (HPTLC and the immunological methods, as radioimmunoassay (RIA and enzyme linked immunosorbent assay (ELISA. These methods have as advantages the high number of samples that can be analyzed by period of time, toghether

Is chondroitin sulfate responsible for the biological effects attributed to the GC protein-derived Macrophage Activating Factor (GcMAF)?

Science.gov (United States)

Ruggiero, Marco; Reinwald, Heinz; Pacini, Stefania

2016-09-01

We hypothesize that a plasma glycosaminoglycan, chondroitin sulfate, may be responsible for the biological and clinical effects attributed to the Gc protein-derived Macrophage Activating Factor (GcMAF), a protein that is extracted from human blood. Thus, Gc protein binds chondroitin sulfate on the cell surface and such an interaction may occur also in blood, colostrum and milk. This interpretation would solve the inconsistencies encountered in explaining the effects of GcMAF in vitro and in vivo. According to our model, the Gc protein or the GcMAF bind to chondroitin sulfate both on the cell surface and in bodily fluids, and the resulting multimolecular complexes, under the form of oligomers trigger a transmembrane signal or, alternatively, are internalized and convey the signal directly to the nucleus thus eliciting the diverse biological effects observed for both GcMAF and chondroitin sulfate. Copyright © 2016 Elsevier Ltd. All rights reserved.

On-line LC-GC and comprehensive two-dimensional LCxGC-ToF MS for the analysis of complex samples

Energy Technology Data Exchange (ETDEWEB)

Janssen, Hans-Gerd [Central Analytical Science, Unilever Research and Development, P.O. Box 114, 3130 AC, Vlaardingen (Netherlands); Koning, Sjaak de [Separation Science Group, LECO Instrumente GmbH, Marie-Bernays-Ring 31, 41199, Moenchengladbach (Germany); Brinkman, Udo A.Th. [Department of Analytical Chemistry and Applied Spectroscopy, Free University, De Boelelaan 1083, 1081 HV, Amsterdam (Netherlands)

2004-04-01

LC x GC is a logical extension of LC-GC. Unlike LC-GC, which only allows detailed analysis of one group of analytes from a complex sample, LC x GC enables detailed mapping of the entire sample. Due to the high degree of orthogonality and the complementary nature of the two dimensions, the method has a very high resolving power. Comprehensive LC x GC chromatograms often show ordered structures which allow group-wise integration as well as detailed target compound analysis. Hyphenation with mass spectrometry is straightforward, which further widens the application range of the technique. (orig.)

NOVAS APLICAÇÕES DE SISTEMAS SFE" HOME MADE".: II. PLANTAS DA AMÉRICA DO SUL

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Fernando M. LANÇAS

1997-12-01

Full Text Available O Laboratório de Cromatografia do IQSC-USP tem desenvolvido pesquisas em conjunto com outros grupos de pesquisa do Brasil e da América Latina, visando a futura implantação da SFE (extração com fluido supercrítico nestes laboratórios. No presente trabalho, apresenta-se alguns dos resultados obtidos na cooperação com pesquisadores do Chile e da Venezuela, direcionados para a SFE de substâncias de potencial interesse econômico, princípios ativos ou substâncias tóxicas: triglicerídeos, ácidos graxos, flavonóides, alcalóides, etc. Foram estudadas plantas nativas do Chile e da Venezuela, algumas delas nunca estudadas por métodos fitoquímicos convencionais e pertencentes a várias famílias vegetais: Leguminosae, Chrysobalanaceae, Annonnaceae, etc. O uso da SFE em conjunto com CGAR-EM (cromatografia gasosa de alta resolução - espectrometria de massas ou CLAE-DAD (cromatografia líquida de alta eficiência com detector" photodiodearray" permitiu a identificação de algumas substâncias presentes em baixa concentração, a partir de pequenas quantidades de material vegetal; estes dados são de grande importância para a caracterização química das espécies estudadas.Further applications of "home made" SFE systems. II. South American plants. The Laboratório de Cromatografia, IQSC-USP, has been developing joint research projects with other research groups from Brazil and Latin America, aiming a future implementation of SFE (supercritical fluid extraction in these laboratories. In the present work, some of the results obtained in the cooperation with researchers from Chile and Venezuela, focused to SFE of potential economical interest compounds, active compounds or toxic molecules, are presented: triglycerides, fatty acids, flavonoids, alkaloids, etc. Native plants from Chile and Venezuela, belonging to several families (Leguminosae, Chrysobalanaceae, Annonnaceae, etc. were studied, some of them never studied by conventional

Análise de ácidos graxos não-esterificados de plasma humano por cromatografia gasosa capilar com injeção sem divisão de fluxo Analysis of non-esterified fatty acids in human plasma by capillary gas-chromatography with splitless injection

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Jacqueline G. Ney

2004-08-01

Full Text Available The aim of the present work was to test the combination of non-esterified fatty acid (NEFA isolation using fumed silicon dioxide with capillary gas-chromatography (C-GC with splitless injection for the analysis of NEFAs in human plasma. Injection volume, solvent re-condensation and split purge flow-rate were the parameters evaluated for the analysis of fatty acid methyl esters by C-GC. The use of a solvent re-condensation technique, associated with 1.0 µL injection and a split purge flow rate of 80 mL/min resulted in satisfactory analysis of NEFAs. Fourteen fatty acids were identified in plasma samples, ranging from 2.03 to 184.0 µmol/L. The combination of both techniques proved useful for routine analyses of plasma NEFAs.

Modern methods of sample preparation for GC analysis

NARCIS (Netherlands)

de Koning, S.; Janssen, H.-G.; Brinkman, U.A.Th.

2009-01-01

Today, a wide variety of techniques is available for the preparation of (semi-) solid, liquid and gaseous samples, prior to their instrumental analysis by means of capillary gas chromatography (GC) or, increasingly, comprehensive two-dimensional GC (GC × GC). In the past two decades, a large number

Efeito da fertilização nitrogenada em videira sobre a formação de alguns compostos volatéis no vinho Effect of vineyard nitrogen fertilization on the formation of some wine volatile coumpounds

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Lúcia Schuch Boeira

1995-01-01

Full Text Available Vitis vinifera cv. Gewürztraminer e Cabemet Sauvignon cultivadas em Santana do Livramento e Garibaldi foram submetidas a diferentes tratamentos nitrogenados realizados durante o período vegetativo de 1992-1993. Após a colheita e esmagamento o mosto obtido foi dividido em quatro lotes e fermentado com diferentes leveduras. As determinações dos compostos voláteis foram realizados através de cromatografia gasosa. Maiores valores de metanol foram encontrados nos vinhos de Cabemet Sauvignon (máximo 225,6mg/l. A fertilização nitrogenada provocou um aumento na concentração (mg/l de propanol-1 (min. 25 -máx. 78,2 e uma diminuição de metil-2 propanol-1 (min. 60,8 - máx. 125,9 e metil-3 + metil-2 butanol-1 (min. 85,8 - máx. 407,8 nos vinhos. Os álcoois superiores apresentaram também diferenças em relação à região, cultivar e levedura utilizada.Vitis vinifera Gewürztraminer (white variety and Cabemet Sauvignon (red growned in Santana do Livramento, RS, and Garibaldi, RS, were added with different nitrogen treatments in the vineyard during me 1992-1993 season. After harvest and crushing, the musts were divided into four lots each one added with a different yeast. The volatiles were analyzed through GC. Maximum amount of methanol was found with the red variety (225.6mg/l. Increasing nitrogen in the soil increased (mg/l propanol-1 (min. 25-max. 78.2 and decreased methyl-2 propanol-1 (min. 60.8-max. 125.9 and methyl-3+methyl-2 butanol-1 (min. 85.8-max. 407.8. The fusel alcohol fraction showed, also, differences between region,grape variety and yeast used.

Chemical characterization and antimicrobial activity of essential oils of salvia L. species Caracterização química e atividade antimicrobiana de óleos essenciais de distintas espécies de salvia L.

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Morgana Karen Pierozan

2009-12-01

Full Text Available In this work, the essential oils of S. officinalis, S. sclarea, S. lavandulifolia and S. triloba were chemically analyzed by gas chromatography coupled to a mass spectrometry detector (GC/MSD, and their antimicrobial activity was tested against 10 microorganisms using the disk diffusion method and the Minimum Inhibitory Concentration (MIC technique. The following major compounds were identified in the essential oils: α - and β-thujone, camphor and 1,8-cineole, except in S. sclarea, where linalool, linalyl acetate and α-terpineol were the major constituents. The antimicrobial activity showed significant differences (p Neste trabalho os óleos essenciais de S. officinalis, S. sclarea, S. lavandulifolia e Salvia sp. foram analisados quimicamente por cromatografia gasosa acoplada a espectrômetro de massas. A atividade antimicrobiana dos óleos essenciais foi testada contra 10 microrganismos utilizando o método de difusão em discos e através da determinação da Concentração Inibitória Mínima (CIM. Cânfora, α - e ß-thujone e 1,8-cineol foram os compostos majoritários identificados na maioria dos óleos essenciais, exceto para S. sclarea, em que linalol, acetato de linalil e α-terpineol foram os compostos majoritários identificados. As atividades antimicrobianas apresentaram diferenças significativas (p < 0,05 somente quando obtidas pelo método CIM. Microorganismos gram-positivos apresentaram grande sensibilidade para os óleos essenciais. A menor CIM foi observada para o Staphylococcus aureus quando exposto a 2,31 mg.mL-1 de óleo essencial de S. lavandulifolia, enquanto que a maior CIM foi observada para Shigella flexneri exposta a 9,25 mg.mL-1 do mesmo óleo essencial, provando que este óleo constitui-se em um eficiente agente bacteriostático contra microrganismos gram-positivos.

Evaluation of volatiles from two subtropical strawberry cultivars using GC-olfactometry, GC-MS odor activity values, and sensory analysis

Science.gov (United States)

Flavor profiles of two Florida strawberry cultivars were determined using GC-olfactometry,GC-MS, odor activity values (OAVs) and sensory analysis. Thirty-six aroma active compounds were detected using GC-O. Thirty-four were identified. The major odor-active compounds in decreasing intensity were: me...

At least two Fc Neu5Gc residues of monoclonal antibodies are required for binding to anti-Neu5Gc antibody.

Science.gov (United States)

Yu, Chuanfei; Gao, Kai; Zhu, Lei; Wang, Wenbo; Wang, Lan; Zhang, Feng; Liu, Chunyu; Li, Meng; Wormald, Mark R; Rudd, Pauline M; Wang, Junzhi

2016-01-29

Two non-human glycan epitopes, galactose-α-1,3-galactose (α-gal) and Neu5Gc-α-2-6-galactose (Neu5Gc) have been shown to be antigenic when attached to Fab oligosaccharides of monoclonal antibodies (mAbs) , while α-gal attached to Fc glycans was not. However, the antigenicity of Neu5Gc on the Fc glycans remains unclear in the context that most mAbs carry only Fc glycans. After studying two clinical mAbs carrying significant amounts of Fc Neu5Gc, we show that their binding activity with anti-Neu5Gc antibody resided in a small subset of mAbs carrying two or more Fc Neu5Gc, while mAbs harboring only one Neu5Gc showed no reactivity. Since most Neu5Gc epitopes were distributed singly on the Fc of mAbs, our results suggest that the potential antigenicity of Fc Neu5Gc is low. Our study could be referenced in the process design and optimization of mAb production in murine myeloma cells and in the quality control of mAbs for industries and regulatory authorities.

Accumulation of GC donor splice signals in mammals

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Koonin Eugene V

2008-07-01

Full Text Available Abstract The GT dinucleotide in the first two intron positions is the most conserved element of the U2 donor splice signals. However, in a small fraction of donor sites, GT is replaced by GC. A substantial enrichment of GC in donor sites of alternatively spliced genes has been observed previously in human, nematode and Arabidopsis, suggesting that GC signals are important for regulation of alternative splicing. We used parsimony analysis to reconstruct evolution of donor splice sites and inferred 298 GT > GC conversion events compared to 40 GC > GT conversion events in primate and rodent genomes. Thus, there was substantive accumulation of GC donor splice sites during the evolution of mammals. Accumulation of GC sites might have been driven by selection for alternative splicing. Reviewers This article was reviewed by Jerzy Jurka and Anton Nekrutenko. For the full reviews, please go to the Reviewers' Reports section.

Identification (GC and GC-MS) of unsaturated acetates in Elasmopalpus lignosellus and their biological activity (GC-EAD and EAG).

Science.gov (United States)

Jham, Gulab N; da Silva, Alexsandro A; Lima, Eraldo R; Viana, Paulo

2005-02-01

Two insect colonies of Elasmopalpus lignosellus were reared in our laboratory, the first being initiated from pupae obtained from a cornfield in the region of Sete Lagoas, Minas Gerais and the second from a cornfield in the region of Goiânia, Goiás. From the two colonies, two extracts were prepared from the pheromone glands of virgin E. lignosellus females. The extract obtained from the first colony was designated as extract 1 while the extract obtained from the second colony was designated as extract 2. Extract 1 was analyzed by gas chromatography-mass spectrometry (GC-MS) with (Z)-9-hexadecenyl acetate [(Z)-9-HDA] and (Z)-11-hexadecenyl acetate [(Z)-11-HDA] being identified and confirmed by the formation of DMDS derivatives. In addition, a third acetate, which could be either (E)-8-hexadecenyl acetate [(E)-8-HDA] or (E)-9-hexadecenyl acetate [(E)-9-HDA] was detected by GC-MS. Extract 2 was analyzed by gas chromatography (GC) and gas chromatography-electroannetography (GC-EAD) revealing the presence of (Z)-11-HDA and (Z)-9-TDA. In addition, the same compounds elicited a response with the E. lignosellus male antenna obtained from the second insect colony. Electroantennography (EAG) screening with the male E. lignosellus antenna (obtained from the second insect colony) was conducted with the 23 possible tetradecenyl acetates (TDA) and 22 hexadecenyl acetates (HDA) as standards. Out of the 23 TDA isomers evaluated, only (Z)-9-TDA elicited a response and out of the 22 HDA [(Z) and (E) isomers gamma2 to delta13] evaluated only (Z)-11-HDA elicited a response. The acetate compositions of two extracts obtained from insects originating from the two states (Minas Gerais and Goiás) of Brazil were different from one another as well as from that obtained from insects in Tifton, GA, USA. The bioactivity data (GC-EAD) of the extract 2 differed from those reported for the Tifton, GA, USA population. These data suggest polymorphism in relation to the insect populations found in

The GC-heterogeneity of teleost fishes

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Gautier Christian

2008-12-01

Full Text Available Abstract Background One of the most striking features of mammalian and birds chromosomes is the variation in the guanine-cytosine (GC content that occurs over scales of hundreds of kilobases to megabases; this is known as the "isochore" structure. Among other vertebrates the presence of isochores depends upon the taxon; isochore are clearly present in Crocodiles and turtles but fish genome seems very homogeneous on GC content. This has suggested a unique isochore origin after the divergence between Sarcopterygii and Actinopterygii, but before that between Sauropsida and mammals. However during more than 30 years of analysis, isochore characteristics have been studied and many important biological properties have been associated with the isochore structure of human genomes. For instance, the genes are more compact and their density is highest in GC rich isochores. Results This paper shows in teleost fish genomes the existence of "GC segmentation" sharing some of the characteristics of isochores although teleost fish genomes presenting a particular homogeneity in CG content. The entire genomes of T nigroviridis and D rerio are now available, and this has made it possible to check whether a mosaic structure associated with isochore properties can be found in these fishes. In this study, hidden Markov models were trained on fish genes (T nigroviridis and D rerio which were classified by using the isochore class of their human orthologous. A clear segmentation of these genomes was detected. Conclusion The GC content is an excellent indicator of isochores in heterogeneous genomes as mammals. The segmentation we obtained were well correlated with GC content and other properties associated to GC content such as gene density, the number of exons per gene and the length of introns. Therefore, the GC content is the main property that allows the detection of isochore but more biological properties have to be taken into account. This method allows detecting

Sensitivity of GC-EI/MS, GC-EI/MS/MS, LC-ESI/MS/MS, LC-Ag(+) CIS/MS/MS, and GC-ESI/MS/MS for analysis of anabolic steroids in doping control.

Science.gov (United States)

Cha, Eunju; Kim, Sohee; Kim, Ho Jun; Lee, Kang Mi; Kim, Ki Hun; Kwon, Oh-Seung; Lee, Jaeick

2015-01-01

This study compared the sensitivity of various separation and ionization methods, including gas chromatography with an electron ionization source (GC-EI), liquid chromatography with an electrospray ionization source (LC-ESI), and liquid chromatography with a silver ion coordination ion spray source (LC-Ag(+) CIS), coupled to a mass spectrometer (MS) for steroid analysis. Chromatographic conditions, mass spectrometric transitions, and ion source parameters were optimized. The majority of steroids in GC-EI/MS/MS and LC-Ag(+) CIS/MS/MS analysis showed higher sensitivities than those obtained with other analytical methods. The limits of detection (LODs) of 65 steroids by GC-EI/MS/MS, 68 steroids by LC-Ag(+) CIS/MS/MS, 56 steroids by GC-EI/MS, 54 steroids by LC-ESI/MS/MS, and 27 steroids by GC-ESI/MS/MS were below cut-off value of 2.0 ng/mL. LODs of steroids that formed protonated ions in LC-ESI/MS/MS analysis were all lower than the cut-off value. Several steroids such as unconjugated C3-hydroxyl with C17-hydroxyl structure showed higher sensitivities in GC-EI/MS/MS analysis relative to those obtained using the LC-based methods. The steroids containing 4, 9, 11-triene structures showed relatively poor sensitivities in GC-EI/MS and GC-ESI/MS/MS analysis. The results of this study provide information that may be useful for selecting suitable analytical methods for confirmatory analysis of steroids. Copyright © 2015 John Wiley & Sons, Ltd.

Analysis of intra-genomic GC content homogeneity within prokaryotes

DEFF Research Database (Denmark)

Bohlin, J; Snipen, L; Hardy, S.P.

2010-01-01

the GC content varies within microbial genomes to assess whether this property can be associated with certain biological functions related to the organism's environment and phylogeny. We utilize a new quantity GCVAR, the intra-genomic GC content variability with respect to the average GC content......Bacterial genomes possess varying GC content (total guanines (Gs) and cytosines (Cs) per total of the four bases within the genome) but within a given genome, GC content can vary locally along the chromosome, with some regions significantly more or less GC rich than on average. We have examined how...... both aerobic and facultative microbes. Although an association has previously been found between mean genomic GC content and oxygen requirement, our analysis suggests that no such association exits when phylogenetic bias is accounted for. A significant association between GCVAR and mean GC content...

Comparison of GC/MSD and GC/AED for the determination of organotin compounds in the environment

Energy Technology Data Exchange (ETDEWEB)

Staeb, J.A. (Inst. of Environmental Studies, Free Univ., Amsterdam (Netherlands)); Cofino, W.P. (Inst. of Environmental Studies, Free Univ., Amsterdam (Netherlands)); Hattum, B. van (Inst. of Environmental Studies, Free Univ., Amsterdam (Netherlands)); Brinkman, U.A.T. (Dept. of Analytical Chemistry, Free Univ., Amsterdam (Netherlands))

Methods are described for the analysis of environmental samples like water, sediment and suspended matter for the determination of all organotin compounds (OTs) that are currently used as biocides: Tributyltin (TBT) triphenyltin (TPT), tricyclohexyltin (TCT) and fenbutatin oxide (FBTO). In water also five degradation products (di and mono substituted analogs) can be determined. Alkylation using a Grignard reagent was used to obtain OT derivatives amenable to gas chromatography (GC). Both methylation and pentylation have been employed for derivatization prior to GC analysis. The present results show that derivatization efficiencies for TPT, TCT and FBTO at trace levels are higher using methylation than pentylation. Detection limits for each type of sample matrix were determined using GC/Mass Selective Detection (GC/MSD) and GC/Atomic Emission Detection (AED). In sediment and suspended matter only tri-substituted OTs (i.e. the parent compounds) could be determined. Detection limits ranged from 0.2 to 10 ng/g dry weight. FBTO, not previously detected in environmental samples, was found at levels of 4 and 11 ng/g in a suspended matter sample and a sediment sample, respectively. In water the OTs and their degradation products were determined at levels of 1-10 ng/l (as tin) using 200 ml water samples. (orig.)

Characterisation of middle-distillates by comprehensive two-dimensional gas chromatography (GC x GC): A powerful alternative for performing various standard analysis of middle-distillates.

Science.gov (United States)

Vendeuvre, Colombe; Ruiz-Guerrero, Rosario; Bertoncini, Fabrice; Duval, Laurent; Thiébaut, Didier; Hennion, Marie-Claire

2005-09-09

The detailed characterisation of middle distillates is essential for a better understanding of reactions involved in refining process. Owing to higher resolution power and enhanced sensitivity, comprehensive two-dimensional gas chromatography (GC x GC) is a powerful tool for improving characterisation of petroleum samples. The aim of this paper is to compare GC x GC and various ASTM methods -- gas chromatography (GC), liquid chromatography (LC) and mass spectrometry (MS) -- for group type separation and detailed hydrocarbon analysis. Best features of GC x GC are demonstrated and compared to these techniques in terms of cost, time consumption and accuracy. In particular, a new approach of simulated distillation (SimDis-GC x GC) is proposed: compared to the standard method ASTM D2887 it gives unequal information for better understanding of conversion process.

The Met Office Global Coupled Model 3.0 and 3.1 (GC3.0 and GC3.1) Configurations

Science.gov (United States)

Williams, K. D.; Copsey, D.; Blockley, E. W.; Bodas-Salcedo, A.; Calvert, D.; Comer, R.; Davis, P.; Graham, T.; Hewitt, H. T.; Hill, R.; Hyder, P.; Ineson, S.; Johns, T. C.; Keen, A. B.; Lee, R. W.; Megann, A.; Milton, S. F.; Rae, J. G. L.; Roberts, M. J.; Scaife, A. A.; Schiemann, R.; Storkey, D.; Thorpe, L.; Watterson, I. G.; Walters, D. N.; West, A.; Wood, R. A.; Woollings, T.; Xavier, P. K.

2018-02-01

The Global Coupled 3 (GC3) configuration of the Met Office Unified Model is presented. Among other applications, GC3 is the basis of the United Kingdom's submission to the Coupled Model Intercomparison Project 6 (CMIP6). This paper documents the model components that make up the configuration (although the scientific descriptions of these components are in companion papers) and details the coupling between them. The performance of GC3 is assessed in terms of mean biases and variability in long climate simulations using present-day forcing. The suitability of the configuration for predictability on shorter time scales (weather and seasonal forecasting) is also briefly discussed. The performance of GC3 is compared against GC2, the previous Met Office coupled model configuration, and against an older configuration (HadGEM2-AO) which was the submission to CMIP5. In many respects, the performance of GC3 is comparable with GC2, however, there is a notable improvement in the Southern Ocean warm sea surface temperature bias which has been reduced by 75%, and there are improvements in cloud amount and some aspects of tropical variability. Relative to HadGEM2-AO, many aspects of the present-day climate are improved in GC3 including tropospheric and stratospheric temperature structure, most aspects of tropical and extratropical variability and top-of-atmosphere and surface fluxes. A number of outstanding errors are identified including a residual asymmetric sea surface temperature bias (cool northern hemisphere, warm Southern Ocean), an overly strong global hydrological cycle and insufficient European blocking.

Volume overload cleanup: An approach for on-line SPE-GC, GPC-GC, and GPC-SPE-GC

NARCIS (Netherlands)

Kerkdijk, H.; Mol, H.G.J.; Nagel, B. van der

2007-01-01

A new concept for cleanup, based on volume overloading of the cleanup column, has been developed for on-line coupling of gel permeation chromatography (GPC), solid-phase extraction (SPE), or both, to gas chromatography (GC). The principle is outlined and the applicability demonstrated by the

COMPONENTES MINORITÁRIOS DO ÓLEO DE MAMONA (Ricinus comunnis L.

Directory of Open Access Journals (Sweden)

Elina Bastos Caramão

2007-12-01

Full Text Available O óleo extraído de sementes de Ricinnus communis L., conhecida como mamona, foi analisado neste trabalho quanto a presença decomponentes minoritários extraídos na fase insaponificável. A extração de insaponificáveis foi realizada conforme o método AOCS(Ca 6a-40 e a análise das amostras de óleo foi realizada por Cromatografia gasosa acoplada a espectrometria de massas (CG-DEMapós derivatização com BSA. Entre as substâncias identificadas encontrou-se o D-tocoferol, g- tocoferol, D5-ergostenol, stigmasterol,obtusifoliol, g-sitosterol, fucosterol e cicloartenol. As amostras de óleo de diferentes variedades de mamona, obtidas por prensagem afrio e por solvente em extrator soxhlet apresentaram diferenças quanto as substâncias separadas. O método empregado para extração eanálise foi apropriado para identificar a presença de componentes minoritários no óleo de mamona.

Optimization of diterpenes bioconversion process by the fungus Cephalosporium aphidicola Otimização do processo de bioconversão de compostos diterpênicos pelo fungo Cephalosporium aphidicola

Directory of Open Access Journals (Sweden)

Jacqueline Aparecida Takahashi

2000-06-01

Full Text Available Parameters for a more efficient biotransformation of diterpene-like compounds by the fungus Cephalosporium aphidicola were established by carrying out microscale feedings at several conditions. Experiments were guided by thin layer chromatography and gas chromatography analysis. It was observed that the substrate should be added in ethanol at concentrations between 15 to 30 mg per 100 ml of medium. The extraction of the product showed to be more efficient when carried out from both mycelia and broth and using ethylacetate as the extracting solvent. The experiment should be stopped six days after feeding the substrate to the fungus for the best product yield.Condições otimizadas para a biotransformação de compostos diterpênicos pelo fungo Cephalosporium aphidicola foram determinadas, realizando-se incubações em microescala nas quais variaram-se parâmetros como o tempo de incubação e a quantidade de substrato adicionado. A velocidade (índice de bioconversão foi monitorada analisando-se os extratos de cultivo através de cromatografia em camada delgada e cromatografia gasosa. Os resultados obtidos mostraram que, para melhores rendimentos, o substrato deve ser adicionado em solução etanólica, na concentração de 15-30 mg por 100 mL de meio de cultura. A extração de produtos deve ser realizada com acetato de etila, a partir da fase aquosa e do micélio, no sexto dia após a adição do substrato. Estes resultados podem ser utilizados como um roteiro para incubações de compostos estruturalmente semelhantes com o fungo Cephalosporium aphidicola.

Characterisation of gas and particle emissions from wildfires =

Science.gov (United States)

Vicente, Ana Margarida Proenca

Os incendios florestais sao uma importante fonte de emissao de compostos gasosos e de aerossois. Em Portugal, onde a maioria dos incendios ocorre no norte e centro do pais, os incendios destroem todos os anos milhares de hectares, com importantes perdas em termos economicos, de vidas humanas e qualidade ambiental. As emissoes podem alterar consideravelmente a quimica da atmosfera, degradar a qualidade do ar e alterar o clima. Contudo, a informacao sobre as carateristicas das emissoes dos incendios florestais nos paises do Mediterrâneo e limitada. Tanto a nivel nacional como internacional, existe um interesse crescente na elaboracao de inventarios de emissoes e de regulamentos sobre as emissoes de carbono para a atmosfera. Do ponto de vista atmosferico da monitorizacao atmosferica, os incendios sao considerados um desafio, dada a sua variabilidade temporal e espacial, sendo de esperar um aumento da sua frequencia, dimensao e severidade, e tambem porque as estimativas de emissoes dependem das carateristicas dos biocombustiveis e da fase de combustao. O objetivo deste estudo foi quantificar e caraterizar as emissoes de gases e aerossois de alguns dos mais representativos incendios florestais que ocorreram no centro de Portugal nos veroes de 2009 e de 2010. Efetuou-se a colheita de amostras de gases e de duas fracoes de particulas (PM2.5 e PM2.5-10) nas plumas de fumo em sacos Tedlar e em filtros de quartzo acoplados a um amostrador de elevado volume, respetivamente. Os hidrocarbonetos totais (THC) e oxidos de carbono (CO e CO2) nas amostras gasosas foram analisados em instrumentos automaticos de ionizacao de chama e detetores nao dispersivos de infravermelhos, respetivamente. Para algumas amostras, foram tambem quantificados alguns compostos de carbonilo apos reamostragem do gas dos sacos Tedlar em cartuchos de silica gel revestidos com 2,4-dinitrofenilhidrazina (DNPH), seguida de analise por cromatografia liquida de alta resolucao. Nas particulas, analisou-se o

Functional characterization of two CITED3 homologs (gcCITED3a and gcCITED3b in the hypoxia-tolerant grass carp, Ctenopharyngodon idellus

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Yu Richard MK

2009-11-01

Full Text Available Abstract Background CITED proteins belong to a family of non-DNA-binding transcriptional co-regulators that are characterized by a conserved ED-rich domain at the C-terminus. This family of genes is involved in the regulation of a variety of transcriptional responses through interactions with the CBP/p300 integrators and various transcription factors. In fish, very little is known about the expression and functions of CITEDs. Results We have characterized two closely related but distinct CITED3 genes, gcCited3a and gcCited3b, from the hypoxia-tolerant grass carp. The deduced gcCITED3a and gcCITED3b proteins share 72% amino acid identity, and are highly similar to the CITED3 proteins of both chicken and Xenopus. Northern blot analysis indicates that the mRNA expression of gcCited3a and gcCited3b is strongly induced by hypoxia in the kidney and liver, respectively. Luciferase reporter assays demonstrated that both gene promoters are activated by gcHIF-1. Further, ChIP assays comparing normal and hypoxic conditions reveal differential in vivo binding of gcHIF-1 to both gene promoters in kidney and liver tissues. HRE-luciferase reporter assays demonstrated that both gcCITED3a and gcCITED3b proteins inhibit gcHIF-1 transcriptional activity, and GST pull-down assays confirmed that both proteins bind specifically to the CH1 domain of the grass carp p300 protein. Conclusion The grass carp gcCITED3a and gcCITED3b genes are differentially expressed and regulated in different fish organs in response to hypoxic stress. This is the first report demonstrating in vivo regulation of two closely-related CITED3 isogenes by HIF-1, as well as CITED3 regulation of HIF-1 transcriptional activity in fish. Overall, our findings suggest that unique molecular mechanisms operate through these two gcCITED3 isoforms that likely play an important regulatory role in the hypoxic response in the grass carp.

At least two Fc Neu5Gc residues of monoclonal antibodies are required for binding to anti-Neu5Gc antibody

OpenAIRE

Yu, Chuanfei; Gao, Kai; Zhu, Lei; Wang, Wenbo; Wang, Lan; Zhang, Feng; Liu, Chunyu; Li, Meng; Wormald, Mark R.; Rudd, Pauline M.; Wang, Junzhi

2016-01-01

Two non-human glycan epitopes, galactose-Į-1,3-galactose (Į-gal) and Neu5Gc-Į-2-6-galactose (Neu5Gc) have been shown to be antigenic when attached to Fab oligosaccharides of monoclonal antibodies (mAbs) , while Į-gal attached to Fc glycans were not. However, the antigenicity of Neu5Gc on the Fc glycans remains unclear in the context that most mAbs carry only Fc glycans. After studying two clinical mAbs carrying significant amounts of Fc Neu5Gc, we show that their binding activity with anti-Ne...

The glycosylation and characterization of the candidate Gc macrophage activating factor

DEFF Research Database (Denmark)

Ravnsborg, Tina; Olsen, Dorthe T; Thysen, Anna Hammerich

2010-01-01

The vitamin D binding protein, Gc globulin, has in recent years received some attention for its role as precursor for the extremely potent macrophage activating factor (GcMAF). An O-linked trisaccharide has been allocated to the threonine residue at position 420 in two of the three most common...... isoforms of Gc globulin (Gc1s and Gc1f). A substitution for a lysine residue at position 420 in Gc2 prevents this isoform from being glycosylated at that position. It has been suggested that Gc globulin subjected sequentially to sialidase and galactosidase treatment generates GcMAF in the form of Gc...... globulin with only a single GalNAc attached to T420. In this study we confirm the location of a linear trisaccharide on T420. Furthermore, we provide the first structural evidence of the generation of the proposed GcMAF by use of glycosidase treatment and mass spectrometry. Additionally the generated GcMAF...

The glycosylation and characterization of the candidate Gc macrophage activating factor.

Science.gov (United States)

Ravnsborg, Tina; Olsen, Dorthe T; Thysen, Anna Hammerich; Christiansen, Maja; Houen, Gunnar; Højrup, Peter

2010-04-01

The vitamin D binding protein, Gc globulin, has in recent years received some attention for its role as precursor for the extremely potent macrophage activating factor (GcMAF). An O-linked trisaccharide has been allocated to the threonine residue at position 420 in two of the three most common isoforms of Gc globulin (Gc1s and Gc1f). A substitution for a lysine residue at position 420 in Gc2 prevents this isoform from being glycosylated at that position. It has been suggested that Gc globulin subjected sequentially to sialidase and galactosidase treatment generates GcMAF in the form of Gc globulin with only a single GalNAc attached to T420. In this study we confirm the location of a linear trisaccharide on T420. Furthermore, we provide the first structural evidence of the generation of the proposed GcMAF by use of glycosidase treatment and mass spectrometry. Additionally the generated GcMAF candidate was tested for its effect on cytokine release from macrophages in human whole blood. Copyright 2010 Elsevier B.V. All rights reserved.

A Monolithically-Integrated μGC Chemical Sensor System

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Davor Copic

2011-06-01

Full Text Available Gas chromatography (GC is used for organic and inorganic gas detection with a range of applications including screening for chemical warfare agents (CWA, breath analysis for diagnostics or law enforcement purposes, and air pollutants/indoor air quality monitoring of homes and commercial buildings. A field-portable, light weight, low power, rapid response, micro-gas chromatography (μGC system is essential for such applications. We describe the design, fabrication and packaging of mGC on monolithically-integrated Si dies, comprised of a preconcentrator (PC, μGC column, detector and coatings for each of these components. An important feature of our system is that the same mechanical micro resonator design is used for the PC and detector. We demonstrate system performance by detecting four different CWA simulants within 2 min. We present theoretical analyses for cost/power comparisons of monolithic versus hybrid μGC systems. We discuss thermal isolation in monolithic systems to improve overall performance. Our monolithically-integrated μGC, relative to its hybrid cousin, will afford equal or slightly lower cost, a footprint that is 1/2 to 1/3 the size and an improved resolution of 4 to 25%.

Pirólise de resíduos de borrachas do setor de mineração para a produção de combustíveis: estudos em escala piloto

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Rochel Montero Lago

Full Text Available Resumo Neste trabalho, estudou-se em escala piloto a pirólise de três diferentes rejeitos de borracha do setor de mineração, i.e. peças de moinho de composição nominal de borracha estireno e butadieno (SBR, peneiras e correias transportadoras com composição nominal à base de borracha natural e butadieno (NR/BR e pneus offroad de composição complexa (mistura de borracha natural, nitrílica, butadieno e estireno-butadieno em temperaturas de 450, 600 e 800°C. As reações realizadas a 450°C mostraram uma pirólise incompleta, sendo que a 600 e 800°C os rejeitos de borracha se convertem totalmente em três produtos: 15-25% de gás, 42-44% sólido e 34-45% de líquido. Análises por cromatografia gasosa (CG dos produtos gasosos mostraram majoritariamente a presença de hidrocarbonetos C1-C4 com valores de poder calorífico inferior (PCI iguais a 8.496 e 7.325 kcal kg-1, similares ao gás liquefeito de petróleo (GLP. Análise dos sólidos obtidos por análise elementar de carbono, hidrogênio e nitrogênio (CHN, espectrômetria de emissão atômica com plasma induzido (ICP-AES Spectro Ciros CCD para a determinação de enxofre, análise térmica gravimétrica e diferencial (TG/DTA, carbono fixo, cinzas, voláteis mostraram a presença de 72-89% de carbono com 2% de enxofre. Análises dos produtos líquidos por cromatografia gasosa acoplado a espectrometria de massas (CG-EM indicaram a presença de misturas complexas de hidrocarbonetos majoritariamente até C20. As amostras NR/BR e pneu produzem líquidos com concentração de compostos aromáticos próxima a 50%, enquanto a amostra SBR resulta na formação de um líquido de concentração próxima a 87%. A mistura dessa fração líquida obtida pela pirólise (sem qualquer purificação com um diesel comercial nas proporções de 0,5, 1 e 3 vol% mostrou que nenhum parâmetro de qualidade de combustível definido pela ANP (Agência Nacional do Petróleo, Gás Natural e Biocombust

Gc globulin as a diagnostic and prognostic marker in horses

DEFF Research Database (Denmark)

Pihl, Tina Holberg

can prevent development of shock and thereby increase survival chances. The in vivo toxicity of Gc-globulin infusion is currently being investigated in horses and other species. Gc-globulin has been demonstrated in horse plasma and its structure closely resembles that of human Gc-globulin. Gc......-globulin concentrations in horses under clinical conditions have never previously been investigated. The Ph.D. project focuses on Gc-globulin as a prognostic marker in horses with acute abdominal pain....

OTIMIZAÇÃO DA ETAPA DE ISOLAMENTO DOS COMPOSTOS VOLÁTEIS DE MEL PARA ANÁLISE POR CROMATOGRAFIA GASOSA

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Deborah H. M. BASTOS

2009-07-01

Full Text Available

O presente trabalho teve por objetivo desenvolver e detalhar uma metodologia de isolamento de compostos voláteis de mel de laranja, utilizando técnica de concentração do headspace e processo de otimização do tempo de captura e do solvente utilizado por meio de métodos sensoriais e instrumentais. Os voláteis foram capturados em polimero Porapak-Q, com tempos de captura variando entre 2 e 4 horas, utilizando-se acetona e hexano para sua desorção. Uma equipe sensorial treinada, composta por oito julgadores selecionados com base em poder discriminativo, repetibilidade e consenso nos julgamentos, avaliou a intensidade de aroma característico de mel em cada um dos isolados obtidos. Realizou-se análise cromatográfica em cada uma das fiações isoladas e o número de picos obtidos foi computado. Análise de variância univariada (ANOVA dos dados sensoriais indicou a acetona como o melhor solvente para eluição dos compostos capturados no polímero poroso e o tempo de captura de 3 horas suficiente para se obter um isolado, apresentando intensidade moderada de aroma característico de mel. Os dados instrumentais confirmaram os resultados obtidos pela análise sensorial dos isolados.

Molecular analysis of intact preen waxes of Calidris Canutus (Aves: Scolopacidae) by GC/MS and GC/MS/MS

NARCIS (Netherlands)

Sinninghe Damsté, J.S.; Dekker, M.H.A.; Piersma, T.

2000-01-01

The intact preen wax esters of the red knot Calidris canutus were studied with gas chromatography/mass spectrometry (GC/MS) and GC/MS/MS. In this latter technique, transitions from the molecular ion to fragment ions representing the fatty acid moiety of the wax esters were measured, providing

Desenvolvimento de metodologia para determinação de multirresiduos de herbicidas e seus metabolitos em agua e em solo por cromatografia liquida de alta eficiencia

OpenAIRE

Glaucia Maria Ferreira Pinto

2002-01-01

Resumo: Com o crescimento da população mundial, a preocupação com o aumento da produção agrícola torna-se mais pronunciada. Para garantir um maior rendimento agrícola tem-se intensificado o uso de agrotóxicos, o que aumentou a contaminação ambiental causada por estes compostos químicos. No presente trabalho foram desenvolvidos e validados métodos envolvendo o uso de extração em fase sólida e cromatografia líquida de alta eficiência, aplicados à análise de amostras ambientais de águas e solos,...

ADAP-GC 3.0: Improved Peak Detection and Deconvolution of Co-eluting Metabolites from GC/TOF-MS Data for Metabolomics Studies.

Science.gov (United States)

Ni, Yan; Su, Mingming; Qiu, Yunping; Jia, Wei; Du, Xiuxia

2016-09-06

ADAP-GC is an automated computational pipeline for untargeted, GC/MS-based metabolomics studies. It takes raw mass spectrometry data as input and carries out a sequence of data processing steps including construction of extracted ion chromatograms, detection of chromatographic peak features, deconvolution of coeluting compounds, and alignment of compounds across samples. Despite the increased accuracy from the original version to version 2.0 in terms of extracting metabolite information for identification and quantitation, ADAP-GC 2.0 requires appropriate specification of a number of parameters and has difficulty in extracting information on compounds that are in low concentration. To overcome these two limitations, ADAP-GC 3.0 was developed to improve both the robustness and sensitivity of compound detection. In this paper, we report how these goals were achieved and compare ADAP-GC 3.0 against three other software tools including ChromaTOF, AnalyzerPro, and AMDIS that are widely used in the metabolomics community.

ADAP-GC 3.0: Improved Peak Detection and Deconvolution of Co-eluting Metabolites from GC/TOF-MS Data for Metabolomics Studies

Science.gov (United States)

Ni, Yan; Su, Mingming; Qiu, Yunping; Jia, Wei

2017-01-01

ADAP-GC is an automated computational pipeline for untargeted, GC-MS-based metabolomics studies. It takes raw mass spectrometry data as input and carries out a sequence of data processing steps including construction of extracted ion chromatograms, detection of chromatographic peak features, deconvolution of co-eluting compounds, and alignment of compounds across samples. Despite the increased accuracy from the original version to version 2.0 in terms of extracting metabolite information for identification and quantitation, ADAP-GC 2.0 requires appropriate specification of a number of parameters and has difficulty in extracting information of compounds that are in low concentration. To overcome these two limitations, ADAP-GC 3.0 was developed to improve both the robustness and sensitivity of compound detection. In this paper, we report how these goals were achieved and compare ADAP-GC 3.0 against three other software tools including ChromaTOF, AnalyzerPro, and AMDIS that are widely used in the metabolomics community. PMID:27461032

Gc protein-derived macrophage-activating factor (GcMAF) stimulates cAMP formation in human mononuclear cells and inhibits angiogenesis in chick embryo chorionallantoic membrane assay.

Science.gov (United States)

Pacini, Stefania; Morucci, Gabriele; Punzi, Tiziana; Gulisano, Massimo; Ruggiero, Marco

2011-04-01

The effects of Gc protein-derived macrophage-activating factor (GcMAF) have been studied in cancer and other conditions where angiogenesis is deregulated. In this study, we demonstrate for the first time that the mitogenic response of human peripheral blood mononuclear cells (PBMCs) to GcMAF was associated with 3'-5'-cyclic adenosine monophosphate (cAMP) formation. The effect was dose dependent, and maximal stimulation was achieved using 0.1 ng/ml. Heparin inhibited the stimulatory effect of GcMAF on PBMCs. In addition, we demonstrate that GcMAF (1 ng/ml) inhibited prostaglandin E(1)- and human breast cancer cell-stimulated angiogenesis in chick embryo chorionallantoic membrane (CAM) assay. Finally, we tested different GcMAF preparations on CAM, and the assay proved to be a reliable, reproducible and inexpensive method to determine the relative potencies of different preparations and their stability; we observed that storage at room temperature for 15 days decreased GcMAF potency by about 50%. These data could prove useful for upcoming clinical trials on GcMAF.

Quantification of compositional changes of petroleum hydrocarbons by GC/FID and GC/MS during a long-term bioremediation experiment

DEFF Research Database (Denmark)

Jensen, Trine S.; Arvin, Erik; Svensmark, Bo

2000-01-01

Samples from a long-term bioremediation experiment contaminated with two crude oils, Arabian Heavy and Gullfax, was used to analyze the compositional change of petroleum hydrocarbons. A time course of five different homologous series of petroleum hydrocarbons were analysed by GC/FID and GC...

Group separation of organohalogenated contaminants by GCxGC

Energy Technology Data Exchange (ETDEWEB)

Korytar, P.; Leonards, P.; Boer, J. de [Netherlands Institute for Fisheries Research, IJmuiden (Netherlands); Parera, J. [Barcelona Univ. (Spain); Brinkman, U. [Vrije Univ., Amsterdam (Netherlands)

2004-09-15

The congener specific analysis of organohalogenated compounds is challenging, because of a large number of possibly interfering compounds not only within the compound class but also from congeners of other compound classes. Therefore, analytical procedures usually include complicated and time-consuming multi-step sample pre-treatment and/or selective detection (e.g. HRMS, MS/MS) in the consequent gas chromatographic analysis, what makes the procedures laborious and expensive. One way how to improve the situation would be to considerably increase the separation efficiency of the gas chromatographic analysis by replacing conventional GC by so-called comprehensive two-dimensional gas chromatography (GC x GC). In GC x GC two independent separations are applied to an entire sample which effects a considerably enhanced overall resolution and also, because of the analyte refocusing during modulation, an improved analyte detectability. One further aspect which makes GC x GC especially attractive is the ordered structure of the two-dimensional chromatograms, which is observed when mixtures of related compounds, homologues or congeners are analysed. One good example are the bands of alkanes, naphthenes and aromatics present in 2D chromatogram when petrochemical samples are analysed. The ordered structure was reported also within the compound class of some organohalogenated contaminants, more precisely, of polychlorinated biphenyls and toxaphenes (ordering to number of chlorine atoms on the skeleton). However, to date, no study of separation among the different compound classes has been reported. In the present paper, this topic will be studied for the most common contaminants. While the principle aim is the group type separation, some attention will be devoted also to within the class separation (e.g., for polychlorinated diphenylethers and polychlorinated alkanes).

Postmortem identification and quantitation of 2,5-dimethoxy-4-n-propylthiophenethylamine using GC-MSD and GC-NPD.

Science.gov (United States)

Curtis, Byron; Kemp, Philip; Harty, Linda; Choi, Chai; Christensen, Dix

2003-10-01

2,5-Dimethoxy-4-n-propylthiophenethylamine (2C-T-7) has structural and pharmacodynamic similarities to methylenedioxymethamphetamine (MDMA). This compound was initially identified from a routine screening procedure in postmortem urine from a 20-year-old male that died in a local emergency room after reportedly insufflating 35 mg. This report describes the development of a quantitative method for 2C-T-7. A number of method parameters were studied including internal standard selection, liquid-liquid extraction scheme, and drug stability in preserved refrigerated blood. The adopted method for blood and urine involves the addition of trimethoxyamphetamine (TMA) as internal standard, alkalinization with ammonium hydroxide, and liquid-liquid extraction with n-chlorobutane. To facilitate recovery from liver, a 1:4 aqueous homogenate was pretreated with dilute perchloric acid, centrifuged, and the supernatant was extracted as previously described. In each case, 0.1% hydrochloric acid in methanol was added during the final concentration step to prevent loss of drug caused by evaporation. Samples were analyzed by gas chromatography with nitrogen-phosphorus detection (GC-NPD) and electron ionization GC-mass spectrometry (MS) utilizing selected ion monitoring. For the GC-MS analysis, the characteristic ions monitored for 2C-T-7 were m/z 226, 255, and 183 and for TMA, m/z 182. The limits of detection and quantitation in blood were 6.0 and 15.6 ng/mL, respectively, by both GC-NPD and GC-MS. The results from the postmortem case were as follows: heart blood, 57 ng/mL; femoral blood, 100 ng/mL; urine, 1120 ng/mL; and liver, 854 ng/g.

Trocas gasosas de mudas de videira, obtidas por dois porta-enxertos, submetidas à deficiência hídrica Gas exchange of vine cuttings obtained from two graftings submitted to water deficiency

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Claudia Rita de Souza

2001-10-01

Full Text Available Este trabalho teve como objetivo avaliar o efeito da deficiência hídrica e de dois porta-enxertos nas trocas gasosas de mudas de videira cultivadas em vasos, nas condições de casa de vegetação. Utilizou-se como copa a 'Niágara Rosada' (Vitis labrusca, e como porta-enxertos, o 101-14 (V. riparia e o 1103 Paulsen (V. rupestris x V. berlandieri. Doze dias após a suspensão da rega, o potencial hídrico foliar da combinação 'Niágara Rosada'/101-14 apresentou os menores valores (-2,80 MPa em relação à 'Niágara Rosada'/1103 Paulsen (-2,10 MPa nas plantas não-irrigadas, enquanto o teor relativo de água variou apenas entre os tratamentos hídricos. Com a evolução do estresse hídrico, houve uma sensível redução nas trocas gasosas da cultivar 'Niágara Rosada', que apresentaram valores próximos de zero, devido ao fechamento dos estômatos, sem diferenças entre os porta-enxertos. Somente após 12 dias sem rega, os porta-enxertos influenciaram a eficiência no uso da água e eficiência fotoquímica do fotossistema II, onde a 'Niágara Rosada' enxertada sobre o 101-14 apresentou valores inferiores ao 1103 Paulsen. Entretanto, durante o período de suspensão da rega, os porta-enxertos não influenciaram as trocas gasosas da cultivar 'Niágara Rosada', e apresentaram comportamento semelhante em condições de baixa disponibilidade hídrica.The present work aimed to evaluate the water deficiency effect and two graftings on the gas exchange of vine cuttings under greenhouse conditions. 'Niágara Rosada' (Vitis labrusca was used as scion, and 101-14 (V. riparia x V. rupestris and 1103 Paulsen (V. rupestris x V. berlandieri were used as rootstocks. Twelve days after watering suspension, the leaf water potential of the combination 'Niágara Rosada'/101-14 showed lower (-2.80 MPa in relation to 'Niágara Rosada'/1103 Paulsen (-2.10 MPa in the non-irrigated plants, while relative water content altered only among watering levels. With the

Chemical Analysis of Essential oil of "Artemisia haussknechtii Boiss" by GC and GC/ MS

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A. Nassir- Ahraadi . A. Rustaiyan

1994-08-01

Full Text Available The composition of the essential oil from the leaves and flowers of "Artemisia haussknechtii Boiss growing wild in the north-west of Iran, was investigated by GC and GC/MS."nThe main components of the volatile oil were 1,8 - cineol (16.5%, camphor (14.1%. artemisia ketone (10.5%, fragranol (9.0%, Yomogi alcohol (7.5% and B- pinene (5.4%. The total contribution of these compounds to the oil amounted to 63.0%."nMonoterpens and sesquiterpenes represent 90.08% and 1.52% of the oil respectively. Of the twenty oxygen-containing monoterpenes which made up a fairly large fraction of the terpenoid composition, the predominant components were 1,8 - cineole and camphor.

Quality Control Of Selected Pesticides With GC

Energy Technology Data Exchange (ETDEWEB)

Karasali, H. [Benaki Phytopathological Institute Laboratory of Physical and Chemical Analysis of Pesticides, Ekalis (Greece)

2009-07-15

The practical quality control of selected pesticides with GC is treated. Detailed descriptions are given on materials and methods used, including sample preparation and GC operating conditions. The systematic validation of multi methods is described, comprising performance characteristics in routine analysis, like selectivity, specificity etc. This is illustrated by chromatograms, calibration curves and tables derived from real laboratory data. (author)

Case Report: GcMAF Treatment in a Patient with Multiple Sclerosis.

Science.gov (United States)

Inui, Toshio; Katsuura, Goro; Kubo, Kentaro; Kuchiike, Daisuke; Chenery, Leslye; Uto, Yoshihiro; Nishikata, Takahito; Mette, Martin

2016-07-01

Gc protein-derived macrophage-activating factor (GcMAF) has various functions as an immune modulator, such as macrophage activation, anti-angiogenic activity and anti-tumor activity. Clinical trials of second-generation GcMAF demonstrated remarkable clinical effects in several types of cancers. Thus, GcMAF-based immunotherapy has a wide application for use in the treatment of many diseases via macrophage activation that can be used as a supportive therapy. Multiple sclerosis (MS) is considered to be an autoimmune disorder that affects the myelinated axons in the central nervous system (CNS). This study was undertaken to examine the effects of second-generation GcMAF in a patient with MS. This case study demonstrated that treatments of GcMAF in a patient with MS have potent therapeutic actions with early beneficial responses, especially improvement of motor dysfunction. GcMAF shows therapeutic potency in the treatment of MS. Copyright© 2016 International Institute of Anticancer Research (Dr. John G. Delinassios), All rights reserved.

Effect of the natural and artificial drying of leaf biomass Piper hispidinervum on the chemical composition of the essential oilEfeito da secagem natural e artificial da biomassa foliar de Piper hispidinervum na composição química do óleo essencial

Directory of Open Access Journals (Sweden)

Marília Pereira Machado

2013-03-01

Full Text Available Piper hispidinervum C.DC. is a plant native to the Amazon region, produces an essential oil rich in safrole. The aim of this study was to evaluate the effect of different methods of drying biomass in chemical composition of the essential oil of P. hispidinervum cultivated in Morretes (PR. The treatments were: fresh leaves; natural drying for 6 and 12 days; oven drying at 40°C for 6 and 12 days. The essential oil was extracted by hydrodistillation from samples of 50 g of each treatment in triplicate. The chemical composition of essential oil was performed by gas chromatography coupled to mass spectrometer (GC/ MS. The experimental design was completely randomized design with three replication and four plants per plot. Data were subjected to analysis of variance. The type and drying time changes the chemical composition of the essential oil of P. hispidinervum. The dried at 40°C for 12 days reduce the amount of essential oil components, but with increasing content of safrole. Piper hispidinervum C.DC. é uma planta nativa da Amazônia, produtora de óleo essencial rico em safrol. O objetivo do presente trabalho foi avaliar o efeito de diferentes métodos de secagem da biomassa folia de pimenta longa (P. hispidinervum, cultivada em Morretes (PR, na composição química do óleo essencial. Os tratamentos avaliados foram: folhas frescas; secagem natural por 6 e 12 dias; secagem em estufa à 40°C por 6 e 12 dias. O óleo essencial foi extraído por hidrodestilação a partir de amostras de 50 g de cada tratamento em triplicata. A determinação da composição química do óleo essencial foi realizada por cromatografia gasosa acoplada ao espectrômetro de massa (GC/MS. O delineamento experimental foi inteiramente casualizado, com três repetições e quatro plantas por parcela. Os dados obtidos foram submetidos à análise de variância. O tipo e tempo de secagem alteram a constituição química do óleo essencial de pimenta-longa. A secagem em

G+C content dominates intrinsic nucleosome occupancy

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Hughes Timothy R

2009-12-01

Full Text Available Abstract Background The relative preference of nucleosomes to form on individual DNA sequences plays a major role in genome packaging. A wide variety of DNA sequence features are believed to influence nucleosome formation, including periodic dinucleotide signals, poly-A stretches and other short motifs, and sequence properties that influence DNA structure, including base content. It was recently shown by Kaplan et al. that a probabilistic model using composition of all 5-mers within a nucleosome-sized tiling window accurately predicts intrinsic nucleosome occupancy across an entire genome in vitro. However, the model is complicated, and it is not clear which specific DNA sequence properties are most important for intrinsic nucleosome-forming preferences. Results We find that a simple linear combination of only 14 simple DNA sequence attributes (G+C content, two transformations of dinucleotide composition, and the frequency of eleven 4-bp sequences explains nucleosome occupancy in vitro and in vivo in a manner comparable to the Kaplan model. G+C content and frequency of AAAA are the most important features. G+C content is dominant, alone explaining ~50% of the variation in nucleosome occupancy in vitro. Conclusions Our findings provide a dramatically simplified means to predict and understand intrinsic nucleosome occupancy. G+C content may dominate because it both reduces frequency of poly-A-like stretches and correlates with many other DNA structural characteristics. Since G+C content is enriched or depleted at many types of features in diverse eukaryotic genomes, our results suggest that variation in nucleotide composition may have a widespread and direct influence on chromatin structure.

A review on g-C3N4-based photocatalysts

International Nuclear Information System (INIS)

Wen, Jiuqing; Xie, Jun; Chen, Xiaobo; Li, Xin

2017-01-01

Graphical abstract: The photocatalytic fundamentals, versatile properties, design strategies and potential applications of g-C 3 N 4 -based photocatalysts were systematically summarized and addressed. - Highlights: • The photocatalytic fundamentals of g-C 3 N 4 were systematically summarized. • The versatile properties of g-C 3 N 4 photocatalysts were highlighted. • The different design strategies of g-C 3 N 4 photocatalysts were reviewed. • The important photocatalytic applications of g-C 3 N 4 were also addressed. - Abstract: As one of the most appealing and attractive technologies, heterogeneous photocatalysis has been utilized to directly harvest, convert and store renewable solar energy for producing sustainable and green solar fuels and a broad range of environmental applications. Due to their unique physicochemical, optical and electrical properties, a wide variety of g-C 3 N 4 -based photocatalysts have been designed to drive various reduction and oxidation reactions under light irradiation with suitable wavelengths. In this review, we have systematically summarized the photocatalytic fundamentals of g-C 3 N 4 -based photocatalysts, including fundamental mechanism of heterogeneous photocatalysis, advantages, challenges and the design considerations of g-C 3 N 4 -based photocatalysts. The versatile properties of g-C 3 N 4 -based photocatalysts are highlighted, including their crystal structural, surface phisicochemical, stability, optical, adsorption, electrochemical, photoelectrochemical and electronic properties. Various design strategies are also thoroughly reviewed, including band-gap engineering, defect control, dimensionality tuning, pore texture tailoring, surface sensitization, heterojunction construction, co-catalyst and nanocarbon loading. Many important applications are also addressed, such as photocatalytic water splitting (H 2 evolution and overall water splitting), degradation of pollutants, carbon dioxide reduction, selective organic

Development of the GC-MS organic aerosol monitor (GC-MS OAM) for in-field detection of particulate organic compounds

Science.gov (United States)

Cropper, Paul M.; Overson, Devon K.; Cary, Robert A.; Eatough, Delbert J.; Chow, Judith C.; Hansen, Jaron C.

2017-11-01

Particulate matter (PM) is among the most harmful air pollutants to human health, but due to its complex chemical composition is poorly characterized. A large fraction of PM is composed of organic compounds, but these compounds are not regularly monitored due to limitations in current sampling and analysis techniques. The Organic Aerosol Monitor (GC-MS OAM) combines a collection device with thermal desorption, gas chromatography and mass spectrometry to quantitatively measure the carbonaceous components of PM on an hourly averaged basis. The GC-MS OAM is fully automated and has been successfully deployed in the field. It uses a chemically deactivated filter for collection followed by thermal desorption and GC-MS analysis. Laboratory tests show that detection limits range from 0.2 to 3 ng for 16 atmospherically relevant compounds, with the possibility for hundreds more. The GC-MS OAM was deployed in the field for semi-continuous measurement of the organic markers, levoglucosan, dehydroabietic acid, and polycyclic aromatic hydrocarbons (PAHs) from January to March 2015. Results illustrate the significance of this monitoring technique to characterize the organic components of PM and identify sources of pollution.

Resíduos de deltametrina em grãos de trigo e em seus produtos processados, determinados por cromatografia gasosa

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Trevizan Luiz Roberto Pimentel

2000-01-01

Full Text Available O objetivo do presente estudo foi avaliar a degradação/persistência do inseticida piretróide deltametrina em grãos de trigo e em seus produtos processados, a saber: farelo, farinha branca, farinha integral e pão. Os grãos foram tratados de modo a alcançar a concentração teórica de 0,35 mg kg-1 do piretróide. As amostras foram tomadas a zero, 15, 30, 60 e 90 dias após a aplicação. Houve tendência de concentração do piretróide no farelo de trigo e um menor acúmulo nas farinhas, sendo que após o processo de cozimento do pão observou-se perda do inseticida.

Bioaccumulation study of acrylate monomers in algae (Chlorella Kessleri) by PY-GC and PY-GC/MS

International Nuclear Information System (INIS)

Halas, L.; Orinak, A.; Adamova, M.; Ladomersky, J.

2004-01-01

Acrylate monomers methylmethacrylate (MMA) and cyclohexylmethacrylate (CHMA) bioaccumulation has been determined in aquatic organism, algae (Chlorella kessleri). Algae were collected in amount of 0.4 mg and directly injected to the paralytic cell. In algae bodies accumulated monomers were analysed by pyrolysis gas chromatography (Py-GC) and pyrolysis gas chromatography coupled with mass spectrometry (Py-GC/MS). Traces of the accumulated monomers in algae body can be determined after 1-, 2 -, 3-weeks of incubation. Maximum content of MMA was determined after 3-week of experiment, contrariwise in the case of CHMA after 2-week exposition. Relationship with pyrolysis temperature has also been studied. (authors)

Middle distillates hydrogen content via GC×GC-FID.

Science.gov (United States)

Vozka, Petr; Mo, Huaping; Šimáček, Pavel; Kilaz, Gozdem

2018-08-15

Liquid transportation fuels in the middle distillate range contain thousands of hydrocarbons making the predictions and calculations of properties from composition a challenging process. We present a new approach of hydrogen content determination by comprehensive two-dimensional gas chromatography with flame ionization detector (GC×GC-FID) using a weighted average method. GC×GC-FID hydrogen determination precision was excellent (0.005 wt% repeatability). The method accuracy was evaluated by high-resolution nuclear magnetic resonance (NMR) technique, which is non-biased, measures the H signal directly and was independently validated by controls in the current study. The hydrogen content (in the range of 12.72-15.54 wt%) in 28 fuel samples were determined using GC×GC-FID. Results were within ± 2% of those obtained via NMR. Owing to the fact that NMR is accepted as an accurate technique for hydrogen content determination, the GC×GC method proposed in this study can be considered precise and accurate. Copyright © 2018 Elsevier B.V. All rights reserved.

The measurement of muscle protein synthesis in broilers with a flooding dose technique: use of 15N-labelled phenylalanine, GC-MS and GC-C-IRMS.

Science.gov (United States)

Dänicke, S; Böttcher, W; Simon, O; Jeroch, H

2001-01-01

An experiment was carried out to measure fractional muscle protein synthesis rates (k(s)) in broilers with injection of a flooding dose of phenylalanine (1 ml/100 g body weight of 150 mM phenylalanine; 38 atom percent excess (APE) [15N]phenylalanine). K(s) was calculated from the [15N] enrichment in phenylalanine of tissue-free and protein-bound phenylalanine using both gas chromatography mass spectrometry (GC-MS) and gas chromatography combustion isotope ratio mass spectrometry (GC-C-IRMS) for measurements after a 10 min isotope incorporation period. The tertiary-butyldimethylsilyl (t-BDMS) derivatives of phenylalanine were used for gas chromatographic separation in both systems. GC-MS and GC-C-IRMS were calibrated for a range of 7 to 37 [15N]APE and 0 to 0.62 [15N]APE, respectively, and for sample sizes of 0.45 to 4.5 nmol phenylalanine and 7 to 40 nmol phenylalanine, respectively. Reproducibility of standards as a measure of precision varied from 0.06 to 0.29 [15N]APE and from 0.0004 to 0.0018 [15N]APE in GC-MS and GC-C-IRMS, respectively. K(s) was measured in the m. pectoralis major of broilers fed rye based diets (56%) which were provided either unsupplemented (-) or supplemented (+) with an enzyme preparation containing xylanase. K(s) in breast muscles was significantly increased from 21.8%/d to 23.9%/d due to enzyme supplementation. It can be concluded from the study that the measurement of protein synthesis in broilers with the flooding dose technique can be carried out by using [15N]phenylalanine, GC-MS and GC-C-IRMS.

Integrated cancer therapy combined radiotherapy and immunotherapy. The challenge of using Gc protein-derived macrophage activating factor (GcMAF) as a key molecule

International Nuclear Information System (INIS)

Uto, Yoshihiro; Hori, Hitoshi

2013-01-01

Radiation oncologists know the conflict between radiotherapy and immunotherapy, but now challenged trails of the integrative cancer therapies combined radiation therapy and various immunoreaction/immune therapies begin. We therefore review the recent results of basic research and clinical trial of the integrated cancer therapies which combined radiotherapy and various immune therapies/immunoreaction, and the challenged studies of combined use of radiotherapy and our developed cancer immunotherapy using serum GcMAF which is human serum containing Gc protein-derived macrophage activating factor (GcMAF). (author)

Comprehensive analysis of yeast metabolite GC x GC-TOFMS data: combining discovery-mode and deconvolution chemometric software.

Science.gov (United States)

Mohler, Rachel E; Dombek, Kenneth M; Hoggard, Jamin C; Pierce, Karisa M; Young, Elton T; Synovec, Robert E

2007-08-01

The first extensive study of yeast metabolite GC x GC-TOFMS data from cells grown under fermenting, R, and respiring, DR, conditions is reported. In this study, recently developed chemometric software for use with three-dimensional instrumentation data was implemented, using a statistically-based Fisher ratio method. The Fisher ratio method is fully automated and will rapidly reduce the data to pinpoint two-dimensional chromatographic peaks differentiating sample types while utilizing all the mass channels. The effect of lowering the Fisher ratio threshold on peak identification was studied. At the lowest threshold (just above the noise level), 73 metabolite peaks were identified, nearly three-fold greater than the number of previously reported metabolite peaks identified (26). In addition to the 73 identified metabolites, 81 unknown metabolites were also located. A Parallel Factor Analysis graphical user interface (PARAFAC GUI) was applied to selected mass channels to obtain a concentration ratio, for each metabolite under the two growth conditions. Of the 73 known metabolites identified by the Fisher ratio method, 54 were statistically changing to the 95% confidence limit between the DR and R conditions according to the rigorous Student's t-test. PARAFAC determined the concentration ratio and provided a fully-deconvoluted (i.e. mathematically resolved) mass spectrum for each of the metabolites. The combination of the Fisher ratio method with the PARAFAC GUI provides high-throughput software for discovery-based metabolomics research, and is novel for GC x GC-TOFMS data due to the use of the entire data set in the analysis (640 MB x 70 runs, double precision floating point).

Expressão de glicoesfingolipídeos no carcinoma espinocelular do trato aerodigestivo superior Glycosphingolipid expression in squamous cell carcinoma of the upper aerodigestive tract

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Marcilio Ferreira Marques Filho

2006-02-01

Full Text Available Os glicoesfingolipídios (GSLs são importantes componentes da membrana celular, organizados em microdomínios, relacionados a receptores de membrana e comportamento anti-social da célula neoplásica como crescimento descontrolado, invasão e ocorrência de metástases. OBJETIVO: Como a expressão de GSLs no carcinoma espinocelular (CEC é tema pouquíssimo estudado decidiu-se realizar estudo prospectivo visando avaliar a expressão de GSLs no CEC do trato aerodigestivo superior. MÉTODO: Coletou-se 33 amostras de CEC e mucosa normal e GSLs extraídos e purificados por cromatografia de fase reversa em coluna de C-18 e hidrólise alcalina em metanol. Os GSLs foram quantificados por densitometria das placas de cromatografia de alta resolução em camada delgada coradas com orcinol. RESULTADOS: Observou-se aumento significativo de GSLs no CEC (3,57µg/mg em comparação à mucosa normal (1,92µg/mg, principalmente do monosialogangliosídeo (GM3, trihexosilceramida (CTH, dihexosilceramida (CDH, globosídeo (Gb4. A expressão de monohexosilceramida (CMH foi semelhante no CEC e na mucosa normal. O aumento do GM3 no CEC foi demonstrado por métodos imunoquímicos empregando-se MAb DH2 (anti-GM3. Analisando-se os carboidratos do CMH por cromatografia gasosa acoplado a espectrômetro de massa constatou-se que a mucosa normal expressa glucosilceramida e o CEC glucosilceramida e galactosilceramida. CONCLUSÃO: O aumento de GSLs no tecido tumoral pode representar alterações dos microdomínios da membrana celular resultantes do processo de transformação maligna, responsáveis por uma maior interação célula-célula e célula-matriz aumentando seu potencial de infiltração e metástase, possibilitando o emprego dos GSLs e de MAbs no diagnóstico e no tratamento do CEC, a exemplo do que ocorre no melanoma.Glycosphingolipids are integral constituents of cellular membrane, arranged in rafts, and with neoplasic cell anti-social behavior, like uncontrolled

GC-Content Normalization for RNA-Seq Data

Science.gov (United States)

2011-01-01

Background Transcriptome sequencing (RNA-Seq) has become the assay of choice for high-throughput studies of gene expression. However, as is the case with microarrays, major technology-related artifacts and biases affect the resulting expression measures. Normalization is therefore essential to ensure accurate inference of expression levels and subsequent analyses thereof. Results We focus on biases related to GC-content and demonstrate the existence of strong sample-specific GC-content effects on RNA-Seq read counts, which can substantially bias differential expression analysis. We propose three simple within-lane gene-level GC-content normalization approaches and assess their performance on two different RNA-Seq datasets, involving different species and experimental designs. Our methods are compared to state-of-the-art normalization procedures in terms of bias and mean squared error for expression fold-change estimation and in terms of Type I error and p-value distributions for tests of differential expression. The exploratory data analysis and normalization methods proposed in this article are implemented in the open-source Bioconductor R package EDASeq. Conclusions Our within-lane normalization procedures, followed by between-lane normalization, reduce GC-content bias and lead to more accurate estimates of expression fold-changes and tests of differential expression. Such results are crucial for the biological interpretation of RNA-Seq experiments, where downstream analyses can be sensitive to the supplied lists of genes. PMID:22177264

Gas chromatography coupled to atmospheric pressure ionization mass spectrometry (GC-API-MS): Review

International Nuclear Information System (INIS)

Li, Du-Xin; Gan, Lin; Bronja, Amela; Schmitz, Oliver J.

2015-01-01

Although the coupling of GC/MS with atmospheric pressure ionization (API) has been reported in 1970s, the interest in coupling GC with atmospheric pressure ion source was expanded in the last decade. The demand of a “soft” ion source for preserving highly diagnostic molecular ion is desirable, as compared to the “hard” ionization technique such as electron ionization (EI) in traditional GC/MS, which fragments the molecule in an extensive way. These API sources include atmospheric pressure chemical ionization (APCI), atmospheric pressure photoionization (APPI), atmospheric pressure laser ionization (APLI), electrospray ionization (ESI) and low temperature plasma (LTP). This review discusses the advantages and drawbacks of this analytical platform. After an introduction in atmospheric pressure ionization the review gives an overview about the history and explains the mechanisms of various atmospheric pressure ionization techniques used in combination with GC such as APCI, APPI, APLI, ESI and LTP. Also new developments made in ion source geometry, ion source miniaturization and multipurpose ion source constructions are discussed and a comparison between GC-FID, GC-EI-MS and GC-API-MS shows the advantages and drawbacks of these techniques. The review ends with an overview of applications realized with GC-API-MS. - Highlights: • Atmospheric pressure ion sources (APCI, ESI, APPI, APLC etc) enable the coupling of LC-based high-end MS to GC. • APIs show advantages in selectivity and sensitivity compared with EI in GC-MS. • Accurate mass database in GC-APCI/MS is emerging as an alternative to GC-EI/MS database.

Gas chromatography coupled to atmospheric pressure ionization mass spectrometry (GC-API-MS): Review

Energy Technology Data Exchange (ETDEWEB)

Li, Du-Xin; Gan, Lin; Bronja, Amela [University of Duisburg-Essen, Applied Analytical Chemistry, Universitaetsstr. 5-7, 45141 Essen (Germany); Schmitz, Oliver J., E-mail: oliver.schmitz@uni-due.de [University of Duisburg-Essen, Applied Analytical Chemistry, Universitaetsstr. 5-7, 45141 Essen (Germany)

2015-09-03

Although the coupling of GC/MS with atmospheric pressure ionization (API) has been reported in 1970s, the interest in coupling GC with atmospheric pressure ion source was expanded in the last decade. The demand of a “soft” ion source for preserving highly diagnostic molecular ion is desirable, as compared to the “hard” ionization technique such as electron ionization (EI) in traditional GC/MS, which fragments the molecule in an extensive way. These API sources include atmospheric pressure chemical ionization (APCI), atmospheric pressure photoionization (APPI), atmospheric pressure laser ionization (APLI), electrospray ionization (ESI) and low temperature plasma (LTP). This review discusses the advantages and drawbacks of this analytical platform. After an introduction in atmospheric pressure ionization the review gives an overview about the history and explains the mechanisms of various atmospheric pressure ionization techniques used in combination with GC such as APCI, APPI, APLI, ESI and LTP. Also new developments made in ion source geometry, ion source miniaturization and multipurpose ion source constructions are discussed and a comparison between GC-FID, GC-EI-MS and GC-API-MS shows the advantages and drawbacks of these techniques. The review ends with an overview of applications realized with GC-API-MS. - Highlights: • Atmospheric pressure ion sources (APCI, ESI, APPI, APLC etc) enable the coupling of LC-based high-end MS to GC. • APIs show advantages in selectivity and sensitivity compared with EI in GC-MS. • Accurate mass database in GC-APCI/MS is emerging as an alternative to GC-EI/MS database.

High GC content causes orphan proteins to be intrinsically disordered.

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Walter Basile

2017-03-01

Full Text Available De novo creation of protein coding genes involves the formation of short ORFs from noncoding regions; some of these ORFs might then become fixed in the population. These orphan proteins need to, at the bare minimum, not cause serious harm to the organism, meaning that they should for instance not aggregate. Therefore, although the creation of short ORFs could be truly random, the fixation should be subjected to some selective pressure. The selective forces acting on orphan proteins have been elusive, and contradictory results have been reported. In Drosophila young proteins are more disordered than ancient ones, while the opposite trend is present in yeast. To the best of our knowledge no valid explanation for this difference has been proposed. To solve this riddle we studied structural properties and age of proteins in 187 eukaryotic organisms. We find that, with the exception of length, there are only small differences in the properties between proteins of different ages. However, when we take the GC content into account we noted that it could explain the opposite trends observed for orphans in yeast (low GC and Drosophila (high GC. GC content is correlated with codons coding for disorder promoting amino acids. This leads us to propose that intrinsic disorder is not a strong determining factor for fixation of orphan proteins. Instead these proteins largely resemble random proteins given a particular GC level. During evolution the properties of a protein change faster than the GC level causing the relationship between disorder and GC to gradually weaken.

Differential GC Content between Exons and Introns Establishes Distinct Strategies of Splice-Site Recognition

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Maayan Amit

2012-05-01

Full Text Available During evolution segments of homeothermic genomes underwent a GC content increase. Our analyses reveal that two exon-intron architectures have evolved from an ancestral state of low GC content exons flanked by short introns with a lower GC content. One group underwent a GC content elevation that abolished the differential exon-intron GC content, with introns remaining short. The other group retained the overall low GC content as well as the differential exon-intron GC content, and is associated with longer introns. We show that differential exon-intron GC content regulates exon inclusion level in this group, in which disease-associated mutations often lead to exon skipping. This group's exons also display higher nucleosome occupancy compared to flanking introns and exons of the other group, thus “marking” them for spliceosomal recognition. Collectively, our results reveal that differential exon-intron GC content is a previously unidentified determinant of exon selection and argue that the two GC content architectures reflect the two mechanisms by which splicing signals are recognized: exon definition and intron definition.

Analysis of poly-beta-hydroxybutyrate in environmental samples by GC-MS/MS.

Science.gov (United States)

Elhottová, D; Tríska, J; Petersen, S O; Santrůcková, H

2000-05-01

Application of gas chromatography-mass spectrometry (GC-MS) can significantly improve trace analyses of compounds in complex matrices from natural environments compared to gas chromatography only. A GC-MS/MS technique for determination of poly-beta-hydroxybutyrate (PHB), a bacterial storage compound, has been developed and used for analysis of two soils stored for up to 319 d, fresh samples of sewage sludge, as well as a pure culture of Bacillus megaterium. Specific derivatization of beta-hydroxybutyrate (3-OH C4:0) PHB monomer units by N-tert-butyl-dimethylsilyl-N-methyltrifluoracetamide (MTBSTFA) improved chromatographic and mass spectrometric properties of the analyte. The diagnostic fragmentation scheme of the derivates tert-butyldimethylsilyl ester and ether of beta-hydroxybutyric acid (MTBSTFA-HB) essential for the PHB identification was shown. The ion trap MS was used, therefore the scan gave the best sensitivity and with MS/MS the noise decreased, so the S/N was better and also with second fragmentation the amount of ions increased compared to SIM. The detection limit for MTBSTFA-HB by GC-MS/MS was about 10(-13) g microL(-1) of injected volume, while by GC (FID) and GC-MS (scan) it was around 10(-10) g microL(-1) of injected volume. Sensitivity of GC-MS/MS measurements of PHB in arable soil and activated sludge samples was down to 10 pg of PHB g(-1) dry matter. Comparison of MTBSTFA-HB detection in natural soil sample by GC (FID), GC-MS (scan) and by GC-MS/MS demonstrated potentials and limitations of the individual measurement techniques.

Screening for γ-Nonalactone in the Headspace of Freshly Cooked Non-Scented Rice Using SPME/GC-O and SPME/GC-MS

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Jie Yu Chen

2009-08-01

Full Text Available The determination of γ-nonalactone as one of the important odor-active compounds in freshly cooked non-scented rice is reported. It was evaluated by gas chromatography-olfactometry (GC-O analysis and identified by gas chromatography-mass spectrometry (GC-MS analysis in the headspace above the freshly cooked non-scented rice samples extracted by using a modified headspace solid-phase microextraction (SPME method. This component had a mass spectrum with a characteristic ion peak at m/z 85 (100% and a linear retention index (RI of 2,023 on a DB Wax column, consistent with those of an authentic sample of γ-nonalactone. The odor characterization of a strong, sweet, coconut-like aroma of this compound was also validated by GC-O comparison with the authentic compound.

GENOTYPE DIFFERENCE OF –572 G>C AND -174 G>C IL-6 GENE POLYMORPHISM BETWEEN BALINESE POSTMENOPAUSAL WOMEN WITH OSTEOPOROSIS AND WITHOUT OSTEOPOROSIS

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E Yulianto

2013-09-01

Full Text Available Background: Osteoporosis is a silent metabolic disease characterized by diminished bone mass and change in bone microstructure which cause increment of fracture risk. Until now, osteoporosis still becomes one of major health problems around the world. In Indonesia, the incidence of osteoporosisis 25%. Previous study have shown the relation between osteoporosis and IL-6 gene polymorphism at-572G>C and -174 G>C. There are some controversies about the correlation between thesepolymorphism and osteoporosis because of different result between each study. Genotype G polymorphism at -572 G>C of IL-6 gene has been correlated with lower Bone mineral density (BMD and Genotype G polymorphism at -174G>C of IL-6 gene has been correlated with higher BMD value.In Indonesia, there are still no study about the association between IL-6 gene polymorphism and osteoporosis. In the future this IL-6 gene polymorphism could be used as a genetic marker for osteoporosis in postmenopausal woman. The objective of this study is to determine the difference ofgenotype of -572G>C and -174G>C polymorphism of IL-6 gene and osteoporosis in Balinese postmenopausal women.Method: This research design is a case control study. Sample was obtained at orthopedic outpatient clinic of Sanglah General Hospital, Bali-Indonesia from June 2012 untilNovember 2012. The diagnosis of osteoporosis is described as BMD value with T score ≤ -2.5 SDusing DEXA. All sample’s peripheral blood are taken to be isolated for DNA and analyzed for IL-6 gene polymorphism at -572G>C and -174G>C using Real Time PCR. Data obtained was analyzed with chi square test using SPSS.Results: This research found 11 osteoporosis sample from total 52 with no difference sample characteristic between case and control (p > 0.05. Using Chi square test,There was a significant differences between genotype -572 G>C; IL-6 gene polymorphism in Balinese postmenopausal woman with osteoporosis and in Balinese

Determination of fatty acids and volatile compounds in fruits of rosehip(Rosa L.) species by HS-SPME/GC-MS and Im-SPME/GC-MS techniques

OpenAIRE

MURATHAN, ZEHRA TUĞBA; ZARIFIKHOSROSHAHI, MOZGAN; KAFKAS, NESİBE EBRU

2016-01-01

In this study, we aimed to compare fatty acid and volatile compound compositions of four rosehip species, namely Rosa pimpinellifolia, R. Villosa, R. Canina, and R. Dumalis, by gas chromatography with flame ionization detector (GC/FID) and headspace and immersion solid-phase microextraction gas chromatography-mass spectrometry (HS-SPME/GC-MS and Im-SPME/GC-MS) techniques. The total lipid contents in fruits of the rosehip species varied from 5.83% (R. Villosa) to 7.84% (R. Dumalis). A total of...

Improvement of Ylang-Ylang Essential Oil Characterization by GC×GC-TOFMS

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Michał Brokl

2013-01-01

Full Text Available A single fraction of essential oil can often contain hundreds of compounds. Despite of the technical improvements and the enhanced selectivity currently offered by the state-of-the-art gas chromatography (GC and mass spectrometry (MS instruments, the complexity of essential oils is frequently underestimated. Comprehensive two-dimensional GC coupled to time-of-flight MS (GC×GC-TOFMS was used to improve the chemical characterization of ylang-ylang essential oil fractions recently reported in a previous one-dimensional (1D GC study. Based on both, the enhanced chromatographic separation and the mass spectral deconvolution, 161 individual compounds were identified and labeled as potentially characteristic analytes found in both low and high boiling fractions issued from distillation of mature ylang-ylang flowers. Compared to the most recent full GC-MS characterization, this represents 75 new compounds, essentially consisting of terpenes, terpenoid esters, and alcohols.

GC ‘Multi-Analyte’ Detection Method

Energy Technology Data Exchange (ETDEWEB)

Dudar, E. [Plant Protection & Soil Conservation Service of Budapest, Budapest (Hungary)

2009-07-15

Elaborated methodologies for GC multi-analyte detection are presented, comprising the steps of method development, chromatographic conditions and procedures including the determination of relative retention times and summary results tables. (author)

Gas chromatography coupled to atmospheric pressure ionization mass spectrometry (GC-API-MS): review.

Science.gov (United States)

Li, Du-Xin; Gan, Lin; Bronja, Amela; Schmitz, Oliver J

2015-09-03

Although the coupling of GC/MS with atmospheric pressure ionization (API) has been reported in 1970s, the interest in coupling GC with atmospheric pressure ion source was expanded in the last decade. The demand of a "soft" ion source for preserving highly diagnostic molecular ion is desirable, as compared to the "hard" ionization technique such as electron ionization (EI) in traditional GC/MS, which fragments the molecule in an extensive way. These API sources include atmospheric pressure chemical ionization (APCI), atmospheric pressure photoionization (APPI), atmospheric pressure laser ionization (APLI), electrospray ionization (ESI) and low temperature plasma (LTP). This review discusses the advantages and drawbacks of this analytical platform. After an introduction in atmospheric pressure ionization the review gives an overview about the history and explains the mechanisms of various atmospheric pressure ionization techniques used in combination with GC such as APCI, APPI, APLI, ESI and LTP. Also new developments made in ion source geometry, ion source miniaturization and multipurpose ion source constructions are discussed and a comparison between GC-FID, GC-EI-MS and GC-API-MS shows the advantages and drawbacks of these techniques. The review ends with an overview of applications realized with GC-API-MS. Copyright © 2015. Published by Elsevier B.V.

Rendimento quântico e trocas gasosas em maracujazeiro amarelo sob salinidade hídrica, biofertilização e cobertura morta

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José Lucínio de Oliveira Freire

Full Text Available Um experimento foi conduzido a céu aberto no município de Remígio, PB, para se avaliar as respostas do maracujazeiro amarelo relacionadas à eficiência fotossintética e trocas gasosas. O delineamento experimental utilizado foi em blocos casualizados, no esquema fatorial 2 x 2 x 2, referente à irrigação com água não salina (0,5 dS m-1 e salina (4,5 dS m-1, sem e com biofertilizante bovino, sem e com cobertura morta, com três repetições e três plantas por parcela, em recipientes plásticos circulares utilizados como lisímetros de pressão, com 130 dm³ de volume e drenos na parte inferior para a lixiviação do excesso de sais. A irrigação com água de baixa salinidade e aplicação de biofertilizante bovino comum estimularam a eficiência fotossintética das plantas. O uso simultâneo de água de alta salinidade, biofertilizante e cobertura morta reduziram a condutância estomática do maracujazeiro amarelo. As plantas sob estresse salino apresentaram atividade fotoquímica do fotossistema II e fotossíntese líquida inibida.

Modelagem de um reator integral aplicado na reação de reforma a vapor de metano - DOI: 10.4025/actascitechnol.v29i2.705

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Giane Gonçalves Lenzi

2008-02-01

Full Text Available Freqüentemente, a validação de modelos matemáticos aplicados a reatores industriais esbarra na dificuldade de obtenção de medidas experimentais confiáveis. Uma maneira de contornar esta limitação corresponde à implantação de uma unidade em escala de bancada devidamente instrumentada, na qual são obtidos dados experimentais em condições controladas. Neste contexto, foram efetuados ensaios em um reator integral de reforma a vapor de metano em escala de bancada, em diversas condições experimentais. As medidas de temperatura no leito foram efetuadas por meio de um termopar multiponto em seis posições axiais distintas, enquanto a composição do efluente do reator foi determinada por cromatografia gasosa. Estes dados experimentais foram comparados com as previsões de um modelo pseudo-homogêneo, unidimensional e dinâmico. Os resultados indicam que o modelo é adequado, sendo que tanto a atividade catalítica como a conversão são sensíveis à temperatura operacional, enquanto a temperatura do leito é praticamente insensível à vazão nas condições experimentais exploradas.

Determination of Porosity in Shale by Double Headspace Extraction GC Analysis.

Science.gov (United States)

Zhang, Chun-Yun; Li, Teng-Fei; Chai, Xin-Sheng; Xiao, Xian-Ming; Barnes, Donald

2015-11-03

This paper reports on a novel method for the rapid determination of the shale porosity by double headspace extraction gas chromatography (DHE-GC). Ground core samples of shale were placed into headspace vials and DHE-GC measurements of released methane gas were performed at a given time interval. A linear correlation between shale porosity and the ratio of consecutive GC signals was established both theoretically and experimentally by comparing with the results from the standard helium pycnometry method. The results showed that (a) the porosity of ground core samples of shale can be measured within 30 min; (b) the new method is not significantly affected by particle size of the sample; (c) the uncertainties of measured porosities of nine shale samples by the present method range from 0.31 to 0.46 p.u.; and (d) the results obtained by the DHE-GC method are in a good agreement with those from the standard helium pycnometry method. In short, the new DHE-GC method is simple, rapid, and accurate, making it a valuable tool for shale gas-related research and applications.

Combination of capillary GC, GC/MS and 13C-NMR for the characterization of the rhizome oil of Piper betle L. (Piperaceae) from Vietnam

NARCIS (Netherlands)

Thanh, L.; Dung, N.X.; Bighelli, A.; Casanova, J.; Leclercq, P.A.

1997-01-01

The essential oil from the rhizomes of Piper betle L. (betel), collected around Hue, was obtained in 0.20% yield. The oil was examined by a combination of capillary GC and GC/MS. 13C-NMR studies confirmed the structure assignments proposed by retention data and mass spectra of the components with a

Towards comprehensive hydrocarbons analysis of middle distillates by LC-GCxGC.

Science.gov (United States)

Adam, Frédérick; Bertoncini, Fabrice; Thiébaut, Didier; Esnault, Sébastien; Espinat, Didier; Hennion, M C

2007-01-01

The detailed characterization of middle distillates is essential for a better understanding of reactions involved in refining processes. Owing to a higher resolution power and an enhanced sensitivity, but especially to a group-type ordering in the chromatographic plane, comprehensive two-dimensional gas chromatography (GCxGC) offers unsurpassed characterization possibilities for petroleum samples. However, GCxGC fails to totally discriminate naphthenes from unsaturates occurring in hydrotreated diesel samples. This article aims at promoting the implementation of LC-GCxGC for the quantitative determination of hydrocarbon distribution in middle distillates, including naphthenes. In this configuration, liquid chromatography (LC) enables the separation of hydrocarbons into two fractions (viz., saturated and unsaturated) before the subsequent analysis of each fraction by GCxGC. In this paper, the choice of GCxGC conditions in order to achieve the separation and identification of hydrocarbons by chemical class is discussed; under these conditions, naphthenes are separated according to the number of saturated rings. For the first time, the presence of di-, tri-, and tetra-naphthenes resulting from the hydroconversion of aromatics can clearly be evidenced. A quantitative procedure for the determination of the distribution of hydrocarbons, including the distribution of naphthenes according to the number of saturated rings, is also proposed and discussed in detail. LC-GCxGC is found to provide an unequalled degree of information that will widely contribute to a better understanding of hydroconversion processes.

A simple model for the influence of meiotic conversion tracts on GC content.

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Marie-Claude Marsolier-Kergoat

Full Text Available A strong correlation between GC content and recombination rate is observed in many eukaryotes, which is thought to be due to conversion events linked to the repair of meiotic double-strand breaks. In several organisms, the length of conversion tracts has been shown to decrease exponentially with increasing distance from the sites of meiotic double-strand breaks. I show here that this behavior leads to a simple analytical model for the evolution and the equilibrium state of the GC content of sequences devoid of meiotic double-strand break sites. In the yeast Saccharomyces cerevisiae, meiotic double-strand breaks are practically excluded from protein-coding sequences. A good fit was observed between the predictions of the model and the variations of the average GC content of the third codon position (GC3 of S. cerevisiae genes. Moreover, recombination parameters that can be extracted by fitting the data to the model coincide with experimentally determined values. These results thus indicate that meiotic recombination plays an important part in determining the fluctuations of GC content in yeast coding sequences. The model also accounted for the different patterns of GC variations observed in the genes of Candida species that exhibit a variety of sexual lifestyles, and hence a wide range of meiotic recombination rates. Finally, the variations of the average GC3 content of human and chicken coding sequences could also be fitted by the model. These results suggest the existence of a widespread pattern of GC variation in eukaryotic genes due to meiotic recombination, which would imply the generality of two features of meiotic recombination: its association with GC-biased gene conversion and the quasi-exclusion of meiotic double-strand breaks from coding sequences. Moreover, the model points out to specific constraints on protein fragments encoded by exon terminal sequences, which are the most affected by the GC bias.

Both selective and neutral processes drive GC content evolution in the human genome

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Cagliani Rachele

2008-03-01

Full Text Available Abstract Background Mammalian genomes consist of regions differing in GC content, referred to as isochores or GC-content domains. The scientific debate is still open as to whether such compositional heterogeneity is a selected or neutral trait. Results Here we analyze SNP allele frequencies, retrotransposon insertion polymorphisms (RIPs, as well as fixed substitutions accumulated in the human lineage since its divergence from chimpanzee to indicate that biased gene conversion (BGC has been playing a role in within-genome GC content variation. Yet, a distinct contribution to GC content evolution is accounted for by a selective process. Accordingly, we searched for independent evidences that GC content distribution does not conform to neutral expectations. Indeed, after correcting for possible biases, we show that intron GC content and size display isochore-specific correlations. Conclusion We consider that the more parsimonious explanation for our results is that GC content is subjected to the action of both weak selection and BGC in the human genome with features such as nucleosome positioning or chromatin conformation possibly representing the final target of selective processes. This view might reconcile previous contrasting findings and add some theoretical background to recent evidences suggesting that GC content domains display different behaviors with respect to highly regulated biological processes such as developmentally-stage related gene expression and programmed replication timing during neural stem cell differentiation.

Aplicação de métodos quimiométricos na caracterização de charutos utilizando extração por dispersão da matriz em fase sólida e análise por cromatografia gasosa acoplada à espectrometria de massas

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Vanessa de Menezes Prata

2011-01-01

Full Text Available In this work, the organic compounds of cigar samples from different brands were analyzed. The compound extraction was made using the matrix solid-phase dispersion (MSPD technique, followed by gas chromatography and identification by mass spectrometry (GC-MS and standards, when available. Thirty eight organic compounds were found in seven different brands. Finally, with the objective of characterizing and discriminating the cigar samples, multivariate statistical analyses were applied to data, e.g.; principal component analysis (PCA and hierarchical cluster analysis (HCA. With such analyses, it was possible to discriminate three main groups of three quality levels.

An ingenious strategy of preparing TiO2/g-C3N4 heterojunction photocatalyst: In situ growth of TiO2 nanocrystals on g-C3N4 nanosheets via impregnation-calcination method

Science.gov (United States)

Zhang, Guanghui; Zhang, Tianyong; Li, Bin; Jiang, Shuang; Zhang, Xia; Hai, Li; Chen, Xingwei; Wu, Wubin

2018-03-01

An ingenious method was employed to design and fabricate the TiO2/g-C3N4 heterojunction photocatalysts in this study. The thermal oxidation etching of g-C3N4 nanosheets and the in situ growth of TiO2 nanocrystal on the surface of g-C3N4 nanosheets were completed simultaneously by the calcination process. The g-C3N4 nanosheets played a crucial role in regulating and assembling the structures and morphologies of TiO2. Furthermore, the thickness and content of g-C3N4, and the crystallinity of TiO2 in TiO2/g-C3N4 composites could be regulated and controlled by the calcination temperature. Among the resultant TiO2/g-C3N4 samples, the TiO2/g-C3N4 sample with 41.6 wt% g-C3N4 exhibited the highest photocatalytic activity. It could degrade almost all MO molecules under visible light irradiation within 3 h. Moreover, it displayed higher visible light photocatalytic performance for degrading MO solution than pure g-C3N4 and D-TiO2. The synergistic effect between TiO2 and g-C3N4 makes significant contributions to the enhancement of the visible light photocatalytic activity. In addition, the favorable photocatalytic performance of TiO2/g-C3N4 nanocomposites is also attributed to the porous structures and uniform morphologies, and large surface area. Furthermore, the resultant TiO2/g-C3N4 exhibits excellent photocatalytic stability. Radical trapping experiments indicated that rad O2- and h+ were the main reactive species during the photodegradation process under visible light irradiation. Hopefully, the results can offer new design and strategy for preparing other g-C3N4-based nanocomposites for environmental and energy applications.

Antitumor effect of degalactosylated gc-globulin on orthotopic grafted lung cancer in mice.

Science.gov (United States)

Hirota, Keiji; Nakagawa, Yoshinori; Takeuchi, Ryota; Uto, Yoshihiro; Hori, Hitoshi; Onizuka, Shinya; Terada, Hiroshi

2013-07-01

Group-specific component (Gc)-globulin-derived macrophage-activating factor (GcMAF) generated by a cascade of catalytic reactions with deglycosidase enzymes exerts antitumor activity. We hypothesized that degalactosyl Gc-globulin (DG3), a precursor of GcMAF, also plays a role in recovery from cancer as well as GcMAF due to progression of deglycosylation by generally resident sialidases and mannosidases. We prepared the subtypes of DG3, such as 1f1f and 1s1s and its 22 homodimers, by using vitamin D3-binding Sepharose CL-6B and examined their antitumor activity in mice bearing Lewis lung carcinoma cells, by counting the number of nodules formed in their lungs. Antitumor activity of DG3 was observed regardless of its subtype, being equivalent to that of GcMAF. The injection route of DG3 affected its antitumor activity, with subcutaneous and intramuscular administration being more favorable than the intraperitoneal or intravenous route. In order to obtain significant antitumor activity, more than 160 ng/kg of DG3 were required. DG3 proved to be promising as an antitumor agent, similarly to GcMAF.

Effects of vitamin D(3)-binding protein-derived macrophage activating factor (GcMAF) on angiogenesis.

Science.gov (United States)

Kanda, Shigeru; Mochizuki, Yasushi; Miyata, Yasuyoshi; Kanetake, Hiroshi; Yamamoto, Nobuto

2002-09-04

The vitamin D(3)-binding protein (Gc protein)-derived macrophage activating factor (GcMAF) activates tumoricidal macrophages against a variety of cancers indiscriminately. We investigated whether GcMAF also acts as an antiangiogenic factor on endothelial cells. The effects of GcMAF on angiogenic growth factor-induced cell proliferation, chemotaxis, and tube formation were examined in vitro by using cultured endothelial cells (murine IBE cells, porcine PAE cells, and human umbilical vein endothelial cells [HUVECs]) and in vivo by using a mouse cornea micropocket assay. Blocking monoclonal antibodies to CD36, a receptor for the antiangiogenic factor thrombospondin-1, which is also a possible receptor for GcMAF, were used to investigate the mechanism of GcMAF action. GcMAF inhibited the endothelial cell proliferation, chemotaxis, and tube formation that were all stimulated by fibroblast growth factor-2 (FGF-2), vascular endothelial growth factor-A, or angiopoietin 2. FGF-2-induced neovascularization in murine cornea was also inhibited by GcMAF. Monoclonal antibodies against murine and human CD36 receptor blocked the antiangiogenic action of GcMAF on the angiogenic factor stimulation of endothelial cell chemotaxis. In addition to its ability to activate tumoricidal macrophages, GcMAF has direct antiangiogenic effects on endothelial cells independent of tissue origin. The antiangiogenic effects of GcMAF may be mediated through the CD36 receptor.

Environmental trace analysis by means of supersensitive GC-IMS

International Nuclear Information System (INIS)

Leonhardt, J.W.

1997-01-01

The effective control of pollutants in ambient air requires their fast in situ identification and concentration determination of chemical compounds in the range of micrograms per m 3 . There are attempts to use conventional analytical techniques as portable GC and GC-MS. These systems are relatively expensive. A new supersensitive ion Mobility Sensor (IMS) was developed and checked by IUT Ltd, which meets the new demands. The use of tritium sources is an advantage in comparison with other IMS being equipped by nickel-63, the application of which is rather critical in respect of the radiation protection. On the other hand an integrated separation column allows to reduce interferences by matrix effects. The technical parameters of the IUT GC- IMS and some of its most important applications are briefly presented

[Study on rapid analysis method of pesticide contamination in processed foods by GC-MS and GC-FPD].

Science.gov (United States)

Kobayashi, Maki; Otsuka, Kenji; Tamura, Yasuhiro; Tomizawa, Sanae; Kamijo, Kyoko; Iwakoshi, Keiko; Sato, Chizuko; Nagayama, Toshihiro; Takano, Ichiro

2011-01-01

A simple and rapid method using GC-MS and GC-FPD for the determination of pesticide contamination in processed food has been developed. Pesticides were extracted from a sample with ethyl acetate in the presence of anhydrous sodium sulfate, then cleaned up with a combination of mini-columns, such as macroporous diatomaceous earth, C18, GCB (graphite carbon black) and PSA. Recovery tests of 57 pesticides (known to be toxic or harmful) from ten kinds of processed foods (butter, cheese, corned beef, dried shrimp, frozen Chinese dumplings, grilled eels, instant noodles, kimchi, retort-packed curry and wine) were performed, and the recovery rates were mostly between 70% and 120%. This method can be used to judge whether or not processed foods are contaminated with pesticides at potentially harmful levels.

Performance of the future MOMA GC-ITMS instrument

Science.gov (United States)

Grand, Noel; Buch, Arnaud; Veronica, Pinnick; Szopa, Cyril; Danell, Ryan; Van Amerom, Friso H. W.; Glavin, Daniel P.; Freissinet, Caroline; Arevalo, Ricardo; Stalport, Fabien; Getty, Stephanie; Coll, Patrice; Steinninger, Harald; Brinckerhoff, William; Mahaffy, Paul; Goesmann, Fred; Raulin, F.; Goetz, Walter; MOMA Team

2016-10-01

The Mars Organic Molecule Analyzer (MOMA) experiment aboard the future ExoMars mission will be the continuation of the SAM expirement aboard the Curiosity rover, with the search for the organic composition of the Mars surface. With ExoMars the sample will be extracted as deep as 2 meters below the martian surface to minimize effects of radiation and oxidation on organic materials. To analyze the wide range of organic composition (volatile and non-volatiles compounds) of the Martian soil MOMA is composed with an UV laser desorption / ionization (LDI) and a pyrolysis gas chromatography ion trap mass spectrometry (pyr-GC-ITMS). In order to analyze refractory organic compounds and chirality samples which undergo GC-ITMS analysis may be submitted to a derivatization process, consisting of the reaction of the sample components with specific reactants (MTBSTFA [1], DMF-DMA [2] or TMAH [3]).To optimize and test the performance of the GC-ITMS instrument we have performed several coupling tests campaigns between the GC, providing by the French team (LISA, LATMOS, CentraleSupelec), and the MS, providing by the US team (NASA, GSFC). Last campaign has been done with the ETU models which is similar to the flight model and which include the oven and the taping station providing by the German team (MPS).The results obtained demonstrate the current status of the end-to-end performance of the gas chromatography-mass spectrometry mode of operation.

Influência da enxertia nas trocas gasosas de dois híbridos de berinjela cultivados em ambiente protegido

Directory of Open Access Journals (Sweden)

Brandão Filho José Usan T.

2003-01-01

Full Text Available Compararam-se os efeitos da enxertia nas trocas gasosas de dois híbridos de berinjela em pé franco e enxertado. Conduziu-se um ensaio em ambiente protegido, na FCA/UNESP, em estrutura simples, tipo arco com 7 m de largura, 40 m de comprimento e 3 m de pé direito, cobertos por filme plástico de 100 micrometros. Foram utilizados os híbridos de berinjela Nápoli e Kokuyo, enxertados em porta-enxerto específico (híbrido Taibyo VF para esta espécie. O delineamento experimental utilizado foi inteiramente casualizado, com quatro tratamentos (Nápoli pé franco, Nápoli enxertada, Kokuyo pé franco e Kokuyo enxertada com dez repetições. A assimilação líquida de CO2 (A, transpiração (E, condutância estomática (g s e eficiência no uso de água (EUA, obtida pela relação (A/E, foram determinadas às 09:00; 12:00; 14:00 e 16:00 horas em um dia sem nebulosidade com fluxo de fótons fotossinteticamente ativos (FFFA de 937±126 mmol m-2 s-1, com um sistema fechado portátil de fotossíntese, IRGA, modelo LI-6200 (LI-COR. Observou-se que as plantas do híbrido Kokuyo apresentaram maiores valores para as variáveis A, E, g s e EUA que o híbrido Nápoli. A enxertia não afetou a capacidade fotossintética dos híbridos, porém, esta resultou em menores valores de E e g s nos dois híbridos, levando à maior EUA, efeito este que na prática pode resultar em menor demanda de água pelas plantas.

Comportamento sazonal do potencial hídrico e das trocas gasosas de quatro variedades de coqueiro-anão Seasonal performance of water potential and gas exchange in four varietes of dwarf coconut

Directory of Open Access Journals (Sweden)

Cíntia Dória Passos

2005-08-01

Full Text Available Avaliou-se o curso diurno e sazonal do potencial hídrico e das trocas gasosas foliares do coqueiro-anão (Cocos nucifera L. sob condições de campo, no município de Ilha das Flores-SE. As quatro variedades estudadas (Anão Vermelho de Camarões - AVC, Anão Vermelho de Gramame - AVG, Anão Amarelo de Gramame - AAG e Anão Verde de Jiqui - AveJ reduziram drasticamente a condutância estomática (gs no período seco. Sob estiagem, os valores de transpiração (E e fotossíntese líquida (A foram reduzidos principalmente nas variedades AVG e AVeJ, as quais apresentaram aumento significativo nos valores de eficiência intrínseca do uso da água (A/gs, principalmente o AVeJ. Na estação chuvosa, as trocas gasosas foram condicionadas pela densidade de fluxo de fótons fotossinteticamente ativos (DFFFA e pela gs. No entanto, durante a estação seca, as trocas gasosas foram condicionadas somente pelos valores de gs, sendo os valores de DFFFA não-limitantes desde as primeiras horas do dia. A variedade AVC apresentou pouca eficiência no controle da perda de água pela transpiração sob condições de estresse hídrico, atingindo os valores mais negativos do potencial hídrico foliar, mantendo, todavia, a fotossíntese líquida mais elevada durante o curso diurno. Por outro lado, o AVeJ controlou eficientemente a transpiração e, mesmo com menores valores de A, apresentou a maior razão A/gs que as demais variedades. Em cultivo tecnificado, como ocorre nos perímetros irrigados, a variedade AVC deverá manter um balanço de carbono mais favorável durante todo o ano, apresentando-se como uma variedade muito promissora.Leaf gas exchange and water potential (psil were assessed daily and seasonaly in four varieties of dwarf coconut (Cocos nuficera L. under field conditions: Cameroon Red Dwarf (CRD, Gramame Red Dwarf (GRD, Gramame yellow Dwarf (GYD and Jiqui Green Dwarf (JGD. All varieties showed strong reduction of stomatal conductance (gs values in

1000 human genomes carry widespread signatures of GC biased gene conversion.

Science.gov (United States)

Dutta, Rajib; Saha-Mandal, Arnab; Cheng, Xi; Qiu, Shuhao; Serpen, Jasmine; Fedorova, Larisa; Fedorov, Alexei

2018-04-16

GC-Biased Gene Conversion (gBGC) is one of the important theories put forward to explain profound long-range non-randomness in nucleotide compositions along mammalian chromosomes. Nucleotide changes due to gBGC are hard to distinguish from regular mutations. Here, we present an algorithm for analysis of millions of known SNPs that detects a subset of so-called "SNP flip-over" events representing recent gBGC nucleotide changes, which occurred in previous generations via non-crossover meiotic recombination. This algorithm has been applied in a large-scale analysis of 1092 sequenced human genomes. Altogether, 56,328 regions on all autosomes have been examined, which revealed 223,955 putative gBGC cases leading to SNP flip-overs. We detected a strong bias (11.7% ± 0.2% excess) in AT- > GC over GC- > AT base pair changes within the entire set of putative gBGC cases. On average, a human gamete acquires 7 SNP flip-over events, in which one allele is replaced by its complementary allele during the process of meiotic non-crossover recombination. In each meiosis event, on average, gBGC results in replacement of 7 AT base pairs by GC base pairs, while only 6 GC pairs are replaced by AT pairs. Therefore, every human gamete is enriched by one GC pair. Happening over millions of years of evolution, this bias may be a noticeable force in changing the nucleotide composition landscape along chromosomes.

Integrated multidimensional and comprehensive 2D GC analysis of fatty acid methyl esters.

Science.gov (United States)

Zeng, Annie Xu; Chin, Sung-Tong; Marriott, Philip J

2013-03-01

Fatty acid methyl ester (FAME) profiling in complex fish oil and milk fat samples was studied using integrated comprehensive 2D GC (GC × GC) and multidimensional GC (MDGC). Using GC × GC, FAME compounds--cis- and trans-isomers, and essential fatty acid isomers--ranging from C18 to C22 in fish oil and C18 in milk fat were clearly displayed in contour plot format according to structural properties and patterns, further identified based on authentic standards. Incompletely resolved regions were subjected to MDGC, with Cn (n = 18, 20) zones transferred to a (2)D column. Elution behavior of C18 FAME on various (2)D column phases (ionic liquids IL111, IL100, IL76, and modified PEG) was evaluated. Individual isolated Cn zones demonstrated about four-fold increased peak capacities. The IL100 provided superior separation, good peak shape, and utilization of elution space. For milk fat-derived FAME, the (2)D chromatogram revealed at least three peaks corresponding to C18:1, more than six peaks for cis/trans-C18:2 isomers, and two peaks for C18:3. More than 17 peaks were obtained for the C20 region of fish oil-derived FAMEs using MDGC, compared with ten peaks using GC × GC. The MDGC strategy is useful for improved FAME isomer separation and confirmation. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Enhanced photocatalytic ozonation of organics by g-C3N4 under visible light irradiation

International Nuclear Information System (INIS)

Liao, Gaozu; Zhu, Dongyun; Li, Laisheng; Lan, Bingyan

2014-01-01

Highlights: • g-C 3 N 4 is employed as active catalyst in the photocatalytic ozonation system. • The more negative conduction band of g-C 3 N 4 benefits the transfer of electrons. • The synergistic effect between photocatalysis and ozonation is promoted by g-C 3 N 4 . • Enhanced degradation of oxalic acid and biphenol A is achieved via g-C 3 N 4 /Vis/O 3 . - Abstract: Graphitic carbon nitride (g-C 3 N 4 ) was employed as the active photocatalyst in the photocatalytic ozonation coupling system in the present study. g-C 3 N 4 was prepared by directly heating thiourea in air at 550 °C. XRD, FT-IR, UV–vis was used to characterize the structure and optical property. Oxalic acid and bisphenol A were selected as model substances for photocatalytic ozonation reactions to evaluate the catalytic ability of g-C 3 N 4 (g-C 3 N 4 /Vis/O 3 ). The results showed that the degradation ratio of oxalic acid with g-C 3 N 4 /Vis/O 3 was 65.2% higher than the sum of ratio when it was individually decomposed by g-C 3 N 4 /Vis and O 3 . The TOC removal of biphenol A with g-C 3 N 4 /Vis/O 3 was 2.17 times as great as the sum of the ratio when using g-C 3 N 4 /Vis and O 3 . This improvement was attributed to the enhanced synergistic effect between photocatalysis and ozonation by g-C 3 N 4 . Under visible light irradiation, the photo-generated electrons produced on g-C 3 N 4 facilitated the electrons transfer owing to the more negative conduction band potential (−1.3 V versus NHE). It meant that the photo-generated electrons could be trapped by ozone and reaction with it more easily. Subsequently, the yield of hydroxyl radicals was improved so as to enhance the organics degradation efficiency. This work indicated that metal-free g-C 3 N 4 could be an excellent catalyst for mineralization of organic compounds in waste control

Environmental trace analysis by means of supersensitive GC-IMS

Energy Technology Data Exchange (ETDEWEB)

Leonhardt, J.W. [IUTLimited, Berlin, (Germany)

1997-10-01

The effective control of pollutants in ambient air requires their fast in situ identification and concentration determination of chemical compounds in the range of micrograms per m{sup 3}. There are attempts to use conventional analytical techniques as portable GC and GC-MS. These systems are relatively expensive. A new supersensitive ion Mobility Sensor (IMS) was developed and checked by IUT Ltd, which meets the new demands. The use of tritium sources is an advantage in comparison with other IMS being equipped by nickel-63, the application of which is rather critical in respect of the radiation protection. On the other hand an integrated separation column allows to reduce interferences by matrix effects. The technical parameters of the IUT GC- IMS and some of its most important applications are briefly presented 6 refs., 1 tab., 5 figs.

GC content around splice sites affects splicing through pre-mRNA secondary structures

Directory of Open Access Journals (Sweden)

Chen Liang

2011-01-01

Full Text Available Abstract Background Alternative splicing increases protein diversity by generating multiple transcript isoforms from a single gene through different combinations of exons or through different selections of splice sites. It has been reported that RNA secondary structures are involved in alternative splicing. Here we perform a genomic study of RNA secondary structures around splice sites in humans (Homo sapiens, mice (Mus musculus, fruit flies (Drosophila melanogaster, and nematodes (Caenorhabditis elegans to further investigate this phenomenon. Results We observe that GC content around splice sites is closely associated with the splice site usage in multiple species. RNA secondary structure is the possible explanation, because the structural stability difference among alternative splice sites, constitutive splice sites, and skipped splice sites can be explained by the GC content difference. Alternative splice sites tend to be GC-enriched and exhibit more stable RNA secondary structures in all of the considered species. In humans and mice, splice sites of first exons and long exons tend to be GC-enriched and hence form more stable structures, indicating the special role of RNA secondary structures in promoter proximal splicing events and the splicing of long exons. In addition, GC-enriched exon-intron junctions tend to be overrepresented in tissue-specific alternative splice sites, indicating the functional consequence of the GC effect. Compared with regions far from splice sites and decoy splice sites, real splice sites are GC-enriched. We also found that the GC-content effect is much stronger than the nucleotide-order effect to form stable secondary structures. Conclusion All of these results indicate that GC content is related to splice site usage and it may mediate the splicing process through RNA secondary structures.

Results of the First Mars Organic Molecule Analyzer (MOMA) GC-MS Coupling

Science.gov (United States)

Buch, Arnaud; Pinnick, Veronica; Szopa, Cyril; Danell, Ryan; Grand, Noel; Van Amerom, Friso; Glavin, Daniel; Freissinet, Caroline; Humeau, Olivier; Coll, Patrice; Arevalo, Ricardo; Stalport, Fabien; Brinckerhoff, William; Steininger, Harald; Goesmann, Fred; Mahaffy, Paul; Raulin, Francois

2014-11-01

The Mars Organic Molecule Analyzer (MOMA) aboard the ExoMars rover will be a key analytical tool in providing chemical (molecular) information from the solid samples collected by the rover, with a particular focus on the char-acterization of the organic content. The core of the MOMA instrument is a gas chromatograph coupled with a mass spectrometer (GC-MS) which provides the unique capability to characterize a broad range of compounds, including both of volatile and non-volatile species. Samples will be crushed and deposited into sample cups seated in a rotating carousel. Soil samples will be analyzed either by UV laser desorption / ionization (LDI) or pyrolysis gas chromatography ion trap mass spectrometry (pyr-GC-ITMS).The French GC brassboard was coupled to the US ion trap mass spectrometer brassboard in a flight-like con-figuration for several coupling campains. The MOMA GC setup is based on the SAM heritage design with a He reservoir and 4 separate analytical modules including traps, columns and Thermal Conductivity Detectors. Solid samples are sealed and heated in this setup using a manual tapping station, designed and built at MPS in Germany, for GC-MS analysis. The gaseous species eluting from the GC are then ionized by an electron impact ionization source in the MS chamber and analyzed by the linear ion trap mass spectrometer. Volatile and non-volatile compounds were injected in the MOMA instrumental suite. Both of these compounds classes were detected by the TCD and by the MS. MS signal (total ion current) and single mass spectra by comparison with the NIST library, gave us an unambiguous confirmation of these identifications. The mass spectra arise from an average of 10 mass spectra averaged around a given time point in the total ion chromatogram.Based on commercial instrument, the MOMA requirement for sensitivity in the GC-MS mode for organic molecules is 1 pmol. In this test, sensitivity was determined for the GC TCD and MS response to a dilution

Degalactosylated/desialylated human serum containing GcMAF induces macrophage phagocytic activity and in vivo antitumor activity.

Science.gov (United States)

Kuchiike, Daisuke; Uto, Yoshihiro; Mukai, Hirotaka; Ishiyama, Noriko; Abe, Chiaki; Tanaka, Daichi; Kawai, Tomohito; Kubo, Kentaro; Mette, Martin; Inui, Toshio; Endo, Yoshio; Hori, Hitoshi

2013-07-01

The group-specific component protein-derived macrophage-activating factor (GcMAF) has various biological activities, such as macrophage activation and antitumor activity. Clinical trials of GcMAF have been carried out for metastatic breast cancer, prostate cancer, and metastatic colorectal cancer. In this study, despite the complicated purification process of GcMAF, we used enzymatically-treated human serum containing GcMAF with a considerable macrophage-stimulating activity and antitumor activity. We detected GcMAF in degalactosylated/desialylated human serum by western blotting using an anti-human Gc globulin antibody, and Helix pomatia agglutinin lectin. We also found that GcMAF-containing human serum significantly enhanced the phagocytic activity of mouse peritoneal macrophages and extended the survival time of mice bearing Ehrlich ascites tumors. We demonstrated that GcMAF-containing human serum can be used as a potential macrophage activator for cancer immunotherapy.

Hantavirus Gc induces long-term immune protection via LAMP-targeting DNA vaccine strategy.

Science.gov (United States)

Jiang, Dong-Bo; Zhang, Jin-Peng; Cheng, Lin-Feng; Zhang, Guan-Wen; Li, Yun; Li, Zi-Chao; Lu, Zhen-Hua; Zhang, Zi-Xin; Lu, Yu-Chen; Zheng, Lian-He; Zhang, Fang-Lin; Yang, Kun

2018-02-01

Hemorrhagic fever with renal syndrome (HFRS) occurs widely throughout Eurasia. Unfortunately, there is no effective treatment, and prophylaxis remains the best option against the major pathogenic agent, hantaan virus (HTNV), which is an Old World hantavirus. However, the absence of cellular immune responses and immunological memory hampers acceptance of the current inactivated HFRS vaccine. Previous studies revealed that a lysosome-associated membrane protein 1 (LAMP1)-targeting strategy involving a DNA vaccine based on the HTNV glycoprotein Gn successfully conferred long-term immunity, and indicated that further research on Gc, another HTNV antigen, was warranted. Plasmids encoding Gc and lysosome-targeted Gc, designated pVAX-Gc and pVAX-LAMP/Gc, respectively, were constructed. Proteins of interest were identified by fluorescence microscopy following cell line transfection. Five groups of 20 female BALB/c mice were subjected to the following inoculations: inactivated HTNV vaccine, pVAX-LAMP/Gc, pVAX-Gc, and, as the negative controls, pVAX-LAMP or the blank vector pVAX1. Humoral and cellular immunity were assessed by enzyme-linked immunosorbent assays (ELISAs) and 15-mer peptide enzyme-linked immunospot (ELISpot) epitope mapping assays. Repeated immunization with pVAX-LAMP/Gc enhanced adaptive immune responses, as demonstrated by the specific and neutralizing antibody titers and increased IFN-γ production. The inactivated vaccine induced a comparable humoral reaction, but the negative controls only elicited insignificant responses. Using a mouse model of HTNV challenge, the in vivo protection conferred by the inactivated vaccine and Gc-based constructs (with/without LAMP recombination) was confirmed. Evidence of pan-epitope reactions highlighted the long-term cellular response to the LAMP-targeting strategy, and histological observations indicated the safety of the LAMP-targeting vaccines. The long-term protective immune responses induced by pVAX-LAMP/Gc may be

Quantification of acetaminophen (paracetamol) in human plasma and urine by stable isotope-dilution GC-MS and GC-MS/MS as pentafluorobenzyl ether derivative.

Science.gov (United States)

Trettin, Arne; Zoerner, Alexander A; Böhmer, Anke; Gutzki, Frank-Mathias; Stichtenoth, Dirk O; Jordan, Jens; Tsikas, Dimitrios

2011-08-01

We report on the quantitative determination of acetaminophen (paracetamol; NAPAP-d(0)) in human plasma and urine by GC-MS and GC-MS/MS in the electron-capture negative-ion chemical ionization (ECNICI) mode after derivatization with pentafluorobenzyl (PFB) bromide (PFB-Br). Commercially available tetradeuterated acetaminophen (NAPAP-d(4)) was used as the internal standard. NAPAP-d(0) and NAPAP-d(4) were extracted from 100-μL aliquots of plasma and urine with 300 μL ethyl acetate (EA) by vortexing (60s). After centrifugation the EA phase was collected, the solvent was removed under a stream of nitrogen gas, and the residue was reconstituted in acetonitrile (MeCN, 100 μL). PFB-Br (10 μL, 30 vol% in MeCN) and N,N-diisopropylethylamine (10 μL) were added and the mixture was incubated for 60 min at 30 °C. Then, solvents and reagents were removed under nitrogen and the residue was taken up with 1000 μL of toluene, from which 1-μL aliquots were injected in the splitless mode. GC-MS quantification was performed by selected-ion monitoring ions due to [M-PFB](-) and [M-PFB-H](-), m/z 150 and m/z 149 for NAPAP-d(0) and m/z 154 and m/z 153 for NAPAP-d(4), respectively. GC-MS/MS quantification was performed by selected-reaction monitoring the transition m/z 150 → m/z 107 and m/z 149 → m/z 134 for NAPAP-d(0) and m/z 154 → m/z 111 and m/z 153 → m/z 138 for NAPAP-d(4). The method was validated for human plasma (range, 0-130 μM NAPAP-d(0)) and urine (range, 0-1300 μM NAPAP-d(0)). Accuracy (recovery, %) ranged between 89 and 119%, and imprecision (RSD, %) was below 19% in these matrices and ranges. A close correlation (r>0.999) was found between the concentrations measured by GC-MS and GC-MS/MS. By this method, acetaminophen can be reliably quantified in small plasma and urine sample volumes (e.g., 10 μL). The analytical performance of the method makes it especially useful in pediatrics. Copyright © 2011 Elsevier B.V. All rights reserved.

Unconventionally prepared TiO2/g-C3N4 photocatalysts for photocatalytic decomposition of nitrous oxide

Science.gov (United States)

Troppová, Ivana; Šihor, Marcel; Reli, Martin; Ritz, Michal; Praus, Petr; Kočí, Kamila

2018-02-01

The TiO2/g-C3N4 nanocomposites with the various TiO2:g-C3N4 weight ratios from 1:1 to 1:3 were prepared unconventionally by pressurized hot water processing in a flow regime. The parent TiO2 and g-C3N4 was prepared by thermal hydrolysis and thermal annealing, respectively. The nanocomposites as well as parent TiO2 and g-C3N4 were characterized using several complementary characterization methods and investigated in the photocatalytic decomposition of N2O under UVA (λ = 365 nm) irradiation. All the prepared TiO2/g-C3N4 nanocomposites showed higher photocatalytic activity in comparison with the pure g-C3N4 and chiefly pure TiO2. The photocatalytic activity of TiO2/g-C3N4 nanocomposites was decreasing in the following sequence: TiO2/g-C3N4 (1:3) > TiO2/g-C3N4 (1:2) > TiO2/g-C3N4 (1:1). In comparison with the parent TiO2 or g-C3N4, the TiO2/g-C3N4 nanocomposites' photocatalytic capability was significantly enhanced by coupling TiO2 with g-C3N4. The generation of TiO2/g-C3N4 Z-scheme photocatalyst mainly benefited from the effective separation of photoinduced electron-hole pairs and the extended optical absorption range. The TiO2/g-C3N4 (1:3) nanocomposite showed the best photocatalytic behavior in a consequence of the optimal weight ratio of TiO2:g-C3N4 and the lowest band gap energy from all nanocomposites. The N2O conversion in its presence was 70.6% after 20 h of UVA irradiation.

Analysis of residual solvents in PET radiopharmaceuticals by GC

International Nuclear Information System (INIS)

Li Yungang; Zhang Xiaojun; Liu Jian; Tian Jiahe; Zhang Jinming

2013-01-01

The residual solvents in PET radiopharmaceuticals were analyzed by GC, which were acetonitrile, ethanol, N, N-dimethylethanolamine (DMEA), dimethylsulfoxide (DMSO). The standard curves were established with the AT-624 capillary column at GC, and the sensitivity of acetonitrile and ethanol were 0.004-0.320 g/L and 0.010-0.120 g/L respectively. The residual solvents of acetonitrile, ethanol, DMEA and DMSO in PET radio- pharmaceuticals were analyzed by GC. The linearity were 0.9994, 0.9999, 0.9997, 0.999 6 respectively. The residual of acetonitrile were (0.0313±0.0433), (0.0829±0.0668), (0.0156±0.0059), (0.0254±0.0266) g/L in 18 F-FDG, 18 F-FLT, 11 C-CFT, 11 C-PIB respectively. The residual of ethanol was (0.0505±0.00528) g/L in 18 F-FDG. The residual of DMSO were (0.0331±0.0180) g/L, (0.0238±0.0100) g/L in 18 F-W372 and 11 C-DTBZ respectively. The residual of DMEA was (0.0348±0.0022) g/L in 11 C-Choline. The survived of organic solvent in PET radiopharmaceuticals can be analyzed with GC directly. The results showed that the QC should be done in PET radiopharmaceuticals purity with semi-HPLC to avoid the high residual. (authors)

Determinação de metil-etil-cetona em amostras de urina com amostragem por micro extração em fase sólida (MEFS em headspace associada à cromatografia gasosa com detector de ionização de chama (CG-DIC Determination of methyl ethyl ketone in urine samples by headspace solid phase micro extraction (SPME sampling associated to gas chromatography with flame-ionization detectoR (GC-FID

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Marina Venzon Antunes

2008-01-01

Full Text Available Methyl ethyl ketone (MEK is a solvent commonly used in chemical, paint and shoe industry. The aim of this study was to develop and validate a method for urinary quantification of MEK, employing headspace solid phase micro extraction sampling (SPME coupled to gas chromatography with flame ionization detection (GC-FID. The calibration curve (y=4.6851x-0.0011 presented good linearity with r²=0.9993. Accuracy (94-109%, intra-assay precision (4.07-5.91% and inter-assay precision (3.03-5.62% were acceptable. The quantification limit was 0.19 mg/L. This low cost method can be used routinely in the biological monitoring of occupational exposure to MEK, according to the requirements of the Brazilian legislation.

Determinação de daidzeína, genisteína e gliciteína em cápsulas de isoflavonas por cromatografia em camada delgada (CCD e cromatografia líquida de alta eficiência (CLAE

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Isabela da Costa César

Full Text Available A utilização de produtos naturais e suplementos contendo extratos secos de isoflavonas aumentou na última década, devido, principalmente, aos efeitos benéficos atribuídos a estes compostos no alívio dos sintomas da menopausa. Genisteína, daidzeína e gliciteína são as agliconas mais abundantes nos extratos de soja, ocorrendo também como glicosídeos. Tendo em vista seus usos, não existe ainda na literatura uma definição da quantidade mínima de cada uma das agliconas que os extratos ou cápsulas de isoflavonas devem ter, e também não existe um método oficial para o controle de qualidade dos mesmos. O presente trabalho apresenta um método por CCD para análise qualitativa das três agliconas e de seus glicosídeos em extratos e cápsulas de isoflavonas, antes e após hidrólise ácida. A análise quantitativa das cápsulas de isoflavonas, realizada por cromatografia líquida de alta eficiência (CLAE, revelou grandes variações nos teores das três agliconas, após hidrólise ácida. Os teores variaram da seguinte forma, nos 18 lotes de cápsulas avaliados: daidzeína (13,34 a 76,20 mg/cápsula, genisteína (0,61 a 27,18 mg/cápsula e gliciteína (0,49 a 8,80 mg/cápsula.

Detection of gamma-irradiated peanuts by ESR spectroscopy and GC analysis of hydrocarbons

Energy Technology Data Exchange (ETDEWEB)

Wei Mingli; An Li [Institute of Agro-food Science and Technology, Chinese Academy of Agricultural Sciences, 100193 Beijing (China); Yi Mingha, E-mail: wangyilwm@163.co [Institute of Agro-food Science and Technology, Chinese Academy of Agricultural Sciences, 100193 Beijing (China); Feng Wang [Institute of Agro-food Science and Technology, Chinese Academy of Agricultural Sciences, 100193 Beijing (China); Yan Lizhang [Division of Metrology in Ionizing Radiation and Medicine, National Institute of Metrology, 100013 Beijing (China)

2011-03-15

Peanuts were analyzed by electron spin resonance (ESR) spectroscopy and gas chromatography (GC) before and after gamma irradiation. Using European protocols, the validity and effectiveness of these two techniques were compared with regard to sample preparation, sample and solvent consumption and dose-response curves after irradiation. The results showed the possibility of using ESR and GC for distinguishing between irradiated and unirradiated peanuts. A radiation dose of 0.1 kGy could be detected by ESR but not by GC. The results also indicated that GC is an effective method for qualitative analysis of irradiated peanut, while ESR is suitable for the rapid detection of irradiated peanuts.

GC-ASM: Synergistic Integration of Graph-Cut and Active Shape Model Strategies for Medical Image Segmentation.

Science.gov (United States)

Chen, Xinjian; Udupa, Jayaram K; Alavi, Abass; Torigian, Drew A

2013-05-01

Image segmentation methods may be classified into two categories: purely image based and model based. Each of these two classes has its own advantages and disadvantages. In this paper, we propose a novel synergistic combination of the image based graph-cut (GC) method with the model based ASM method to arrive at the GC-ASM method for medical image segmentation. A multi-object GC cost function is proposed which effectively integrates the ASM shape information into the GC framework. The proposed method consists of two phases: model building and segmentation. In the model building phase, the ASM model is built and the parameters of the GC are estimated. The segmentation phase consists of two main steps: initialization (recognition) and delineation. For initialization, an automatic method is proposed which estimates the pose (translation, orientation, and scale) of the model, and obtains a rough segmentation result which also provides the shape information for the GC method. For delineation, an iterative GC-ASM algorithm is proposed which performs finer delineation based on the initialization results. The proposed methods are implemented to operate on 2D images and evaluated on clinical chest CT, abdominal CT, and foot MRI data sets. The results show the following: (a) An overall delineation accuracy of TPVF > 96%, FPVF ASM for different objects, modalities, and body regions. (b) GC-ASM improves over ASM in its accuracy and precision to search region. (c) GC-ASM requires far fewer landmarks (about 1/3 of ASM) than ASM. (d) GC-ASM achieves full automation in the segmentation step compared to GC which requires seed specification and improves on the accuracy of GC. (e) One disadvantage of GC-ASM is its increased computational expense owing to the iterative nature of the algorithm.

Gc-protein-derived macrophage activating factor counteracts the neuronal damage induced by oxaliplatin.

Science.gov (United States)

Morucci, Gabriele; Branca, Jacopo J V; Gulisano, Massimo; Ruggiero, Marco; Paternostro, Ferdinando; Pacini, Alessandra; Di Cesare Mannelli, Lorenzo; Pacini, Stefania

2015-02-01

Oxaliplatin-based regimens are effective in metastasized advanced cancers. However, a major limitation to their widespread use is represented by neurotoxicity that leads to peripheral neuropathy. In this study we evaluated the roles of a proven immunotherapeutic agent [Gc-protein-derived macrophage activating factor (GcMAF)] in preventing or decreasing oxaliplatin-induced neuronal damage and in modulating microglia activation following oxaliplatin-induced damage. The effects of oxaliplatin and of a commercially available formula of GcMAF [oleic acid-GcMAF (OA-GcMAF)] were studied in human neurons (SH-SY5Y cells) and in human microglial cells (C13NJ). Cell density, morphology and viability, as well as production of cAMP and expression of vascular endothelial growth factor (VEGF), markers of neuron regeneration [neuromodulin or growth associated protein-43 (Gap-43)] and markers of microglia activation [ionized calcium binding adaptor molecule 1 (Iba1) and B7-2], were determined. OA-GcMAF reverted the damage inflicted by oxaliplatin on human neurons and preserved their viability. The neuroprotective effect was accompanied by increased intracellular cAMP production, as well as by increased expression of VEGF and neuromodulin. OA-GcMAF did not revert the effects of oxaliplatin on microglial cell viability. However, it increased microglial activation following oxaliplatin-induced damage, resulting in an increased expression of the markers Iba1 and B7-2 without any concomitant increase in cell number. When neurons and microglial cells were co-cultured, the presence of OA-GcMAF significantly counteracted the toxic effects of oxaliplatin. Our results demonstrate that OA-GcMAF, already used in the immunotherapy of advanced cancers, may significantly contribute to neutralizing the neurotoxicity induced by oxaliplatin, at the same time possibly concurring to an integrated anticancer effect. The association between these two powerful anticancer molecules would probably produce

Preparation of WO3/g-C3N4 composites and their application in oxidative desulfurization

International Nuclear Information System (INIS)

Zhao, Rongxiang; Li, Xiuping; Su, Jianxun; Gao, Xiaohan

2017-01-01

Highlights: • The WO 3 /g-C 3 N 4 was successfully synthesized through simple calcination. • The process is simple and the cost raw materials is cheap. • The WO 3 /g-C 3 N 4 firstly applied to ODS. • The desulpurization rate of WO 3 /g-C 3 N 4 may attach to 91.2%. • Five recycles of WO 3 /g-C 3 N 4 still attach to 89.5% due to heterogeneous catalysis. - Abstract: WO 3 /graphitic carbon nitride (g-C 3 N 4 ) composites were successfully synthesized through direct calcining of a mixture of WO 3 and g-C 3 N 4 at 400 °C for 2 h. The WO 3 was prepared by calcination of phosphotungstic acid at 550 °C for 4 h, and the g-C 3 N 4 was obtained by calcination of melamine at 520 °C for 4 h. The WO 3 /g-C 3 N 4 composites were characterized by X-ray diffraction (XRD), Scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FT-IR), and Brunner−Emmett−Teller analysis (BET). The WO 3 /g-C 3 N 4 composites exhibited stronger XRD peaks of WO 3 and g-C 3 N 4 than the WO 3 and pure g-C 3 N 4 . In addition, two WO 3 peaks at 25.7° and 26.6° emerged for the 36% −WO 3 /g-C 3 N 4 composite. This finding indicated that WO 3 was highly dispersed on the surface of the g-C 3 N 4 nanosheets and interacted with the nanosheets, which resulted in the appearance of (012) and (022) planes of WO 3 . The WO 3 /g-C 3 N 4 composite also exhibited a larger specific surface area and higher degree of crystallization than WO 3 or pure g-C 3 N 4 , which resulted in high catalytic activity of the catalyst. Desulfurization experiments demonstrated that the desulfurization rate of dibenzothiophene (DBT) in model oil reached 91.2% under optimal conditions. Moreover, the activity of the catalyst was not significantly decreased after five recycles.

Immunotherapy of metastatic colorectal cancer with vitamin D-binding protein-derived macrophage-activating factor, GcMAF.

Science.gov (United States)

Yamamoto, Nobuto; Suyama, Hirofumi; Nakazato, Hiroaki; Yamamoto, Nobuyuki; Koga, Yoshihiko

2008-07-01

Serum vitamin D binding protein (Gc protein) is the precursor for the principal macrophage-activating factor (MAF). The MAF precursor activity of serum Gc protein of colorectal cancer patients was lost or reduced because Gc protein is deglycosylated by serum alpha-N-acetylgalactosaminidase (Nagalase) secreted from cancerous cells. Deglycosylated Gc protein cannot be converted to MAF, leading to immunosuppression. Stepwise treatment of purified Gc protein with immobilized beta-galactosidase and sialidase generated the most potent macrophage-activating factor (GcMAF) ever discovered, but it produces no side effect in humans. Macrophages treated with GcMAF (100 microg/ml) develop an enormous variation of receptors and are highly tumoricidal to a variety of cancers indiscriminately. Administration of 100 nanogram (ng)/ human maximally activates systemic macrophages that can kill cancerous cells. Since the half-life of the activated macrophages is approximately 6 days, 100 ng GcMAF was administered weekly to eight nonanemic colorectal cancer patients who had previously received tumor-resection but still carried significant amounts of metastatic tumor cells. As GcMAF therapy progressed, the MAF precursor activities of all patients increased and conversely their serum Nagalase activities decreased. Since serum Nagalase is proportional to tumor burden, serum Nagalase activity was used as a prognostic index for time course analysis of GcMAF therapy. After 32-50 weekly administrations of 100 ng GcMAF, all colorectal cancer patients exhibited healthy control levels of the serum Nagalase activity, indicating eradication of metastatic tumor cells. During 7 years after the completion of GcMAF therapy, their serum Nagalase activity did not increase, indicating no recurrence of cancer, which was also supported by the annual CT scans of these patients.

Arroz comercializado na região sul do Brasil: aspectos micotoxicológicos e microscópicos Rice comercialized in Southern Brazil: micotoxicological and microscopic aspects

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Itaciara Larroza Nunes

2003-08-01

Full Text Available Foi realizado um levantamento de características micotoxicológicas e microscópicas em arroz destinado ao consumo humano, comercializado nas cidades de Pelotas e Rio Grande, RS. As amostras, arroz integral [16], arroz parboilizado [16] e arroz branco polido [24] foram coletadas em supermercados, no período de maio a setembro de 2000. A avaliação de ocorrência de aflatoxinas B1, B2, G1, G2, ocratoxina A, zearalenona, desoxinivalenol e toxina T-2 foi realizada pela técnica de cromatografia de camada delgada (ccd. As duas últimas toxinas foram avaliadas também pela técnica de cromatografia gasosa (cg. A micoflora foi determinada através de plaqueamento em superfície em Ágar Batata Dextrose Acidificado, com incubação a 25ºC por 5 dias. As colônias mais freqüentes foram identificadas através da técnica de microcultivo. Dentre as amostras analisadas, duas apresentaram contaminação por ocratoxina A (104 e 128mig.Kg-1, três por zearalenona (559, 1117 e 1955mig.Kg-1, sendo uma co-contaminação com a primeira. Uma das amostras estava contaminada com desoxinivalenol (266 e 300mig.Kg-1, este quantificado por CCD e CG. Quanto à enumeração de bolores e leveduras, os resultados mostraram que 3,6% das amostras apresentaram valores superiores a 10 4 UFC.g -1 e 11% valores próximos deste. Sujidades microscópicas, acima dos limites da legislação (0,25%, foi detectada em uma amostra de arroz integral.A survey was carried out of the micotoxicological and microscopic characteristics of rice comercialized in Pelotas and Rio Grande, RS, Brazil. Samples of whole [16], parboilized [16] and polished white rice [24] were collected in supermarkets, from may until september 2000.The occurrence of aflatoxin B1, B2, G1, G2, ochratoxin A, zearelenone, desoxynivalenol and T2 toxin was evaluated using thin layer chromatographic technique (TLC. The last two toxins were also evaluated by gas chromatography (CG. Mycoflora was determined using a surface

Considerações sobre a determinação quantitativa de alendronato de sódio: titulometria x cromatografia

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ANA FERREIRA RIBEIRO

2010-06-01

Full Text Available O alendronato de sódio é um composto aminodifosfonado capaz de se fixar à matriz óssea e inibir a reabsorção mediada por osteoclastos. A escassez de metodologias oficiais para a determinação quantitativa deste fármaco levou ao desenvolvimento de diversos métodos, os quais empregam, em sua maioria, a cromatografia líquida de alta eficiência (CLAE, com a derivatização do fármaco para poder empregar detectores de ultravioleta. Também há relatos sobre metodologias mais simples para a análise do alendronato, utilizando titulometria ou análise espectrofotométrica. Neste trabalho foi avaliado o emprego da titulometria de neutralização na determinação quantitativa do alendronato de sódio em três lotes de matéria-prima, utilizando NaOH 0,1 M como titulante. Os resultados obtidos na titulometria foram comparados aos encontrados em método cromatográfico de referência (CLAE com derivatização por 9-fluorenilmetilcloroformato ou FMOC, descrito na Farmacopéia Americana (United States Pharmacopeia, os quais apresentaram valores estatisticamente diferentes. Ensaios para a caracterização das amostras também foram realizados e foi observado comportamento distinto das 3 matérias-primas em relação à substância de referência (padrão secundário. O método titulométrico apresentou adequada precisão, mas não mostrou especificidade para a determinação das matérias-primas, embora possa ser validado para determinação do fármaco em produto acabado. Palavras-chave: Alendronato. Titulação ácido-base. Cromatografia. Derivatização. ABSTRACT Observations on the quantitative determination of alendronate sodium: titrimetry vs. chromatography Alendronate sodium is an aminobisphosphonate compound that can bind to the bone matrix and inhibit its osteoclast-mediated resorption. The lack of official monographs on the quantitative analysis of this drug has led to the proposal of a number of different methods for its

Classification of Coffee Beans by GC-C-IRMS, GC-MS, and 1H-NMR

Science.gov (United States)

Arana, Victoria Andrea; Esseiva, Pierre; Pazos, Diego

2016-01-01

In a previous work using 1H-NMR we reported encouraging steps towards the construction of a robust expert system for the discrimination of coffees from Colombia versus nearby countries (Brazil and Peru), to assist the recent protected geographical indication granted to Colombian coffee in 2007. This system relies on fingerprints acquired on a 400 MHz magnet and is thus well suited for small scale random screening of samples obtained at resellers or coffee shops. However, this approach cannot easily be implemented at harbour's installations, due to the elevated operational costs of cryogenic magnets. This limitation implies shipping the samples to the NMR laboratory, making the overall approach slower and thereby more expensive and less attractive for large scale screening at harbours. In this work, we report on our attempt to obtain comparable classification results using alternative techniques that have been reported promising as an alternative to NMR: GC-MS and GC-C-IRMS. Although statistically significant information could be obtained by all three methods, the results show that the quality of the classifiers depends mainly on the number of variables included in the analysis; hence NMR provides an advantage since more molecules are detected to obtain a model with better predictions. PMID:27516919

Classification of Coffee Beans by GC-C-IRMS, GC-MS, and (1)H-NMR.

Science.gov (United States)

Arana, Victoria Andrea; Medina, Jessica; Esseiva, Pierre; Pazos, Diego; Wist, Julien

2016-01-01

In a previous work using (1)H-NMR we reported encouraging steps towards the construction of a robust expert system for the discrimination of coffees from Colombia versus nearby countries (Brazil and Peru), to assist the recent protected geographical indication granted to Colombian coffee in 2007. This system relies on fingerprints acquired on a 400 MHz magnet and is thus well suited for small scale random screening of samples obtained at resellers or coffee shops. However, this approach cannot easily be implemented at harbour's installations, due to the elevated operational costs of cryogenic magnets. This limitation implies shipping the samples to the NMR laboratory, making the overall approach slower and thereby more expensive and less attractive for large scale screening at harbours. In this work, we report on our attempt to obtain comparable classification results using alternative techniques that have been reported promising as an alternative to NMR: GC-MS and GC-C-IRMS. Although statistically significant information could be obtained by all three methods, the results show that the quality of the classifiers depends mainly on the number of variables included in the analysis; hence NMR provides an advantage since more molecules are detected to obtain a model with better predictions.

Development and Validation of a GC-FID Method for Diagnosis of Methylmalonic Acidemia

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Fatemeh Keyfi

2016-05-01

Full Text Available Background: Urinary organic acids are water-soluble intermediates and end products of the metabolism of amino acids, carbohydrates, lipids, and a number of other metabolic processes. In the hereditary diseases known as organic acidurias, an enzyme or co-factor defect in a metabolic pathway leads to the accumulation and increased excretion of one or more of these acidic metabolites. Gas chromatography is the most commonly-used technology to separate and identify these metabolites. In this report the analytical conditions for the determination of methylmalonic acid using a gas chromatography/flame ionization detector (GC-FID are studied with the aim to establish a method to analyze organic acids in human urine. Methods: Studies included the GC-FID method development, the conditions of the derivatization (trimethylsilylation reaction, and the stability of the methylmalonic acid standard solution and trimethylsilyl derivatives during storage. Also, a systematic comparison between GC-FID and gas chromatography/mass spectrometry (GC-MS was performed. Results: The highest resolution and sensitivity were obtained at 60 oC with a 30 min reaction time. Standard solutions and derivatized samples were stable for 7 days at 4-8 oC. Relative standard deviations of within-day and day-to-day assay results were less than 5%. Methylmalonic acid was detected in thirty human urine samples by the proposed GC-FID, and the results were compared with gold standard technique GC-MS. The correlation coefficient between GC-MS and GC-FID was obtained with R2= 0.997. Conclusions: The developed method was applied to the quantitative analysis of methylmalonic acid in urine from hospitalized children with methylmalonic acidemia. With this method we aim to support pediatric clinics in Iran and assist in clinical diagnostics.

Biased Gene Conversion and GC-Content Evolution in the Coding Sequences of Reptiles and Vertebrates

Science.gov (United States)

Figuet, Emeric; Ballenghien, Marion; Romiguier, Jonathan; Galtier, Nicolas

2015-01-01

Mammalian and avian genomes are characterized by a substantial spatial heterogeneity of GC-content, which is often interpreted as reflecting the effect of local GC-biased gene conversion (gBGC), a meiotic repair bias that favors G and C over A and T alleles in high-recombining genomic regions. Surprisingly, the first fully sequenced nonavian sauropsid (i.e., reptile), the green anole Anolis carolinensis, revealed a highly homogeneous genomic GC-content landscape, suggesting the possibility that gBGC might not be at work in this lineage. Here, we analyze GC-content evolution at third-codon positions (GC3) in 44 vertebrates species, including eight newly sequenced transcriptomes, with a specific focus on nonavian sauropsids. We report that reptiles, including the green anole, have a genome-wide distribution of GC3 similar to that of mammals and birds, and we infer a strong GC3-heterogeneity to be already present in the tetrapod ancestor. We further show that the dynamic of coding sequence GC-content is largely governed by karyotypic features in vertebrates, notably in the green anole, in agreement with the gBGC hypothesis. The discrepancy between third-codon positions and noncoding DNA regarding GC-content dynamics in the green anole could not be explained by the activity of transposable elements or selection on codon usage. This analysis highlights the unique value of third-codon positions as an insertion/deletion-free marker of nucleotide substitution biases that ultimately affect the evolution of proteins. PMID:25527834

GC protein-derived macrophage-activating factor decreases α-N-acetylgalactosaminidase levels in advanced cancer patients.

Science.gov (United States)

Thyer, Lynda; Ward, Emma; Smith, Rodney; Branca, Jacopo Jv; Morucci, Gabriele; Gulisano, Massimo; Noakes, David; Eslinger, Robert; Pacini, Stefania

2013-08-01

α- N -acetylgalactosaminidase (nagalase) accumulates in the serum of cancer patients and its activity correlates with tumor burden, aggressiveness and clinical disease progression. The administration of GC protein-derived macrophage-activating factor (GcMAF) to cancer patients with elevated levels of nagalase has been associated with a decrease of serum nagalase activity and with significant clinical benefits. Here, we report the results of the administration of GcMAF to a heterogeneous cohort of patients with histologically diverse, advanced neoplasms, generally considered as "incurable" diseases. In most cases, GcMAF therapy was initiated at late stages of tumor progression. As this is an open-label, non-controlled, retrospective analysis, caution must be employed when establishing cause-effect relationships between the administration GcMAF and disease outcome. However, the response to GcMAF was generally robust and some trends emerged. All patients (n = 20) presented with elevated serum nagalase activity, well above normal values. All patients but one showed a significant decrease of serum nagalase activity upon weekly GcMAF injections. Decreased nagalase activity was associated with improved clinical conditions and no adverse side effects were reported. The observations reported here confirm and extend previous results and pave the way to further studies aimed at assessing the precise role and indications for GcMAF-based anticancer immunotherapy.

Identification of refined petroleum products in contaminated soils using an identification index for GC chromatograms.

Science.gov (United States)

Kwon, Dongwook; Ko, Myoung-Soo; Yang, Jung-Seok; Kwon, Man Jae; Lee, Seung-Woo; Lee, Seunghak

2015-08-01

Hydrocarbons found in the environment are typically characterized by gas chromatography (GC). The shape of the GC chromatogram has been used to identify the source of petroleum contamination. However, the conventional practice of simply comparing the peak patterns of source products to those of environmental samples is dependent on the subjective decisions of individual analysts. We have developed and verified a quantitative analytical method for interpreting GC chromatograms to distinguish refined petroleum products in contaminated soils. We found that chromatograms for gasoline, kerosene, and diesel could be divided into three ranges with boundaries at C6, C8, C16, and C26. In addition, the relative peak area (RPA(GC)) of each range, a dimensionless ratio of the peak area within each range to that of the total range (C6-C26), had a unique value for each petroleum product. An identification index for GC chromatograms (ID(GC)), defined as the ratio of RPA(GC) of C8-C16 to that of C16-C26, was able to identify diesel and kerosene sources in samples extracted from artificially contaminated soils even after weathering. Thus, the ID(GC) can be used to effectively distinguish between refined petroleum products in contaminated soils.

Teor e composição química do óleo essencial de Hyptis marrubioides Epl., Lamiaceae em função da sazonalidade = Content and chemical composition of Hyptis marrubioides essential oil in function of seasons

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Suzan Kelly Vilela Bertolucci

2010-07-01

Full Text Available Os oleos essenciais sao principios odoriferos armazenados em celulas especiais da planta. O oleo essencial no genero Hyptis e usado como anestesico, antiespasmodico, antiinflamatorio e pode induzir aborto em doses elevadas. O objetivo deste trabalho foi avaliar a influencia da sazonalidade no teor e composicao do oleo essencial de Hyptis marrubioides. O delineamento experimental foi inteiramente casualizado, com quatro tratamentos (inverno, primavera, verao e outono e seis repeticoes, totalizando 60 plantas. O oleo essencial foi extraido por hidrodestilacao, em aparelho de Clevenger. A analise qualitativa do oleo essencial foi por cromatografia em fase gasosa (CG/EM. Na estacao do verao, as folhas das plantas de H. marrubiodes apresentaram os maiores teores de oleo essencial. Nas demais estacoes, os teores de oleo essencial obtidos foram semelhantes entre si. Os componentes majoritarios no oleo essencial foram os monoterpenoides α-tujona e β-tujona. As concentracoes relativas dos picos correspondentes a β-tujona nao apresentaram diferencas consideraveis nas quatro estacoes. Os sesquiterpenoides oxigenados (cedrol e cariofilenol e nao-oxigenados (α-copaeno, β-cariofileno, germacreno D e cadaleno foram encontrados em menores quantidades no oleo essencial, entretanto observam-se diferencas quantitativas ao longo das estacoes.Essential oils are odorous principles stored in special plant cells. The essential oil in the Hyptis genus is traditionally used as an anesthetic, antispasmodic, antiinflammatory, and can induce abortion in high doses. The purpose of this work was to evaluate the influence of seasons in essential oil content and chemical composition of species H. marrubioides. A completely randomized complete design was used with four treatments (winter, spring, summer and autumn and six replications, totaling 60 plants. The essential oil was obtained by hydrodistillation with a Clevenger apparatus. The qualitative analysis of the

Used frying oil biodiesel production: experimental factorial design and multivariate analysis

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Rosana de Cassia de Souza Schneider

2009-01-01

Full Text Available Biodiesel é derivado de fontes renováveis ereduz significativamente as emissões atmosféricas. Pode serobtido de diversos processos, como a alcoolise. Nestetrabalho, o biodiesel foi produzido através da alcoolise doóleo de fritura usado de indústrias de alimentação. Umplanejamento experimental foi utilizado e os produtos dereação foram analisados por cromatografia gasosa (CGespectroscopia na região do infravermelho com acessório dereflexão total atenuada horizontal (IV-HATR e análiseexploratória por análise de componentes principais (PCA eanálise hierárquica de grupos (HCA. De acordo com ascondições analisadas obteve-se alta conversão em ésteresmetílicos. Por IV-HATR, a conversão máxima foi observadaem condições experimentais de temperatura ( 50 e 60°C,concentração de catalisador (0,6 e 1,2% e a 1:8 de relaçãomolar entre óleo e metanol. Também foi possíveldiscriminar por análise quimiométrica, 4 grupos noplanejamento experimental e determinar as melhorescondições para a produção de biodiesel de óleo de friturausado.Abstract Biodiesel is derived from renewable sources and it significantly reduces atmospheric emissions. It can be obtained byseveral processes, such as alcoholysis. In this work, biodiesel was produced through alcoholysis of used frying oil from a cateringbusiness. An experimental factorial design was used and the reaction products were analyzed through gas chromatography (GC,horizontal attenuated total reflection Fourier transform infrared (HATR/FT-IR spectroscopy and exploratory analysis withprincipal component analysis (PCA and hierarchical cluster analysis (HCA. Under the conditions analyzed, a high degree ofconversion to methyl ester was found. As shown by HATR/FT-IR, the maximum conversion was obtained when the experimentalconditions had the temperature ( 50 e 60°C, largest catalyst concentration (0,6 e 1,2% and a 1:8 molar proportion of oil tomethanol. It was possible to discriminate

Optimasi Instrumen GC Shimadzu-2014 Terhadap Beberapa Senyawa Metil Ester Asam Lemak (FAME)

OpenAIRE

Tanaty, Muhammad Zaid M. M; Pontoh, Julius; Fatimah, Feti

2016-01-01

Telah dilakukan penelitian mengenai penentuan batas deteksi (LOD) dan respon faktor (RF) GC Shimadzhu-2014 terhadap beberapa senyawa metil ester asam lemak (FAME). Adapun kajian yang dilakukan meliputi pembuatan dan pengenceran larutan FAME standard serta analisis dengan GC sebanyak 2 kali pengulangan sehingga didapat kurva standar senyawa FAME. Berdasarkan hasil analisis dengan GC, kurva standar masing-masing senyawa FAME memiliki presisi yang cukup baik yakni berkisar antara 0.995-0.999. Pe...

Immunotherapy of metastatic breast cancer patients with vitamin D-binding protein-derived macrophage activating factor (GcMAF).

Science.gov (United States)

Yamamoto, Nobuto; Suyama, Hirofumi; Yamamoto, Nobuyuki; Ushijima, Naofumi

2008-01-15

Serum vitamin D3-binding protein (Gc protein) is the precursor for the principal macrophage activating factor (MAF). The MAF precursor activity of serum Gc protein of breast cancer patients was lost or reduced because Gc protein was deglycosylated by serum alpha-N-acetylgalactosaminidase (Nagalase) secreted from cancerous cells. Patient serum Nagalase activity is proportional to tumor burden. The deglycosylated Gc protein cannot be converted to MAF, resulting in no macrophage activation and immunosuppression. Stepwise incubation of purified Gc protein with immobilized beta-galactosidase and sialidase generated probably the most potent macrophage activating factor (termed GcMAF) ever discovered, which produces no adverse effect in humans. Macrophages treated in vitro with GcMAF (100 pg/ml) are highly tumoricidal to mammary adenocarcinomas. Efficacy of GcMAF for treatment of metastatic breast cancer was investigated with 16 nonanemic patients who received weekly administration of GcMAF (100 ng). As GcMAF therapy progresses, the MAF precursor activity of patient Gc protein increased with a concomitant decrease in serum Nagalase. Because of proportionality of serum Nagalase activity to tumor burden, the time course progress of GcMAF therapy was assessed by serum Nagalase activity as a prognostic index. These patients had the initial Nagalase activities ranging from 2.32 to 6.28 nmole/min/mg protein. After about 16-22 administrations (approximately 3.5-5 months) of GcMAF, these patients had insignificantly low serum enzyme levels equivalent to healthy control enzyme levels, ranging from 0.38 to 0.63 nmole/min/mg protein, indicating eradication of the tumors. This therapeutic procedure resulted in no recurrence for more than 4 years. Copyright 2007 Wiley-Liss, Inc.

Preparation of WO3/g-C3N4 composites and their application in oxidative desulfurization

Science.gov (United States)

Zhao, Rongxiang; Li, Xiuping; Su, Jianxun; Gao, Xiaohan

2017-01-01

WO3/graphitic carbon nitride (g-C3N4) composites were successfully synthesized through direct calcining of a mixture of WO3 and g-C3N4 at 400 °C for 2 h. The WO3 was prepared by calcination of phosphotungstic acid at 550 °C for 4 h, and the g-C3N4 was obtained by calcination of melamine at 520 °C for 4 h. The WO3/g-C3N4 composites were characterized by X-ray diffraction (XRD), Scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FT-IR), and Brunner-Emmett-Teller analysis (BET). The WO3/g-C3N4 composites exhibited stronger XRD peaks of WO3 and g-C3N4 than the WO3 and pure g-C3N4. In addition, two WO3 peaks at 25.7° and 26.6° emerged for the 36% -WO3/g-C3N4 composite. This finding indicated that WO3 was highly dispersed on the surface of the g-C3N4 nanosheets and interacted with the nanosheets, which resulted in the appearance of (012) and (022) planes of WO3. The WO3/g-C3N4 composite also exhibited a larger specific surface area and higher degree of crystallization than WO3 or pure g-C3N4, which resulted in high catalytic activity of the catalyst. Desulfurization experiments demonstrated that the desulfurization rate of dibenzothiophene (DBT) in model oil reached 91.2% under optimal conditions. Moreover, the activity of the catalyst was not significantly decreased after five recycles.

Anàlisi instrumental

OpenAIRE

Casas Sabata, Josep M.

1994-01-01

Conté: 2. Cromatografia i electroforesi Aquest text pretén donar una visió general de l'ampli camp dels mètodes instrumentals de separació aplicats al laboratori d'anàlis segons un concepte eminentment pràctic. S'ha dividit en cinc capítols temàtics: teoria de la cromatografia, cromatografia clàssica, cromatografia de gasos, cromatografia de líquids i electroforesi. Va destinat als estudiants d'enginyeria i de les facultats de ciències que dins el seu pla d'estudis incorporin la matèria d'...

Trocas gasosas e teores de minerais no feijão-de-corda irrigado com água salina em diferentes estádios Gas exchange and mineral concentration in cowpea irrigated with saline water at different stages

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Antonia L. R. Neves

2009-12-01

Full Text Available Realizou-se este trabalho com o objetivo de estudar os efeitos da aplicação de água salina nos diferentes estádios de desenvolvimento de plantas de feijão-de-corda sobre as trocas gasosas, o crescimento e os teores de minerais. O experimento foi conduzido no campo e obedeceu o delineamento em blocos ao acaso, com cinco tratamentos e cinco repetições. Os tratamentos utilizados foram: T1 - água do poço (CEa de 0,8 dS m-1 durante todo o ciclo (controle; T2 - água salina (CEa de 5,0 dS m-1 durante todo o ciclo; T3, T4 e T5 - água salina de 0 a 22, de 23 a 42 e de 43 a 62 dias após o plantio (DAP, respectivamente. As plantas dos tratamentos T3, T4 e T5 foram irrigadas com água do poço nas demais fases do ciclo. Realizaram-se, ao longo do ciclo da cultura, medições de trocas gasosas e se determinaram a produção de matéria seca e os teores de Na+, Cl-, K+, Ca2+, N e P. Os tratamentos T2 e T3 em relação ao T1 (controle, reduziram as taxas de fotossíntese e transpiração e as taxas de crescimento vegetativo e provocaram acúmulo, especialmente de Na+ e Cl-, porém se verificou, nas plantas do T3, recuperação de todas essas variáveis ao final do ciclo da cultura. As alterações no acúmulo de Na+ e Cl- nas plantas dos tratamentos T4 e T5 não foram suficientes para provocar efeitos significativos nas trocas gasosas nem nas taxas de crescimento da cultura, em comparação com as plantas do T1.The objective of this paper was to evaluate the effect of irrigation with saline water, applied at different development stages of cowpea, on gas exchange, growth and nutrient concentration. The experiment was set up in the field, in a completely randomized block design, with five treatments and five repetitions. The treatments studied were: T1 - Groundwater with electrical conductivity (ECw of 0.8 dS m-1 during the whole crop cycle (control; T2 - saline water (ECw = 5.0 dS m-1 during the whole crop cycle; T3, T4 and T5 - saline water from 0

Photosynthetic CO2 fixation in guard cells (GC)

International Nuclear Information System (INIS)

Gotow, K.; Taylor, S.; Zeiger, E.

1987-01-01

Recent studies indicate that carbon metabolism in GC is modulated by light quality. The fate of 14 CO 2 supplied to highly purified Vicia GC protoplasts irradiated with red light was investigated. The suspension was stirred at 25 0 C and dark-adapted for 5 min. After 5 min. in red light, 4.8 uCi of NaH 14 CO 3 was added (final concentration: 100 uM). Metabolism was quenched after 30 s with boiling ethanol. Anionic compounds were separated by 2D PC and TLC, and quantified. Rates of CO 2 fixation were 5- to 8-fold higher in the light. In the dark, malate and aspartate had 90% of the total label; in the light, 3-PGA, sugar monophosphates (SMP) and sugar diophosphates (SDP) had up to 60% of the label. Phosphates treatment and rechromatography of labelled SDP showed the presence of ribulose, a specific PCRP metabolite. In time-course experiments, labelled 3-PGA was detected within 5 s. With time, the percentage of label in 3-PGA decreased and that in SMP increased. The authors conclude that 3-PGA is a primary carboxylation product of the PCRP in GC and that the activity of the PCRP and PEP-carboxylase is metabolically regulated

iGC-an integrated analysis package of gene expression and copy number alteration.

Science.gov (United States)

Lai, Yi-Pin; Wang, Liang-Bo; Wang, Wei-An; Lai, Liang-Chuan; Tsai, Mong-Hsun; Lu, Tzu-Pin; Chuang, Eric Y

2017-01-14

With the advancement in high-throughput technologies, researchers can simultaneously investigate gene expression and copy number alteration (CNA) data from individual patients at a lower cost. Traditional analysis methods analyze each type of data individually and integrate their results using Venn diagrams. Challenges arise, however, when the results are irreproducible and inconsistent across multiple platforms. To address these issues, one possible approach is to concurrently analyze both gene expression profiling and CNAs in the same individual. We have developed an open-source R/Bioconductor package (iGC). Multiple input formats are supported and users can define their own criteria for identifying differentially expressed genes driven by CNAs. The analysis of two real microarray datasets demonstrated that the CNA-driven genes identified by the iGC package showed significantly higher Pearson correlation coefficients with their gene expression levels and copy numbers than those genes located in a genomic region with CNA. Compared with the Venn diagram approach, the iGC package showed better performance. The iGC package is effective and useful for identifying CNA-driven genes. By simultaneously considering both comparative genomic and transcriptomic data, it can provide better understanding of biological and medical questions. The iGC package's source code and manual are freely available at https://www.bioconductor.org/packages/release/bioc/html/iGC.html .

Derivatizations for improved detection of alcohols by gas chromatography and photoionization detection (GC-PID)

International Nuclear Information System (INIS)

Krull, I.S.; Swartz, M.; Driscoll, J.N.

1984-01-01

Pentafluorophenyldimethylsilyl chloride (flophemesyl chloride, Fl) is a well known derivatization reagent for improved electron capture detection (ECD) in gas chromatography (GC)(GC-ECD), but it has never been utilized for improved detectability and sensitivity in GC-photoionization detection (GC-PID). A wide variety of flophemesyl alcohol derivatives have been used in order to show a new approach for realizing greatly reduced minimum detection limits (MDL) of virtually all alcohol derivatives in GC-PID analysis. This particular derivatization approach is inexpensive and easy to apply, leading to quantitative or near 100% conversion of the starting alcohols to the expected flophemesyl ethers (silyl ethers). Detection limits can be lowered by 2-3 orders of magnitude for such derivatives when compared with the starting alcohols, along with calibration plots that are linear over 5-7 orders of magnitude. Specific GC conditions have been developed for many flophemesyl derivatives, in all cases using packed columns. Both ECD and PID relative response factors (RRFs) and normalized RRFs have been determined, and such ratios can now be used for improved analytic identification from complex sample matrices, where appropriate. 28 references, 2 figures, 5 tables

Synthesis of g-C3N4/Ag3PO4 heterojunction with enhanced photocatalytic performance

International Nuclear Information System (INIS)

He, Peizhi; Song, Limin; Zhang, Shujuan; Wu, Xiaoqing; Wei, Qingwu

2014-01-01

Graphical abstract: g-C 3 N 4 /Ag 3 PO 4 heterojunction photocatalyst with visible-light response was prepared by a facile coprecipitation method. The results show that g-C 3 N 4 /Ag 3 PO 4 possesses a much higher activity for the decomposition of RhB than that of the pure Ag 3 PO 4 particles. The most mechanism is that g-C 3 N 4 /Ag 3 PO 4 heterojunction photocatalyst can efficiently separate the photogenerated electron–hole pairs, enhancing the photocatalytic activity of g-C 3 N 4 /Ag 3 PO 4 composites. - Highlights: • g-C 3 N 4 /Ag 3 PO 4 heterojunction showed much higher activity than that of Ag 3 PO 4 . • The high activity could be attributed to g-C 3 N 4 for modifying Ag 3 PO 4 . • More ·OH radicals may be significant reason to improve Ag 3 PO 4 activity. - Abstract: g-C 3 N 4 /Ag 3 PO 4 heterojunction photocatalyst with visible-light response was prepared by a facile coprecipitation method. The photocatalysts were characterized by X-ray powder diffraction, transmission electron microscopy, UV–vis absorption spectroscopy and Fourier transform infrared spectroscopy. The photocatalytic activities of the obtained samples were tested by using Rhodamine B (RhB) as the degradation target under visible light irradiation. g-C 3 N 4 /Ag 3 PO 4 decomposed RhB more effectively than the pure Ag 3 PO 4 particles did, and 2 wt.% g-C 3 N 4 had the highest activity. Furthermore, 2 wt.% g-C 3 N 4 /Ag 3 PO 4 degraded high-concentration RhB more potently than unmodified Ag 3 PO 4 did, probably because g-C 3 N 4 /Ag 3 PO 4 heterojunction photocatalyst enhanced the photocatalytic activity by efficiently separating the photogenerated electron–hole pairs

A simple method for assessment of human anti-Neu5Gc antibodies applied to Kawasaki disease.

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Vered Padler-Karavani

Full Text Available N-glycolylneuraminic acid (Neu5Gc is an immunogenic sugar of dietary origin that metabolically incorporates into diverse native glycoconjugates in humans. Anti-Neu5Gc antibodies are detected in all human sera, though with variable levels and epitope-recognition profiles. These antibodies likely play a role in several inflammation-mediated pathologies including cardiovascular diseases and cancer. In cancer, they have dualistic and opposing roles, either stimulating or repressing disease, as a function of their dose, and some of these antibodies serve as carcinoma biomarkers. Thus, anti-Neu5Gc antibodies may signify risk of inflammation-mediated diseases, and changes in their levels could potentially be used to monitor disease progression and/or response to therapy. Currently, it is difficult to determine levels of anti-Neu5Gc antibodies in individual human samples because these antibodies recognize multiple Neu5Gc-epitopes. Here we describe a simple and specific method for detection and overall estimation of human anti-Neu5Gc antibodies. We exploit the difference between two mouse models that differ only by Neu5Gc-presence (wild-type or Neu5Gc-absence (Cmah(-/- knockout. We characterize mouse serum from both strains by HPLC, lectin and mass-spectrometry analysis and show the target Neu5Gc-epitopes. We then use Cmah(-/- knockout sera to inhibit all non-Neu5Gc-reactivity followed by binding to wild-type sera to detect overall anti-Neu5Gc response in a single assay. We applied this methodology to characterize and quantify anti-Neu5Gc IgG and IgA in sera of patients with Kawasaki disease (KD at various stages compared to controls. KD is an acute childhood febrile disease characterized by inflammation of coronary arteries that untreated may lead to coronary artery aneurysms with risk of thrombosis and myocardial infarction. This estimated response is comparable to the average of detailed anti-Neu5Gc IgG profile analyzed by a sialoglycan microarray

On-line Analysis of Catalytic Reaction Products Using a High-Pressure Tandem Micro-reactor GC/MS.

Science.gov (United States)

Watanabe, Atsushi; Kim, Young-Min; Hosaka, Akihiko; Watanabe, Chuichi; Teramae, Norio; Ohtani, Hajime; Kim, Seungdo; Park, Young-Kwon; Wang, Kaige; Freeman, Robert R

2017-01-01

When a GC/MS system is coupled with a pressurized reactor, the separation efficiency and the retention time are directly affected by the reactor pressure. To keep the GC column flow rate constant irrespective of the reaction pressure, a restrictor capillary tube and an open split interface are attached between the GC injection port and the head of a GC separation column. The capability of the attached modules is demonstrated for the on-line GC/MS analysis of catalytic reaction products of a bio-oil model sample (guaiacol), produced under a pressure of 1 to 3 MPa.

Multiresidue analysis of persistent organic pollutants in contaminated soil using GC-LRMS, GC-HRMS and isotope dilution analysis

International Nuclear Information System (INIS)

Badea, Silviu-Laurentiu; Lundstedt, Staffan; Liljelind, Per; Tysklind, Mats

2009-01-01

In this study we evaluated a multiresidue analytical protocol for selected Persistent Organic Pollutants (POPs) in soil, that later can be used in adsorption and leaching studies. The method used was based on Soxhlet extraction and open column chromatographic fractionation and clean-up, as well as liquid-liquid extraction and acetylation for phenolic compounds. Target analytes, i.e. polychlorinated phenols (PCPhs), hexachlorobenzene (HCB), polychlorinated dibenzodioxins and furans (PCDDs/Fs), polychlorinated biphenyl (PCBs) PAHs, were detected and quantified using Gas Chromatography-Low Resolution Mass Spectrometry (GC-LRMS) and Gas Chromatography-High Resolution Mass Spectrometry (GC-HRMS) and isotope dilution methodology. Generally, the results show a good recovery and a low standard deviation for those isomers that have also a 13 C labeled compound present in the sample: 4-mono, 2,4 di, 2,4,5 tri, 2,3,4,5 and penta chlorinated phenols. Our results clearly demonstrate that it is possible to analyse a wide range of compounds in complex soil matrixes. (authors(

Behavioral properties of essential oils of zanthoxylum armatum dc leaves: augmented by chemical profile using gc/gc-ms

International Nuclear Information System (INIS)

Muhammad, N.; Khan, A.Z.; Barkatullah, A.; Ibrar, M.

2013-01-01

In the present study, the essential oils of the leaves of Zanthoxylum armatum (ZEO) were screened for various behavioral properties viz., sedative-hypnotic, anxiolytic, antidepressant, and muscle relaxant activities. In sedative-hypnotic assays, ZEO demonstrated marked reduction in mice movement in open field test at 100 and 200 mg/kg i.p. and potentiated the duration of sleep, in phenobarbitone induced sleeping mice. Profound reduction in the number of steps and rearing were observed at 100 and 200 mg/kg in a dose dependent manner. When analyzed in forced swimming test, it was devoid of any antidepressant effect at test doses. Similarly, ZEO showed significant muscle relaxant activity at 100 and 200 mg/kg i.p. in both chimney test and inclined plant test. GC/GC-MS analysis of ZEO led to the identification of 34 components, linalool being the most dominant constituent. The results suggested that ZEO has strong sedative-hypnotic, anxiolytic and muscle relaxant properties in various animal models. (author)

The DBP Phenotype Gc-1f/Gc-1f Is Associated with Reduced Risk of Cancer. The Tromsø Study.

Directory of Open Access Journals (Sweden)

Rolf Jorde

Full Text Available In addition to its role as a transport protein, the vitamin D binding protein (DBP may also affect lipid metabolism, inflammation and carcinogenesis. There are three common variants of the DBP, Gc1s (1s, Gc1f (1f, Gc2 (2 that result in six common phenotypes (1s/1s, 1s/1f, 1s/2, 1f/1f, 1f/2, and 2/2. These phenotypes can be identified by genotyping for the two single nucleotide polymorphisms rs7041 and rs4588 in the GC gene. The DBP variants have different binding coefficients for the vitamin D metabolites, and accordingly there may be important relations between DBP phenotypes and health.DNA was prepared from subjects who participated in the fourth survey of the Tromsø Study in 1994-1995 and who were registered with the endpoints myocardial infarction (MI, type 2 diabetes (T2DM, cancer or death as well as a randomly selected control group. The endpoint registers were complete up to 2010- 2013. Genotyping was performed for rs7041 and rs4588 and serum 25-hydroxyvitamin D (25(OHD was measured.Genotyping for rs7041 and rs4588 was performed successfully in 11 704 subjects. Among these, 1660 were registered with incident MI, 958 with T2DM, 2410 with cancer and 4318 had died. Subjects with the DBP phenotype 1f/1f had 23 - 26 % reduced risk of incident cancer compared to the 1s/1s and 2/2 phenotypes (P < 0.02, Cox regression with gender as covariate. Differences in serum 25(OHD levels could not explain the apparent cancer protective effect of the DBP variant 1f. In addition to cancer and 25(OHD, there were significant associations between DBP phenotype and body height, hip circumference and serum calcium.There are important biological differences between the common DBP phenotypes. If the relation between the DBP variant 1f and cancer is confirmed in other studies, determination of DBP phenotype may have clinical importance.

Organotin analysis by gas chromatography-pulsed flame-photometric detection (GC-PFPD)

Energy Technology Data Exchange (ETDEWEB)

Leermakers, M.; Nuyttens, J.; Baeyens, W. [Vrije Universiteit Brussel, Analytical and Environmental Chemistry (ANCH), Brussel (Belgium)

2005-03-01

Monobutyltin (MBuT), dibutyltin (DBuT), and tributyltin (TBuT) mixtures have been separated and quantified by gas chromatography with pulsed flame-photometric detection (GC-PFPD). The compounds were first derivatized with NaBEt{sub 4}, then extracted with hexane and injected into the GC in splitless mode. Optimum GC and detector conditions were established. For GC, various injector temperatures and oven temperature programs were tested. For the PFPD detector, gate settings (gate delay and gate width) and detector temperature were optimized. A very good linearity was obtained up to 100-150 ppb for all organotin compounds. The detection limits obtained were: MBuT (0.7 ppb), DBuT (0.8 ppb), and TBuT (0.6 ppb). RSD for repeatability and reproducibility were well below 20% when the instrument was in routine operation. A biological sample (CRM 477) was also analyzed for organotins. Extraction from the biological matrix was performed with TMAH. Besides the increased risk of contamination, the derivatization step seemed to be critical. pH and amount of derivatizing agent were tested. When using an internal standard (TPrT) between 90% and 110% of the certified amounts of organotin were recovered. (orig.)

Determinação e padronização da vitamina E e seus isomeros : comparação entre o metodo de cromatografia liquida de alta eficiencia (CLAE) e o metodo espectrofotometrico por redução de ions cupricos

OpenAIRE

Andrea Scabora Boix Caro

2002-01-01

Resumo: A presente Tese visou estudar a determinação da vitamina E, estabelecendo uma comparação entre o método clássico modificado com um outro método de determinação, a cromatografia líquida de alta eficiência (CLAE).Para efeito de comparação foram utilizados cinco tipos de amostras diferentes: suplementos vitamínicos, óleos vegetais, DDOS, farinha de germe de trigo e fígados liofilizados de ratos. Os resultados encontrados nos métodos avaliados diferiram quanto ao tipo de isômero encontrad...

ANÁLISE DE RISCO DE PRAGUICIDAS EM LEITE CRU E CARACTERIZAÇÃO DO USO EM PROPRIEDADES LEITEIRAS

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Rafael Fagnani

2011-12-01

Full Text Available Este trabalho teve como objetivo a caracterização do uso de praguicidas em propriedades leiteiras no agreste de Pernambuco e estudar a contaminação do leite cru por praguicidas organofosforados (OF e carbamatos (CB, estimando a ingestão diária provável desses resíduos pelo leite. Em 28 propriedades e em dois tanques resfriadores comunitários do agreste pernambucano foram coletadas 30 amostras de leite. A quantificação de praguicidas nas amostras foi realizada por cromatografia gasosa. Doze amostras (40% apresentaram resíduos, sendo seis (20% positivas para OF, cinco (16,7% para CB e uma (3,32% para ambos praguicidas. As médias dos praguicidas detectados no leite em ng/ml foram: 0,04 para coumafós, 0,01 para dimetoato, 0,06 para fention, 0,02 para malation, 0,02 para aldicarb, 0,02 para carbaril e 0,01 para carbofuran. Quando a Ingestão Diária Provável Média dos princípios ativos detectados no leite foi comparada à respectiva Ingestão Diária Aceitável, não houve risco para nenhuma faixa etária, considerando o consumo per capta Brasileiro, pernambucano e o consumo recomendado pelo Ministério da Saúde de leite.

USED FRYING OIL BIODIESEL PRODUCTION: EXPERIMENTAL FACTORIAL DESIGN AND MULTIVARIATE ANALYSIS

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Rosana de Cassia de Souza Schneider

2009-07-01

Full Text Available RESUMO: Biodiesel é derivado de fontes renováveis e reduz significativamente as emissões atmosféricas. Pode ser obtido de diversos processos, como a alcoolise. Neste trabalho, o biodiesel foi produzido através da alcoolise do óleo de fritura usado de indústrias de alimentação. Um planejamento experimental foi utilizado e os produtos de reação foram analisados por cromatografia gasosa (CG espectroscopia na região do infravermelho com acessório de reflexão total atenuada horizontal (IV-HATR e análise exploratória por análise de componentes principais (PCA e análise hierárquica de grupos (HCA. De acordo com as condições analisadas obteve-se alta conversão em ésteres metílicos. Por IV-HATR, a conversão máxima foi observada em condições experimentais de temperatura ( 50 e 60°C, concentração de catalisador (0,6 e 1,2% e a 1:8 de relação molar entre óleo e metanol. Também foi possível discriminar por análise quimiométrica, 4 grupos no planejamento experimental e determinar as melhores condições para a produção de biodiesel de óleo de fritura usado.

Methanogenesis in an impacted and two dystrophic coastal lagoons (Macaé, Brazil

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André Luiz dos Santos Furtado

2002-06-01

Full Text Available This study investigated the methanogenic activity in sediment of the Imboacica (human impacted, Cabiúnas and Comprida coastal lagoons in Rio de Janeiro State (Brazil. Methane was not detected in water and sediment samples from the three lagoons. The measured nutrient concentrations in the pore-water indicated that methanogens activity was not limited by nutrients. Methanogenic activity was not detected under in vitro conditions, indicating that terminal organic carbon mineralisation via methanogenesis was negligible for the top 6 cm of sediment at the sampling time.O objetivo deste estudo foi investigar a atividade metanogênica no sedimento das lagoas Imboacica, Cabiúnas e Comprida (Macaé, Rio de Janeiro. As amostras de água e sedimento foram coletadas em duas estações em cada lagoa. A atividade metanogênica nas três lagoas foi abaixo do limite de detecção do método utilizado (cromatografia gasosa. Os resultados obtidos indicaram que a atividade metanogênica não foi limitada pela concentração de nutrientes na água intersticial. Sob condições experimentais, a atividade metanogênica foi nula, indicando que a mineralização do carbono orgânico via metanogênese foi desprezível nas três lagoas durante o período amostrado.

Degradação de xenobióticos por fungos filamentosos isolados de areia fenólica

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J. H. Silva

2000-09-01

Full Text Available Microrganismos foram isolados de areia fenólica resultante de atividades metalúrgicas, utilizando meio mínimo para fungos e pentaclorofenol (PCF como única fonte de carbono. Após quatro repiques sucessivos em intervalos de 15 dias de incubação, as culturas foram plaqueadas em meio de Martin. Três gêneros de fungos foram isolados e identificados como Acremonium sp., Paecilomyces sp. e Penicillium sp. Estes foram testados para degradar os corantes índigo e RBBR (Azul Brilhante de Remazol - R e o organoclorado PCF. A descoloração do índigo foi de 99%, para Paecilomyces e Penicillium, e de 74%, para Acremonium, e a de RBBR foi de 16%, para Penicillium; 14%, para Acremonium, e 5%, para Paecilomyces. Usando azul de bromotimol como indicador de degradação de PCF, foram obtidos 24% de descoloração para Acremonium; 22%, para Penicillium, e 17%, para Paecilomyces Utilizando cromatografia gasosa, detectou-se degradação de PCF de 69%, para Penicillium; 65%, para Paecilomyces, e 40% para Acremonium, respectivamente. Os resultados mostraram que foi possível isolar microrganismos de uma areia de fundição, altamente contaminada com fenóis, e os fungos isolados foram capazes de degradar PCF e outros xenobióticos testados.

Perfil lipídico de ovos desidratados com ênfase no seu teor de gorduras trans Lipid profile of dehydrated eggs with emphasis on the contents of trans fatty acids

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Silce Adeline Danelon Guassi

2008-03-01

Full Text Available O presente trabalho objetivou a determinação do perfil lipídico de ovos integrais desidratados, bem como de gemas desidratadas, a fim de enfatizar seu conteúdo de ácidos graxos de configuração trans. A fração lipídica das amostras foi extraída com hexano/isopropanol e, a seguir, metilada. Os ácidos graxos foram identificados via cromatografia gasosa. Constatou-se que a natureza lipídica dos ovos tem caráter predominantemente insaturado: 63,65% dos lipídios totais nos ovos integrais e 62,63% nas gemas. Além disso, foram identificados apenas traços de gorduras trans (0,24% nos ovos integrais e 0,27% nas gemas.The objective of this work was to determine fatty acids composition in dehydrated eggs and egg yolks emphasizing its contents of trans fatty acids. The fatty acids fraction of the samples was extracted with hexane/isopropanol (3:2 and then methylated. The profile of the fatty acids was identified by gas chromatography with predominant evidence of insaturated character: 63.65 and 62.63% of the lipids were unsatureted in the eggs and in the egg yolks, respectively. Traces of trans fatty were also identified (0.24% in the hole eggs and 0.27% in the egg yolks.

Composição de voláteis e perfil de aroma e sabor de méis de eucalipto e laranja

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Bastos Deborah Helena Markowicz

2002-01-01

Full Text Available Neste trabalho foram analisados os compostos voláteis de amostras de mel de eucalipto e laranja colhidos nos estados de São Paulo e de Minas Gerais. O isolamento dos voláteis foi realizado empregando-se uma técnica de ''headspace'' dinâmico, a separação efetuada por cromatografia gasosa de alta resolução e a identificação por espectrometria de massas, Índices de Kovats e padrões, quando disponíveis. Foram identificados no mel de laranja o benzaldeído, o óxido cis de linalol, n-heptanal, 6-metil-5-hepten-2-ona, octanal e fenilacetaldeído, e em mel de eucalipto, o nonanal, 2-heptanona, 2-heptanol, octanol e nonanol. A caracterização sensorial desses méis foi obtida por Análise Descritiva Quantitativa e a aplicação de Análise dos Componentes Principais aos dados revelou que os descritores ''queimado'' e ''sabor residual'' caracterizam o mel de eucalipto, enquanto ''floral'' e ''cera'' caracterizam o mel de laranja. Entre os compostos identificados, o nonanal e o nonanol apresentaram contribuição sensorial importante ao mel de eucalipto, enquanto o fenilacetaldeído e o benzaldeído foram relacionados com os principais descritores do mel de laranja.

Catalisadores sol-gel de Ni-SiO2 e Ni-Al2O3 aplicados na reforma de metano com CO2 - DOI: 10.4025/actascitechnol.v27i1.1492

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Giane Gonçalves

2005-03-01

Full Text Available A reação de reforma do metano com CO2 apresenta-se como um processo promissor de geração de gás de síntese e hidrogênio. Neste sentido, foram preparados catalisadores de níquel-sílica e níquel-alumina pelo método sol-gel, com carga metálica nominal de 8% em massa. Os catalisadores foram caracterizados por redução à temperatura programada, análise termogravimétrica e determinação da área superficial específica. A reação de reforma do metano com CO2 foi realizada em um micro-reator contendo 500 mg de catalisador, previamente ativado em uma mistura redutora contendo hidrogênio. Os ensaios de reforma a seco do metano foram realizados a 800C, na pressão atmosférica, por um período de 12 horas, com uma razão molar de alimentação de [CO2:CH4] = 6. Os produtos da reação foram analisados por cromatografia gasosa. Dentre os catalisadores avaliados, nas condições de reação estudadas, o catalisador de níquel suportado em sílica foi o que apresentou o melhor desempenho

Características físico-químicas e compostos aromáticos do suco de melão clarificado por microfiltração tangencial

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Raimundo Marcelino Silva Neto

2016-10-01

Full Text Available Polpa e suco de melão clarificado por microfiltração tangencial foram avaliados com relação as suas características físico-químicas e compostos aromáticos. A polpa do melão (Cucumis melo var inodorus foi extraída, tratada com as enzimas Pectinex Ultra SP-L e Celuclast e clarificada por microfiltração à pressão média de 3,0 bar. O suco clarificado apresentou-se incolor com uma leve tonalidade esverdeada. As características físico-químicas da polpa e do suco clarificado, como pH, brix, acidez titulável, turbidez, glicose, frutose, sacarose, foram identificadas, assim como seu perfil aromático por meio de micro-extração em fase sólida (SPME e cromatografia gasosa acoplada com espectrometria de massa (CG-EM. A microfiltração permitiu obter uma bebida de valor agregado partindo de uma matéria-prima de descarte do mercado externo, preservando suas características físico-químicas iniciais, indicando seu potencial de uso em blends de sucos de frutas tropicais. Adicionalmente, a fração retida poderá ser incorporada na polpa do melão e direcionada ao mercado de bebidas funcionais.

GC protein-derived macrophage-activating factor decreases ?-N-acetylgalactosaminidase levels in advanced cancer patients

OpenAIRE

Thyer, Lynda; Ward, Emma; Smith, Rodney; Branca, Jacopo JV; Morucci, Gabriele; Gulisano, Massimo; Noakes, David; Eslinger, Robert; Pacini, Stefania

2013-01-01

?-N-acetylgalactosaminidase (nagalase) accumulates in the serum of cancer patients and its activity correlates with tumor burden, aggressiveness and clinical disease progression. The administration of GC protein-derived macrophage-activating factor (GcMAF) to cancer patients with elevated levels of nagalase has been associated with a decrease of serum nagalase activity and with significant clinical benefits. Here, we report the results of the administration of GcMAF to a heterogeneous cohort ...

On the analysis of mercuric nitrate in flue gas by GC-MS

Energy Technology Data Exchange (ETDEWEB)

Olson, Edwin S.; Sharma, Ramesh K.; Pavlish, John H. [Energy and Environmental Research Center, University of North Dakota, Grand Forks, ND 58202 (United States)

2002-11-01

Recent research has demonstrated that in a simulated flue gas stream containing NO{sub 2} and SO{sub 2} elemental mercury is initially captured on a carbon or manganese oxide sorbent. After approximately an hour, however, mercury breaks through relatively rapidly, and the volatile form of mercury emitted is an oxidized species. The volatile mercury species emitted from a granular MnO{sub 2} sorbent was trapped in an impinger containing cold acetonitrile. Subsequent evaporation of 95% of the acetonitrile in a Kuderna-Danish apparatus and gas chromatography (GC) of the concentrate resulted in a single mercury-containing GC peak at 5.5 min; the retention time and mass spectrum of this compound matched exactly those of a standard mercury(II) nitrate hydrate, Hg(NO{sub 3}){sub 2}.H{sub 2}O dissolved in acetonitrile. The volatile mercury component analyzed from injection of this standard solution was shown to be a form of methylmercury that is produced in the GC column by reaction of the highly reactive mercury nitrate with the methylsiloxane GC phase. Because the on-column derivatization reaction seems to be unique to mercury nitrate, the GC-MS (gas chromatography-mass spectroscopic) analysis provides strong evidence for identification of the trapped oxidized mercury species as mercury nitrate although, because the nitrate becomes detached from the mercury atom in the on-column reaction, the identity is not proven. (orig.)

Patterns and effects of GC3 heterogeneity and parsimony informative sites on the phylogenetic tree of genes.

Science.gov (United States)

Ma, Shuai; Wu, Qi; Hu, Yibo; Wei, Fuwen

2018-05-20

The explosive growth in genomic data has provided novel insights into the conflicting signals hidden in phylogenetic trees. Although some studies have explored the effects of the GC content and parsimony informative sites (PIS) on the phylogenetic tree, the effect of the heterogeneity of the GC content at the first/second/third codon position on parsimony informative sites (GC1/2/3 PIS ) among different species and the effect of PIS on phylogenetic tree construction remain largely unexplored. Here, we used two different mammal genomic datasets to explore the patterns of GC1/2/3 PIS heterogeneity and the effect of PIS on the phylogenetic tree of genes: (i) all GC1/2/3 PIS have obvious heterogeneity between different mammals, and the levels of heterogeneity are GC3 PIS  > GC2 PIS  > GC1 PIS ; (ii) the number of PIS is positively correlated with the metrics of "good" gene tree topologies, and excluding the third codon position (C3) decreases the quality of gene trees by removing too many PIS. These results provide novel insights into the heterogeneity pattern of GC1/2/3 PIS in mammals and the relationship between GC3/PIS and gene trees. Additionally, it is necessary to carefully consider whether to exclude C3 to improve the quality of gene trees, especially in the super-tree method. Copyright © 2018 Elsevier B.V. All rights reserved.

Volatilizable Biogenic Organic Compounds (VBOCs with two dimensional Gas Chromatography-Time of Flight Mass Spectrometry (GC × GC-TOFMS: sampling methods, VBOC complexity, and chromatographic retention data

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C. Chen

2012-02-01

Full Text Available Two dimensional gas chromatography (GC × GC with detection by time-of-flight mass spectrometry (TOFMS was applied in the rapid analysis of air samples containing highly complex mixtures of volatilizable biogenic organic compounds (VBOCs. VBOC analytical methodologies are briefly reviewed, and optimal conditions are discussed for sampling with both adsorption/thermal desorption (ATD cartridges and solid-phase microextraction (SPME fibers. Air samples containing VBOC emissions from leaves of two tree species (Cedrus atlantica and Calycolpus moritzianus were obtained by both ATD and SPME. The optimized gas chromatographic conditions utilized a 45 m, 0.25 mm I.D. low-polarity primary column (DB-VRX, 1.4 μm film and a 1.5 m, 0.25 mm I.D. polar secondary column (StabilwaxTM, 0.25 μm film. Excellent separation was achieved in a 36 min temperature programmed GC × GC chromatogram. Thousands of VBOC peaks were present in the sample chromatograms; hundreds of tentative identifications by NIST mass spectral matching are provided. Very few of the tentatively identified compounds are currently available as authentic standards. Minimum detection limit values for a 5 l ATD sample were 3.5 pptv (10 ng m−3 for isoprene, methyl vinyl ketone, and methacrolein, and ~1.5 pptv (~10 ng m−3 for monoterpenes and sesquiterpenes. Kovats-type chromatographic retention index values on the primary column and relative retention time values on the secondary column are provided for 21 standard compounds and for 417 tentatively identified VBOCs. 19 of the 21 authentic standard compounds were found in one of the Cedrus atlantica SPME samples. In addition, easily quantifiable levels of at least 13 sesquiterpenes were found in an ATD sample obtained from a branch enclosure of Calycolpus moritzianus. Overall, the results obtained via GC × GC-TOFMS highlight an extreme, and largely uncharacterized diversity of VBOCs, consistent with the hypothesis that sesquiterpenes and

Volatilizable Biogenic Organic Compounds (VBOCs) with two dimensional Gas Chromatography-Time of Flight Mass Spectrometry (GC × GC-TOFMS): sampling methods, VBOC complexity, and chromatographic retention data

Science.gov (United States)

Pankow, J. F.; Luo, W.; Melnychenko, A. N.; Barsanti, K. C.; Isabelle, L. M.; Chen, C.; Guenther, A. B.; Rosenstiel, T. N.

2012-02-01

Two dimensional gas chromatography (GC × GC) with detection by time-of-flight mass spectrometry (TOFMS) was applied in the rapid analysis of air samples containing highly complex mixtures of volatilizable biogenic organic compounds (VBOCs). VBOC analytical methodologies are briefly reviewed, and optimal conditions are discussed for sampling with both adsorption/thermal desorption (ATD) cartridges and solid-phase microextraction (SPME) fibers. Air samples containing VBOC emissions from leaves of two tree species (Cedrus atlantica and Calycolpus moritzianus) were obtained by both ATD and SPME. The optimized gas chromatographic conditions utilized a 45 m, 0.25 mm I.D. low-polarity primary column (DB-VRX, 1.4 μm film) and a 1.5 m, 0.25 mm I.D. polar secondary column (StabilwaxTM, 0.25 μm film). Excellent separation was achieved in a 36 min temperature programmed GC × GC chromatogram. Thousands of VBOC peaks were present in the sample chromatograms; hundreds of tentative identifications by NIST mass spectral matching are provided. Very few of the tentatively identified compounds are currently available as authentic standards. Minimum detection limit values for a 5 l ATD sample were 3.5 pptv (10 ng m-3) for isoprene, methyl vinyl ketone, and methacrolein, and ~1.5 pptv (~10 ng m-3) for monoterpenes and sesquiterpenes. Kovats-type chromatographic retention index values on the primary column and relative retention time values on the secondary column are provided for 21 standard compounds and for 417 tentatively identified VBOCs. 19 of the 21 authentic standard compounds were found in one of the Cedrus atlantica SPME samples. In addition, easily quantifiable levels of at least 13 sesquiterpenes were found in an ATD sample obtained from a branch enclosure of Calycolpus moritzianus. Overall, the results obtained via GC × GC-TOFMS highlight an extreme, and largely uncharacterized diversity of VBOCs, consistent with the hypothesis that sesquiterpenes and other compounds

THE IDENTIFICATION OF THE BINDING MEDIA IN THE TANG DYNASTY CHINESE WALL PAINTINGS BY USING Py-GC/MS AND GC/MS TECHNIQUES

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Hong GUO

2011-06-01

Full Text Available The archaeological discoveries of Tang tomb murals in Xi’an, China brought to light unprecedented data for the study of the art of the Tang Dynasty (618-907 AD. The spectacular murals with their particular contents provided first-hand material for the study of Chinese history and the techniques of wall paintings during the Tang Dynasty. In order to gain a better understanding of the materials used and to preserve those paintings, pyrolysis-gas chromatography-mass spectrometry (Py-GC/MS and gas chromatography-mass spectrometry (GC/MS were applied for the characterization of the binding media in the paintings. The combination of these analytical techniques is an ideal methodology to identify binding media in unknown samples.

Trocas gasosas de cafeeiros (Coffea arabica L. e seringueiras (Hevea brasiliensis Muell. Arg. em diferentes sistemas de cultivo na região de larvas, MG Gas exchange in coffe (Coffea arabica L. and rubber tree (Hevea brasiliensis Muell. Arg. in different crop systems in lavras, MG

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Cláudio Roberto Meira de Oliveira

2006-04-01

Full Text Available O uso de sistemas de cultivo agrícola que favorecem a conservação dos recursos naturais e a diversidade de produção representa uma alternativa para produtores que visam menores custos em uma produção sustentável. Dentre esses sistemas de cultivo, destaca-se o sistema de consórcio entre cafeeiros e seringueiras, que tem sido estudado na região sul de Minas Gerais. Nesse contexto, avaliaram-se características de trocas gasosas, fluorescência da clorofila e relações hídricas de cafeeiros e seringueiras, em monocultivo e consórcio, na fase de implantação dos cultivos, com o objetivo de verificar o comportamento dessas espécies em diferentes sistemas de cultivo. Os resultados apontaram que um ambiente caracterizado por níveis de radiação e temperatura menores favorece as trocas gasosas do cafeeiro, enquanto maior disponibilidade hídrica e valores elevados de radiação são favoráveis ao desenvolvimento da seringueira quando em sistemas consorciados.Crop systems that improve conservation of natural resources and diversity of production is a promising practice for farmers seeking low costs and a sustainable agriculture. The coffee - rubber tree intercropping has been studied in the south of Minas Gerais - Brazil. Within this context, the objective of this work was to evaluate the characteristics gas exchange, chlorophyll fluorescence and water relations of coffee and rubber tree in both intercropping and monocroping systems, in the early stage of the plantation establishment. The results showed that the reduction in radiation levels and temperature promote gas exchange increase in coffee, while higher photosynthetic radiation values and soil water availability are favorable to rubber tree in intercropping systems.

SPME GC/MS Analysis of Three Ornithogalum L. species from Turkey

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Gülin Renda

2016-01-01

Full Text Available In this study, a solid phase micro extraction (SPME method with gas chromatography-mass spectrometry (GC-MS was used for analysis of volatile compounds in flowers and bulbs of three Ornithogalum species. The samples of flowers and bulbs of Ornithogalum sigmoideum, Ornithogalum orthophyllum, Ornithogalum oligophyllum was separately analyzed by SPME-GC-MS. A comparison of volatile compounds was made between species and the parts studied. A total of 70 compounds were identified and different volatile compounds were determined in distinct parts of the species. The major volatile organic compound of the flowers of O. sigmoideum and O. ornithogalum was furan (54.5% and 57.0% respectively. For O. oligophyllum the major volatile organic compound was nonanal (19.2%. Analyses revealed that SPME-GC-MS method is appropriate for the analysis of volatile compounds of Ornithogalum species.

Photocatalytic decomposition of N2O over TiO2/g-C3N4 photocatalysts heterojunction

Science.gov (United States)

Kočí, K.; Reli, M.; Troppová, I.; Šihor, M.; Kupková, J.; Kustrowski, P.; Praus, P.

2017-02-01

TiO2/g-C3N4 photocatalysts with the various TiO2/g-C3N4 weight ratios from 1:2 to 1:6 were fabricated by mechanical mixing in water suspension followed by calcination. Pure TiO2 was prepared by thermal hydrolysis and pure g-C3N4 was prepared from commercial melamine by thermal annealing at 620 °C. All the nanocomposites were characterized by X-ray powder diffraction, UV-vis diffuse reflectance spectroscopy, Raman spectroscopy, infrared spectroscopy, scanning electron microscopy, transmission electron microscopy, photoelectrochemical measurements and nitrogen physisorption. The prepared mixtures along with pure TiO2 and g-C3N4 were tested for the photocatalytic decomposition of nitrous oxide under UVC (λ = 254 nm), UVA (λ = 365 nm) and Vis (λ > 400 nm) irradiation. The TiO2/g-C3N4 nanocomposites showed moderate improvement compared to pure g-C3N4 but pure TiO2 proved to be a better photocatalyst under UVC irradiation. However, under UVA irradiation conditions, the photocatalytic activity of TiO2/g-C3N4 (1:2) nanocomposite exhibited an increase compared to pure TiO2. Nevertheless, further increase of g-C3N4 amount leads/led to a decrease in reactivity. These results are suggesting the nanocomposite with the optimal weight ratio of TiO2 and g-C3N4 have shifted absorption edge energy towards longer wavelengths and decreased the recombination rate of charge carriers compared to pure g-C3N4. This is probably due to the generation of heterojunction on the TiO2/g-C3N4 interface.

No predictive value of GC phenotypes for HIV infection and progression to AIDS

NARCIS (Netherlands)

Pronk, J. C.; Frants, R. R.; Crusius, B.; Eriksson, A. W.; de Wolf, F.; Boucher, C. A.; Bakker, M.; Goudsmit, J.

1988-01-01

The genetic polymorphism of group-specific component (GC) was investigated with isoelectric focusing in 351 homosexual men at risk for HIV infection, 96 male patients with AIDS, and 86 heterosexual controls. No significant differences in GC phenotype distribution were seen between controls and any

Hantavirus Gn and Gc glycoproteins self-assemble into virus-like particles.

Science.gov (United States)

Acuña, Rodrigo; Cifuentes-Muñoz, Nicolás; Márquez, Chantal L; Bulling, Manuela; Klingström, Jonas; Mancini, Roberta; Lozach, Pierre-Yves; Tischler, Nicole D

2014-02-01

How hantaviruses assemble and exit infected cells remains largely unknown. Here, we show that the expression of Andes (ANDV) and Puumala (PUUV) hantavirus Gn and Gc envelope glycoproteins lead to their self-assembly into virus-like particles (VLPs) which were released to cell supernatants. The viral nucleoprotein was not required for particle formation. Further, a Gc endodomain deletion mutant did not abrogate VLP formation. The VLPs were pleomorphic, exposed protrusions and reacted with patient sera.

Determination of selected organophosphorus pesticides using GC ...

African Journals Online (AJOL)

A reproducible analytical method utilising GC-MS is presented for the analysis of thirteen organophosphorus insecticides (OPs) often found in environmental aqueous samples. Extraction of filtered river and canal water (100 mL), fortified with the OPs, was conducted using solid-phase extraction and eluted with a variety of ...

Tumor cell alpha-N-acetylgalactosaminidase activity and its involvement in GcMAF-related macrophage activation.

Science.gov (United States)

Mohamad, Saharuddin B; Nagasawa, Hideko; Uto, Yoshihiro; Hori, Hitoshi

2002-05-01

Alpha-N-acetyl galactosaminidase (alpha-NaGalase) has been reported to accumulate in serum of cancer patients and be responsible for deglycosylation of Gc protein, which is a precursor of GcMAF-mediated macrophage activation cascade, finally leading to immunosuppression in advanced cancer patients. We studied the biochemical characterization of alpha-NaGalase from several human tumor cell lines. We also examined its effect on the potency of GcMAF to activate mouse peritoneal macrophage to produce superoxide in GcMAF-mediated macrophage activation cascade. The specific activity of alpha-NaGalases from human colon tumor cell line HCT116, human hepatoma cell line HepG2, and normal human liver cells (Chang liver cell line) were evaluated using two types of substrates; GalNAc-alpha-PNP (exo-type substrate) and Gal-beta-GalNAc-alpha-PNP (endo-type substrate). Tumor-derived alpha-NaGalase having higher activity than normal alpha-NaGalase, had higher substrate specificity to the exo-type substrate than to the endo-type substrate, and still maintained its activity at pH 7. GcMAF enhance superoxide production in mouse macrophage, and pre-treatment of GcMAF with tumor cell lysate reduce the activity. We conclude that tumor-derived alpha-NaGalase is different in biochemical characterization compared to normal alpha-NaGalase from normal Chang liver cells. In addition, tumor cell-derived alpha-NaGalase decreases the potency of GcMAF on macrophage activation.

Clinical experience of integrative cancer immunotherapy with GcMAF.

Science.gov (United States)

Inui, Toshio; Kuchiike, Daisuke; Kubo, Kentaro; Mette, Martin; Uto, Yoshihiro; Hori, Hitoshi; Sakamoto, Norihiro

2013-07-01

Immunotherapy has become an attractive new strategy in the treatment of cancer. The laboratory and clinical study of cancer immunotherapy is rapidly advancing. However, in the clinical setting, the results of cancer immunotherapy are mixed. We therefore contend that cancer immunotherapy should be customized to each patient individually based on their immune status and propose an integrative immunotherapy approach with second-generation group-specific component macrophage activating factor (GcMAF)-containing human serum. The standard protocol of our integrative cancer immunotherapy is as follows: i) 0.5 ml GcMAF-containing human serum is administered intramuscularly or subcutaneously once or twice per week for the duration of cancer therapy until all cancer cells are eradicated; ii) hyper T/natural killer (NK) cell therapy is given once per week for six weeks; iii) high-dose vitamin C is administered intravenously twice per week; iv) alpha lipoic acid (600 mg) is administered orally daily; v) vitamin D3 (5,000-10,000 IU) is administered orally daily. By March 2013, Saisei Mirai have treated over 345 patients with GcMAF. Among them we here present the cases of three patients for whom our integrative immunotherapy was remarkably effective. The results of our integrative immunotherapy seem hopeful. We also plan to conduct a comparative clinical study.>

Glycan structure of Gc Protein-derived Macrophage Activating Factor as revealed by mass spectrometry.

Science.gov (United States)

Borges, Chad R; Rehder, Douglas S

2016-09-15

Disagreement exists regarding the O-glycan structure attached to human vitamin D binding protein (DBP). Previously reported evidence indicated that the O-glycan of the Gc1S allele product is the linear core 1 NeuNAc-Gal-GalNAc-Thr trisaccharide. Here, glycan structural evidence is provided from glycan linkage analysis and over 30 serial glycosidase-digestion experiments which were followed by analysis of the intact protein by electrospray ionization mass spectrometry (ESI-MS). Results demonstrate that the O-glycan from the Gc1F protein is the same linear trisaccharide found on the Gc1S protein and that the hexose residue is galactose. In addition, the putative anti-cancer derivative of DBP known as Gc Protein-derived Macrophage Activating Factor (GcMAF, which is formed by the combined action of β-galactosidase and neuraminidase upon DBP) was analyzed intact by ESI-MS, revealing that the activating E. coli β-galactosidase cleaves nothing from the protein-leaving the glycan structure of active GcMAF as a Gal-GalNAc-Thr disaccharide, regardless of the order in which β-galactosidase and neuraminidase are applied. Moreover, glycosidase digestion results show that α-N-Acetylgalactosamindase (nagalase) lacks endoglycosidic function and only cleaves the DBP O-glycan once it has been trimmed down to a GalNAc-Thr monosaccharide-precluding the possibility of this enzyme removing the O-glycan trisaccharide from cancer-patient DBP in vivo. Copyright © 2016 Elsevier Inc. All rights reserved.

Application of accelerator mass spectrometry to environmental research, Trial of GC-AMS

International Nuclear Information System (INIS)

Shibata, Yasuyuki

2003-01-01

The accelerator analysis facility of the National Institute for Environmental Studies, which aims to develop a new device capable of measuring "1"4C age for each compound, is promoting the study to establish the GC-AMS that combines two-dimensional gas chromatograph (GC) and accelerator mass spectrometry (AMS). The on-line GC-AMS system for the metabolic measurement of "1"4C-labeled compounds for medicinal biochemical research is a system, in which a GC-separated sample is continuously converted into CO_2 in a combustion tube and introduced directly to a gas ion source to continuously measure "1"4C. In the "1"4C detection experiment, the concentration of CO_2 gas was changed using a helium introduction line and a sample injection valve, and CO_2 gas plus helium gas were introduced into the gas ion source. As a result, it was found that the online GC-AMS has feasibility and high potential capability. For off-line GC-AMS for environmental samples, after purification with preparative gas chromatography, the sample is converted to graphite in a vacuum line and applied to common AMS measurement. The authors collected Northwest Pacific Ocean bottom sediment cores, and performed the extraction and purification of fatty acids of specific stratigraphy and the "1"4C measurement of each compound. The age of the compound derived from the surface layer planktons was the result capable of indicating the sedimentary age of the stratigraphy. In addition, as an application study to explore the source of pollutants in the environment using "1"4C as a tracer representing the characteristics of each source, the authors started to conduct the research choosing atmospheric dust samples. As a starting point, the authors attempted to measure the "1"4C concentration of vehicle exhaust particles and incinerator fly ash particles respectively. There was hardly any "1"4C in vehicle exhaust particles. (A.O.)

GC-MS Based Plasma Metabolomics for Identification of Candidate Biomarkers for Hepatocellular Carcinoma in Egyptian Cohort.

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Mohammad R Nezami Ranjbar

Full Text Available This study evaluates changes in metabolite levels in hepatocellular carcinoma (HCC cases vs. patients with liver cirrhosis by analysis of human blood plasma using gas chromatography coupled with mass spectrometry (GC-MS. Untargeted metabolomic analysis of plasma samples from participants recruited in Egypt was performed using two GC-MS platforms: a GC coupled to single quadruple mass spectrometer (GC-qMS and a GC coupled to a time-of-flight mass spectrometer (GC-TOFMS. Analytes that showed statistically significant changes in ion intensities were selected using ANOVA models. These analytes and other candidates selected from related studies were further evaluated by targeted analysis in plasma samples from the same participants as in the untargeted metabolomic analysis. The targeted analysis was performed using the GC-qMS in selected ion monitoring (SIM mode. The method confirmed significant changes in the levels of glutamic acid, citric acid, lactic acid, valine, isoleucine, leucine, alpha tocopherol, cholesterol, and sorbose in HCC cases vs. patients with liver cirrhosis. Specifically, our findings indicate up-regulation of metabolites involved in branched-chain amino acid (BCAA metabolism. Although BCAAs are increasingly used as a treatment for cancer cachexia, others have shown that BCAA supplementation caused significant enhancement of tumor growth via activation of mTOR/AKT pathway, which is consistent with our results that BCAAs are up-regulated in HCC.

Case report: A breast cancer patient treated with GcMAF, sonodynamic therapy and hormone therapy.

Science.gov (United States)

Inui, Toshio; Makita, Kaori; Miura, Hirona; Matsuda, Akiko; Kuchiike, Daisuke; Kubo, Kentaro; Mette, Martin; Uto, Yoshihiro; Nishikata, Takahito; Hori, Hitoshi; Sakamoto, Norihiro

2014-08-01

Gc protein-derived macrophage-activating factor (GcMAF) occurs naturally in the human body. It has various functions, such as macrophage activation and antitumor activities. Recently, immunotherapy has become an attractive new strategy in the treatment of cancer. GcMAF-based immunotherapy can be combined with many other therapies. Sonodynamic therapy (SDT) using low-intensity ultrasound is a novel therapeutic modality. Ultrasound has been demonstrated to activate a number of sonosensitive agents allowing for the possibility of non-invasive targeted treatment for both superficial and deep-seated tumors. The current case study demonstrates that GcMAF and SDT can be used in combination with conventional therapies in patients with metastatic cancer, especially where treatment options are limited due to factors such as toxicity. This case study also suggests a new concept of cancer treatment using local destruction of cancer tissue, in this case conducted with SDT, to be used in combination with GcMAF immunotherapy as a systemic treatment. Copyright© 2014 International Institute of Anticancer Research (Dr. John G. Delinassios), All rights reserved.

Enhanced visible light photocatalytic activity of g-C3N4 assisted by hydrogen peroxide

Science.gov (United States)

Chen, Quan-Liang; Liu, Yi-Ling; Tong, Li-Ge

2018-04-01

Water pollution has caused much attention nowadays. Photocatalysis as a kind of advanced oxidation technology has been widely studied in the field of environmental pollution control. As a stable non-metal photocatalyst, the photocatalytic activity of g-C3N4 assisted by H2O2 was investigated for the degradation of Rhodamine B (RhB) under visible light irradiation. The combination of g-C3N4 and H2O2 has much higher activity than that of pure g-C3N4 or H2O2. Neutral solution is preferred for the high phtotocatalytic activity of g-C3N4 with H2O2. The effect of the amount of catalyst, H2O2 concentration and RhB concentration was investigated. Photocatalytic mechanism study using radical scavenger showed free radicals {{{{O}}}2}- and · OH are the main active species. g-C3N4 assisted by H2O2 showed good photostability and repeatability after five cycles of degradation experiment.

Vascular endothelial growth factor (VEGF-634G/C) polymorphism and retinopathy of prematurity: a meta-analysis

Science.gov (United States)

Malik, Manzoor Ahmad; Shukla, Swati; Azad, Shorya Vardhan; Kaur, Jasbir

2014-01-01

Purpose Vascular endothelial growth factor polymorphism (VEGF-634G/C, rs 2010963) has been considered a risk factor for the development of retinopathy of prematurity (ROP). However, the results remain controversial. Therefore, the aim of the present meta-analysis was to determine the association between VEGF-634G/C polymorphism and ROP risk. Methods Published literature from PubMed and other databases were retrieved. All studies evaluating the association between VEGF-634G/C polymorphism and ROP risk were included. Pooled odds ratio (OR) and 95% confidence interval (CI) were calculated using random or fixed effects model. A total of six case-control studies including 355 cases and 471 controls were included. Results By pooling all the studies, we found that VEGF-634G/C polymorphism was not associated with ROP risk at co-dominant and allele levels and no association was also found in dominant and recessive models. While stratifying on ethnicity level no association was observed in Caucasian and Asian population. Discussion This meta-analysis suggests that VEGF-634G/C polymorphism may not be associated with ROP risk, the association between single VEGF-634G/C polymorphism and ROP risk awaits further investigation. PMID:25473347

Clandestine laboratory scene investigation and processing using portable GC/MS

Science.gov (United States)

Matejczyk, Raymond J.

1997-02-01

This presentation describes the use of portable gas chromatography/mass spectrometry for on-scene investigation and processing of clandestine laboratories. Clandestine laboratory investigations present special problems to forensic investigators. These crime scenes contain many chemical hazards that must be detected, identified and collected as evidence. Gas chromatography/mass spectrometry performed on-scene with a rugged, portable unit is capable of analyzing a variety of matrices for drugs and chemicals used in the manufacture of illicit drugs, such as methamphetamine. Technologies used to detect various materials at a scene have particular applications but do not address the wide range of samples, chemicals, matrices and mixtures that exist in clan labs. Typical analyses performed by GC/MS are for the purpose of positively establishing the identity of starting materials, chemicals and end-product collected from clandestine laboratories. Concerns for the public and investigator safety and the environment are also important factors for rapid on-scene data generation. Here is described the implementation of a portable multiple-inlet GC/MS system designed for rapid deployment to a scene to perform forensic investigations of clandestine drug manufacturing laboratories. GC/MS has long been held as the 'gold standard' in performing forensic chemical analyses. With the capability of GC/MS to separate and produce a 'chemical fingerprint' of compounds, it is utilized as an essential technique for detecting and positively identifying chemical evidence. Rapid and conclusive on-scene analysis of evidence will assist the forensic investigators in collecting only pertinent evidence thereby reducing the amount of evidence to be transported, reducing chain of custody concerns, reducing costs and hazards, maintaining sample integrity and speeding the completion of the investigative process.

Determination of polycyclic aromatic hydrocarbons in deposited waste using GC-MSD. Bestimmung von polycyclischen aromatischen Kohlenwasserstoffen in Deponiegut mittels GC-MSD

Energy Technology Data Exchange (ETDEWEB)

Treffert, U. (chemlab, Gesellschaft fuer Analytik und Umweltberatung mbH, Bensheim (Germany). Abt. ' ' Organische Analytik' ' ); Kolb, M. (Fachhochschule Aalen (Germany)); Stoerk, H. (chemlab, Gesellschaft fuer Analytik und Umweltberatung mbH, Bensheim (Germany))

1999-06-01

The articel describes an analysis method for the determination of 16 polycyclic aromatic hydrocarbons in deposited waste. The single steps are described very detailed: sample preparation by extraction, evaporation, flash-chromatography (Al[sub 2]O[sub 3]), quantitative analysis by GC-MSD. (SR)

GC-MS profile of antimicrobial and antioxidant fractions from Cordia rothii roots.

Science.gov (United States)

Khan, Kehkashan; Firdous, Sadiqa; Ahmad, Aqeel; Fayyaz, Nida; Nadir, Muhammad; Rasheed, Munawwer; Faizi, Shaheen

2016-11-01

An ethnobotanical survey of Cordia rothii Roem. & Schult. (Boraginaceae) reveals it as a medicinal plant. Antimicrobial and antioxidant potential evaluation and identification of chemical constituents via GC-MS of C. rothii roots fractions. To the best of our knowledge, this is the first systematic investigation of the roots exploiting GC-MS. Extraction and fractionation of C. rothii roots furnished various fractions using solvents of varying polarity, i.e., n-hexane, chloroform, ethyl acetate, acetone and methanol. In vitro antimicrobial and antioxidant screening was performed using disk diffusion and DPPH methods, respectively. MIC of active fractions was also determined using disk diffusion method. GC-MS was used to identify constituents which may be responsible for these activities. Among various fractions from C. rothii roots, fraction KA-C showed strong antibacterial activity against 17 microorganisms tested, with MIC ranging from 250-31.25 μg/mL. Fractions KA-A, KM and KM-A exhibited significant antioxidant potential with EC 50 46.875 μg/mL, while fractions KEA-PE, KM-PE and KM-M were good with EC 50 93.750 μg/mL. Forty-five phytochemicals were identified in GC-MS studies including eight hydrocarbons, six free fatty acids, 11 fatty acids esters, two phenylpropanoids, four aromatics, four terpenoid quinones/hydroquinones, three triterpenes, four phytosterols, two hexose metabolites and a DNA base. Of these, 32 constituents have been reported for the first time from C. rothii, 24 from genus Cordia and 15 from Boraginaceae. Strong antibacterial and antioxidant potential of C. rothii roots may be due to the contribution of phytoconstituents identified through GC-MS studies.

X-linked adrenoleukodystrophy: clinical and laboratory findings in 15 Brazilian patients

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Carmen R. Vargas

2000-06-01

Full Text Available Adrenoleukodystrophy (X-ALD is an X-linked recessively inherited peroxisomal disorder, phenotypically heterogeneous, characterized by progressive white-matter demyelination of the central nervous system and adrenocortical insufficiency. We investigated 15 male X-ALD patients varying in age from 7 to 39, diagnosed among 108 suspected patients referred for investigation. Plasma levels of very long chain fatty acids (VLCFA were measured at our laboratory using gas chromatography (GC. Eleven cases of childhood X-ALD and four cases of adrenomyeloneuropathy (AMN were diagnosed. Adrenal leukodystrophy insufficiency and limb weakness were the most frequent symptoms, appearing in 12, 8 and 6 of the patients, respectively. Physician awareness of X-ALD seems inadequate to judge by age at diagnosis and lengthy interval between the start of symptoms and diagnosis. This is the first published series of Brazilian patients with X-ALD. We determined signs and symptoms relevant for diagnosis, as early identification seems important for treatment outcome. In addition, diagnosis identifies carriers, who could benefit from genetic counselling and prenatal diagnosis.Adrenoleucodistrofia (X-ALD é uma desordem peroxissomal com padrão de herança ligada ao X, fenotipicamente heterogênea, caracterizada por uma progressiva desmielinização da substância branca do sistema nervoso central e por insuficiência adrenal. Foram investigados por nós 15 pacientes do sexo masculino com sinais clínicos sugestivos de X-ALD, com idade entre 7 e 39 anos, diagnosticados entre 108 pacientes encaminhados para investigação por suspeita clínica. Os níveis plasmáticos dos ácidos graxos de cadeia muito longa (VLCFA foram dosados em nosso laboratório através de cromatografia gasosa (GC. Onze (73% casos da forma infantil de X-ALD (ALD e 4 (27% casos de adrenomieloneuropatia (AMN foram diagnosticados. Insuficiência leucodistrofia adrenal e fraqueza muscular foram os sinais mais

Efeito do óleo essencial de pimenta longa (Piper hispidinervum C. DC e do emulsificante Tween® 80 sobre o crescimento micelial de Alternaria alternata (Fungi: Hyphomycetes The effect of Long-pepper essential oil (Piper hispidinervum C. DC. and of Tween®; 80 emulsifier on the mycelial growth of Alternaria alternate (Fungi: Hyphomycetes

Directory of Open Access Journals (Sweden)

Fabiane Reis Nascimento

2008-01-01

Full Text Available Este trabalho objetivou avaliar o efeito do óleo essencial de folhas de pimenta longa (Piper hispidinervum C. DC, sobre o crescimento micelial de Alternaria alternata e a análise da influência da concentração do emulsificante Tween® 80 no controle deste fitopatógeno. O óleo essencial foi obtido pela técnica "arraste a vapor d'água", utilizando-se aparelho de Clevenger modificado, e posteriormente submetido, à análise por cromatografia em fase gasosa acoplada a espectrômetro de massas CG-EM a CG. Para os ensaios biológicos, o método foi o bioanalítico in vitro observando-se o crescimento ou inibição do micélio de A. alternata no meio de cultura BDA na presença de diferentes concentrações do óleo essencial (0, 100, 250, 500 e 1000 mgL-1 sob diferentes concentrações de Tween® 80. Adotou-se esquema fatorial com quatro repetições, em delineamento inteiramente casualizado (DIC. Observou-se que o óleo essencial de pimenta longa apresentou inibição sobre o crescimento micelial do fungo A. alternataem todas as concentrações analisadas, sendo que na concentração de 1000 mgL-1 esta inibição foi de 100% , e a porcentagem de emulsificante (Tween® 80, influenciou na atividade fungitóxica das concentrações de 250 mgL -1 e 500 mgL -1 do óleo essencial.The object of this work was to evaluate the effectof essential oils from Long-pepper leaves Piper hispidinervum on the mycelial growth of Alternaria alternata and to analyze the influence of emulsifier Tween® 80 concentration in the control of this phytopathogen. The essential oil was obtained by steam stream distillation, using a modified Clevenger apparatus, and the chemical composition was analyzed by gas chromatography coupled to mass spectroscopy GC-MS and GC. For biological tests, the bioanalytical in vitro method was used, observing the growth or inhibition of such phytopathogen in BDA culture media, in the presence of different essential oil concentrations (0, 100

GC and GC-MS characterization of crude oil transformation in sediments and microbial mat samples after the 1991 oil spill in the Saudi Arabian Gulf coast

International Nuclear Information System (INIS)

Garcia de Oteyza, T.; Grimalt, J.O.

2006-01-01

The massive oil discharge in the Saudi Arabian coast at the end of the 1991 Gulf War is used here as a natural experiment to study the ability of microbial mats to transform oil residues after major spills. The degree of oil transformation has been evaluated from the analysis of the aliphatic and aromatic hydrocarbons by gas chromatography (GC) and GC coupled to mass spectrometry (GC-MS). The oil-polluted microbial mat samples from coastal environments exhibited an intermediate degree of transformation between that observed in superficial and deep sediments. Evaporation, photo-oxidation and water-washing seemed to lead to more effective and rapid elimination of hydrocarbons than cyanobacteria and its associated microorganisms. Furthermore, comparison of some compounds (e.g. regular isoprenoid hydrocarbons or alkylnaphthalenes) in the oil collected in the area after the spill or in the mixtures retained by cyanobacterial growth gave rise to an apparent effect of hydrocarbon preservation in the microbial mat ecosystems. - Cyanobacterial mats inhibit degradation of oil by reducing exposure to the atmosphere and seawater

Analysis of pesticide residues in strawberries and soils by GC-MS/MS, LC-MS/MS and two-dimensional GC-time-of-flight MS comparing organic and integrated pest management farming.

Science.gov (United States)

Fernandes, Virgínia C; Lehotay, Steven J; Geis-Asteggiante, Lucía; Kwon, Hyeyoung; Mol, Hans G J; van der Kamp, Henk; Mateus, Nuno; Domingues, Valentina F; Delerue-Matos, Cristina

2014-01-01

This study analysed 22 strawberry and soil samples after their collection over the course of 2 years to compare the residue profiles from organic farming with integrated pest management practices in Portugal. For sample preparation, we used the citrate-buffered version of the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method. We applied three different methods for analysis: (1) 27 pesticides were targeted using LC-MS/MS; (2) 143 were targeted using low pressure GC-tandem mass spectrometry (LP-GC-MS/MS); and (3) more than 600 pesticides were screened in a targeted and untargeted approach using comprehensive, two-dimensional gas chromatography time-of-flight mass spectrometry (GC × GC-TOF-MS). Comparison was made of the analyses using the different methods for the shared samples. The results were similar, thereby providing satisfactory confirmation of both similarly positive and negative findings. No pesticides were found in the organic-farmed samples. In samples from integrated pest management practices, nine pesticides were determined and confirmed to be present, ranging from 2 µg kg(-1) for fluazifop-p-butyl to 50 µg kg(-1) for fenpropathrin. Concentrations of residues in strawberries were less than European maximum residue limits.

TOXICOLOGICAL DRUG SCREENING BY GC-MS VERSUS HPLC-DAD USING A COMMON EFFICIENT EXTRACTION PROCEDURE SCREENING TOXICOLOGIQUE DES MEDICAMENTS PAR HPLC-DAD ET GC-MS: PROTOCOLE D’EXTRACTION UNIQUE

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SELOUA ELMRABEH

2015-05-01

Full Text Available This paper presents a common extraction method for toxicological drug screening by gas chromatography-mass spectrometry (GC-MS and high-performance liquid chromatography with diode-array detection (HPLC-DAD. Liquid-liquid extraction was performed using plasma of 104 samples at the Laboratory of Moroccan Poison Control and Pharmacovigilance Center during a period of 12 months. The results obtained by HPLC-DAD are compared with those determined with GC-MS. 76 cases (73.08 % were found positive for at least by one of these two techniques. HPLC-DAD identified 59.87 % of all positive results, and 10 molecules were identified only by HPLC-DAD. GC/MS identified 40.13 % of all positives, and 4 molecules were identified only by GC/MS. In order to evaluate the performance of this extraction method, an extraction yield was calculated for three classes of drugs. All the analyzed molecules were obtained in satisfactory yields (higher than 50 % except for carbamazepine, amitriptyline and nortriptyline. Overall, the results indicate that the extraction method is well adapted for toxicological drug screening. The use of common extraction simultaneously for the two techniques can reduce workload and costs of screening, while increasing the validity and reliability of the results.

N-Glycans on the Rift Valley Fever Virus Envelope Glycoproteins Gn and Gc Redundantly Support Viral Infection via DC-SIGN

Science.gov (United States)

Phoenix, Inaia; Nishiyama, Shoko; Lokugamage, Nandadeva; Hill, Terence E.; Huante, Matthew B.; Slack, Olga A.L.; Carpio, Victor H.; Freiberg, Alexander N.; Ikegami, Tetsuro

2016-01-01

Rift Valley fever is a mosquito-transmitted, zoonotic disease that infects humans and ruminants. Dendritic cell specific intercellular adhesion molecule 3 (ICAM-3) grabbing non-integrin (DC-SIGN) acts as a receptor for members of the phlebovirus genus. The Rift Valley fever virus (RVFV) glycoproteins (Gn/Gc) encode five putative N-glycan sequons (asparagine (N)–any amino acid (X)–serine (S)/threonine (T)) at positions: N438 (Gn), and N794, N829, N1035, and N1077 (Gc). The N-glycosylation profile and significance in viral infection via DC-SIGN have not been elucidated. Gc N-glycosylation was first evaluated by using Gc asparagine (N) to glutamine (Q) mutants. Subsequently, we generated a series of recombinant RVFV MP-12 strain mutants, which encode N-to-Q mutations, and the infectivity of each mutant in Jurkat cells stably expressing DC-SIGN was evaluated. Results showed that Gc N794, N1035, and N1077 were N-glycosylated but N829 was not. Gc N1077 was heterogeneously N-glycosylated. RVFV Gc made two distinct N-glycoforms: “Gc-large” and “Gc-small”, and N1077 was responsible for “Gc-large” band. RVFV showed increased infection of cells expressing DC-SIGN compared to cells lacking DC-SIGN. Infection via DC-SIGN was increased in the presence of either Gn N438 or Gc N1077. Our study showed that N-glycans on the Gc and Gn surface glycoproteins redundantly support RVFV infection via DC-SIGN. PMID:27223297

Optimization of temperature-programmed GC separations. II. Off-line simplex optimization and column selection

NARCIS (Netherlands)

Snijders, H.M.J.; Janssen, J.G.M.; Cramers, C.A.M.G.; Sandra, P; Bertsch, W.; Sandra, P.; Devos, G.

1996-01-01

In this work a method is described which allows off-line optimization of temperature programmed GC separations. Recently, we described a new numerical method to predict off-line retention times and peak widths of a mixture containing components with known identities in capillary GC. In the present

Safety Pharmacology, Toxicology and Pharmacokinetic Assessment of Human Gc Globulin (Vitamin D Binding Protein)

DEFF Research Database (Denmark)

Pihl, Tina Holberg; Jørgensen, Charlotte Svaerke; Santoni-Rugiu, Eric

2010-01-01

Gc globulin is an important protein of the plasma actin-scavenger system. As such, it has been shown to bind free actin and prevent hypercoagulation and shock in patients with massive actin release resulting from severe tissue injuries. Treatment of such patients with Gc globulin could therefore...

In situ loading of Ag_2WO_4 on ultrathin g-C_3N_4 nanosheets with highly enhanced photocatalytic performance

International Nuclear Information System (INIS)

Li, Yunfeng; Jin, Renxi; Fang, Xu; Yang, Yang; Yang, Man; Liu, Xianchun; Xing, Yan; Song, Shuyan

2016-01-01

Graphical abstract: Ultrathin g-C_3N_4 nanosheets (g-C_3N_4−NS) with improved electron transport ability and large number of active sites are employed instead of bulk g-C_3N_4 to prepare the Ag_2WO_4/g-C_3N_4−NS heterostructured photocatalysts, which exhibit remarkable photocatalytic activity for wastewater treatment. - Highlights: • Ag2WO4/g-C3N4-NS photocatalysts were obtained by a deposition-precipitation method. • Ag2WO4/g-C3N4-NS possess large surface areas and increased lifetime of charges. • Ag2WO4/g-C3N4-NS exhibit enhanced activity on degradation of RhB and MO. • The photocatalytic mechanism of the Ag2WO4/g-C3N4-NS system were investigated. - Abstract: The g-C_3N_4 nanosheets (g-C_3N_4−NS) exhibit more excellent property than common bulk g-C_3N_4 (g-C_3N_4-B) due to their large surface areas, improved electron transport ability and well dispersion in water. In this work, ultrathin g-C_3N_4−NS with a thickness of about 2.7 nm have been synthesized by a simple thermal exfoliation of bulk g-C_3N_4, and then Ag_2WO_4 nanoparticles are in situ loaded on their surface to construct the Ag_2WO_4/g-C_3N_4−NS heterostructured photocatalysts. Due to their unique physicochemical properties, the as-prepared heterostructures possess a fast interfacial charge transfer and increased lifetime of photo-excited charge carriers, and exhibit much higher photocatalytic activity. Under visible light irradiation, the optimum photocatalytic activity of Ag_2WO_4/g-C_3N_4−NS composites is almost 53.6 and 26.5 times higher than that of pure g-C_3N_4-B and Ag_2WO_4/g-C_3N_4-B heterostructures towards the degradation of rhodamine B, respectively, and is almost 30.6 and 9.8 times higher towards the degradation of methyl orange, respectively. In addition, the natural sunlight photocatalytic activities of the as-prepared samples are also investigated.

Emprego de cromatografia líquida de alta eficiência hidrofílica na determinação dos aminoácidos de hidrolisados de caseína

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Carreira Raquel Linhares

2002-01-01

Full Text Available O emprego de cromatografia líquida de alta eficiência de interação hidrofílica (HILIC foi estudado visando a separação e a quantificação dos aminoácidos essenciais. Alguns parâmetros foram testados, tais como a composição da fase móvel e a velocidade do fluxo. Determinou-se, ainda, o limite de quantificação, a linearidade e a repetibilidade desta técnica. Os resultados obtidos indicaram as vantagens desta metodologia em termos de tempo, economia e simplicidade, quando comparada a outras técnicas de determinação dos aminoácidos, uma vez que dispensa a derivação pré-coluna e permite trabalhar em modo isocrático. A sua aplicação, na análise de frações cromatográficas de hidrolisados de caseína, revelou a importância da HILIC na avaliação nutricional destas preparações.

Safety pharmacology, toxicology and pharmacokinetic assesment of human Gc globulin (vitamin d binding protein)

DEFF Research Database (Denmark)

Pihl, Tina Holberg; Jørgensen, Charlotte Sværke; Santoni Rugiu, Eric

2010-01-01

  Gc globulin is an important protein of the plasma actin-scavenger system. As such, it has been shown to bind free actin and prevent hypercoagulation and shock in patients with massive actin release resulting from severe tissue injuries. Treatment of such patients with Gc globulin could therefore...

Gas Chromatography (GC) – Mass Spectrometry (MS) analysis of ...

African Journals Online (AJOL)

MS. Glycosides, phenolics and alkaloids were indicated in large amount; eugenols and terpenes were also present while saponin, tannins and steroid were absent. Major components detected by GC-MS were 2-Hydroxy hexadecanoic acid ...

Survivin -31 G/C polymorphism might contribute to colorectal cancer (CRC) risk: a meta-analysis.

Science.gov (United States)

Yao, Linhua; Hu, Yi; Deng, Zhongmin; Li, Jingjing

2015-01-01

Published data has shown inconsistent findings about the association of survivin -31 G/C polymorphism with the risk of colorectal cancer (CRC). This meta-analysis quantitatively assesses the results from published studies to provide a more precise estimate of the association between survivin -31 G/C polymorphism as a possible predictor of the risk of CRC. We conducted a literature search in the PubMed, Web of Science, and Cochrane Library databases. Stata 12 software was used to calculate the pooled odds ratios (ORs) with 95% confidence intervals (CIs) based on the available data from each article. Six studies including 1840 cases with CRC and 1804 controls were included in this study. Survivin -31 G/C polymorphism was associated with a significantly increased risk of CRC (OR = 1.78; 95% CI, 1.53-2.07; I(2) = 0%). In the race subgroup analysis, both Asians (OR = 1.72; 95% CI, 1.44-2.05; I(2) = 0%) and Caucasians (OR = 1.93; 95% CI, 1.46-2.55; I(2) = 0%) with survivin -31 G/C polymorphism had increased CRC risk. In the subgroup analysis according to site of CRC, survivin -31 G/C polymorphism was not associated with colon cancer risk (OR = 2.02; 95% CI, 0.79-5.22; I(2) = 82%). However, this polymorphism was significantly associated with rectum cancer risk (OR = 1.98; 95% CI, 1.42-2.74; I(2) = 0%). In the subgroup analysis by clinical stage, both early stage (I+II) and advanced stage (III+IV) were associated with survivin -31 G/C polymorphism (OR = 1.61; 95% CI, 1.20-2.16; I(2) = 0% and OR = 2.30; 95% CI, 1.70-3.13; I(2) = 0%, respectively). In the subgroup analysis by smoke status, both smokers and non-smokers with survivin -31 G/C polymorphism showed increased CRC risk (OR = 1.47; 95% CI, 1.01-2.13; I(2) = 60% and OR = 1.71; 95% CI, 1.28-2.30; I(2) = 0%, respectively). In the subgroup analysis by drink status, both drinkers and non-drinkers with survivin -31 G/C polymorphism showed increased CRC risk (OR = 1.58; 95% CI, 1.06-2.37; I(2) = 8% and OR = 1.61; 95% CI, 1

Can mutational GC-pressure create new linear B-cell epitopes in herpes simplex virus type 1 glycoprotein B?

Science.gov (United States)

Khrustalev, Vladislav Victorovich

2009-01-01

We showed that GC-content of nucleotide sequences coding for linear B-cell epitopes of herpes simplex virus type 1 (HSV1) glycoprotein B (gB) is higher than GC-content of sequences coding for epitope-free regions of this glycoprotein (G + C = 73 and 64%, respectively). Linear B-cell epitopes have been predicted in HSV1 gB by BepiPred algorithm ( www.cbs.dtu.dk/services/BepiPred ). Proline is an acrophilic amino acid residue (it is usually situated on the surface of protein globules, and so included in linear B-cell epitopes). Indeed, the level of proline is much higher in predicted epitopes of gB than in epitope-free regions (17.8% versus 1.8%). This amino acid is coded by GC-rich codons (CCX) that can be produced due to nucleotide substitutions caused by mutational GC-pressure. GC-pressure will also lead to disappearance of acrophobic phenylalanine, isoleucine, methionine and tyrosine coded by GC-poor codons. Results of our "in-silico directed mutagenesis" showed that single nonsynonymous substitutions in AT to GC direction in two long epitope-free regions of gB will cause formation of new linear epitopes or elongation of previously existing epitopes flanking these regions in 25% of 539 possible cases. The calculations of GC-content and amino acid content have been performed by CodonChanges algorithm ( www.barkovsky.hotmail.ru ).

Insights into the photocatalytic mechanism of mediator-free direct Z-scheme g-C3N4/Bi2MoO6(010) and g-C3N4/Bi2WO6(010) heterostructures: A hybrid density functional theory study

Science.gov (United States)

Opoku, Francis; Govender, Krishna Kuben; Sittert, Cornelia Gertina Catharina Elizabeth van; Govender, Penny Poomani

2018-01-01

Graphite-like carbon nitride (g-C3N4)-based heterostructures have received much attention due to their prominent photocatalytic activity. The g-C3N4/Bi2WO6 and g-C3N4/Bi2MoO6 heterostructures, which follow a typical hetero-junction charge transfer mechanisms show a weak potential for hydrogen evolution and reactive radical generation under visible light irradiation. A mediator-free Z-scheme g-C3N4/Bi2MoO6(010) and g-C3N4/Bi2WO6(010) heterostructures photocatalyst are designed for the first time using first-principles studies. Moreover, theoretical understanding of the underlying mechanism, the effects of interfacial composition and the role the interface play in the overall photoactivity is still unexplained. The calculated band gap of the heterostructures is reduced compared to the bulk Bi2WO6 and Bi2MoO6. In this study, we systematically calculated energy band structure, optical properties and charge transfer of the g-C3N4/Bi2MoO6(010) and g-C3N4/Bi2WO6(010) heterostructures using the hybrid density functional theory approach. The results show that the charge transfer at the interface of the heterostructures induces a built-in potential, which benefits the separation of photogenerated charge carriers. The g-C3N4/Bi2MoO6(010) heterostructure with more negative adhesion energy (-1.10 eVA-2) is predicted to have a better adsorptive ability and can form more easily compared to the g-C3N4/Bi2WO6(010) interface (-1.16 eVA-2). Therefore, our results show that the g-C3N4 interaction with Bi2MoO6 is stronger than Bi2WO6, which is also verified by the smaller vertical separation (3.25 Å) between Bi2MoO6 and g-C3N4 compared to the g-C3N4/Bi2WO6(010) interface (3.36 Å). The optical absorption verifies that these proposed Z-scheme heterostructures are excellent visible light harvesting semiconductor photocatalyst materials. This enhancement is ascribed to the role of g-C3N4 monolayer as an electron acceptor and the direct Z-scheme charge carrier transfer at the interface of

Ultrathin g-C3N4 films supported on Attapulgite nanofibers with enhanced photocatalytic performance

Science.gov (United States)

Xu, Yongshuai; Zhang, Lili; Yin, Minghui; Xie, Dengyu; Chen, Jiaqi; Yin, Jingzhou; Fu, Yongsheng; Zhao, Pusu; Zhong, Hui; Zhao, Yijiang; Wang, Xin

2018-05-01

A novel visible-light-responsive photocatalyst is fabricated by introducing g-C3N4 ultrathin films onto the surface of attapulgite (ATP) via a simple in-situ depositing technique, in which ATP was pre-grafted using (3-Glycidyloxypropyl) trimethoxysilane (KH560) as the surfactant. A combination of XRD, FT-IR, BET, XPS, UV-vis, TEM and SEM techniques are utilized to characterize the composition, morphology and optical properties of the products. The results show that with the help of KH560, g-C3N4 presented as ultrathin layer is uniformly loaded onto the surface of ATP by forming a new chemical bond (Sisbnd Osbnd C). Comparing with g-C3N4 and ATP, ATP/g-C3N4 exhibits remarkably enhanced visible-light photocatalytic activity in degradation of methyl orange (MO) because of its high surface area, appropriate band gap and the synergistic effect between g-C3N4 and ATP. To achieve the best photocatalyst, the ratio of g-C3N4 was adjusted by controlling the mass portion between ATP-KH560 and melamine (r = m (ATP-KH560)/m (melamine)). The highest decomposition rate of methyl orange (MO) was 96.06% when r = 0.5 and this degradation efficiency remained unchanged after 4 cycles, which is 10 times as that of pure g-C3N4 particles. Possible photocatalytic mechanism is presented.

Exploring the formation and electronic structure properties of the g-C3N4 nanoribbon with density functional theory.

Science.gov (United States)

Wu, Hong-Zhang; Zhong, Qing-Hua; Bandaru, Sateesh; Liu, Jin; Lau, Woon Ming; Li, Li-Li; Wang, Zhenling

2018-04-18

The optical properties and condensation degree (structure) of polymeric g-C 3 N 4 depend strongly on the process temperature. For polymeric g-C 3 N 4 , its structure and condensation degree depend on the structure of molecular strand(s). Here, the formation and electronic structure properties of the g-C 3 N 4 nanoribbon are investigated by studying the polymerization and crystallinity of molecular strand(s) employing first-principle density functional theory. The calculations show that the width of the molecular strand has a significant effect on the electronic structure of polymerized and crystallized g-C 3 N 4 nanoribbons, a conclusion which would be indirect evidence that the electronic structure depends on the structure of g-C 3 N 4 . The edge shape also has a distinct effect on the electronic structure of the crystallized g-C 3 N 4 nanoribbon. Furthermore, the conductive band minimum and valence band maximum of the polymeric g-C 3 N 4 nanoribbon show a strong localization, which is in good agreement with the quasi-monomer characters. In addition, molecular strands prefer to grow along the planar direction on graphene. These results provide new insight on the properties of the g-C 3 N 4 nanoribbon and the relationship between the structure and properties of g-C 3 N 4 .

Metabolomic and elemental analysis of camel and bovine urine by GC-MS and ICP-MS.

Science.gov (United States)

Ahamad, Syed Rizwan; Alhaider, Abdul Qader; Raish, Mohammad; Shakeel, Faiyaz

2017-01-01

Recent studies from the author's laboratory indicated that camel urine possesses antiplatelet activity and anti-cancer activity which is not present in bovine urine. The objective of this study is to compare the volatile and elemental components of bovine and camel urine using GC-MS and ICP-MS analysis. We are interested to know the component that performs these biological activities. The freeze dried urine was dissolved in dichloromethane and then derivatization process followed by using BSTFA for GC-MS analysis. Thirty different compounds were analyzed by the derivatization process in full scan mode. For ICP-MS analysis twenty eight important elements were analyzed in both bovine and camel urine. The results of GC-MS and ICP-MS analysis showed marked difference in the urinary metabolites. GC-MS evaluation of camel urine finds a lot of products of metabolism like benzene propanoic acid derivatives, fatty acid derivatives, amino acid derivatives, sugars, prostaglandins and canavanine. Several research reports reveal the metabolomics studies on camel urine but none of them completely reported the pharmacology related metabolomics. The present data of GC-MS suggest and support the previous studies and activities related to camel urine.

Experimento didático sobre cromatografia gasosa: uma abordagem analítica e ambiental Didactic experiment on gas chromatography: an environmental and analytical approach

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José Carlos P. Penteado

2008-01-01

Full Text Available This paper describes an experiment to teach the principles of gas chromatography exploring the boiling points and polarities to explain the elution order of a series of alcohols, benzene and n-propanone, as well as to teach the response factor concept and the internal standard addition method. Retention times and response factors are used for qualitative identification and quantitative analysis of a hypothetical contamination source in a simulated water sample. The internal standard n-propanol is further used for quantification of benzene and n-butanol in the water sample. This experiment has been taught in the instrumental analysis course offered to chemistry and oceanography students.

Open Probe fast GC-MS - combining ambient sampling ultra-fast separation and in-vacuum ionization for real-time analysis.

Science.gov (United States)

Keshet, U; Alon, T; Fialkov, A B; Amirav, A

2017-07-01

An Open Probe inlet was combined with a low thermal mass ultra-fast gas chromatograph (GC), in-vacuum electron ionization ion source and a mass spectrometer (MS) of GC-MS for obtaining real-time analysis with separation. The Open Probe enables ambient sampling via sample vaporization in an oven that is open to room air, and the ultra-fast GC provides ~30-s separation, while if no separation is required, it can act as a transfer line with 2 to 3-s sample transfer time. Sample analysis is as simple as touching the sample, pushing the sample holder into the Open Probe oven and obtaining the results in 30 s. The Open Probe fast GC was mounted on a standard Agilent 7890 GC that was coupled with an Agilent 5977A MS. Open Probe fast GC-MS provides real-time analysis combined with GC separation and library identification, and it uses the low-cost MS of GC-MS. The operation of Open Probe fast GC-MS is demonstrated in the 30-s separation and 50-s full analysis cycle time of tetrahydrocannabinol and cannabinol in Cannabis flower, sub 1-min analysis of trace trinitrotoluene transferred from a finger onto a glass surface, vitamin E in canola oil, sterols in olive oil, polybrominated flame retardants in plastics, alprazolam in Xanax drug pill and free fatty acids and cholesterol in human blood. The extrapolated limit of detection for pyrene is Open Probe fast GC-MS is demonstrated in the analysis of heroin in its street drug powder. The use of Open Probe with the fast GC acting as a transfer line is demonstrated in <10-s analysis without separation of ibuprofen and estradiol. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

Genomic Mapping of Human DNA provides Evidence of Difference in Stretch between AT and GC rich regions

Science.gov (United States)

Reifenberger, Jeffrey; Dorfman, Kevin; Cao, Han

Human DNA is a not a polymer consisting of a uniform distribution of all 4 nucleic acids, but rather contains regions of high AT and high GC content. When confined, these regions could have different stretch due to the extra hydrogen bond present in the GC basepair. To measure this potential difference, human genomic DNA was nicked with NtBspQI, labeled with a cy3 like fluorophore at the nick site, stained with YOYO, loaded into a device containing an array of nanochannels, and imaged. Over 473,000 individual molecules of DNA, corresponding to roughly 30x coverage of a human genome, were collected and aligned to the human reference. Based on the known AT/GC content between aligned pairs of labels, the stretch was measured for regions of similar size but different AT/GC content. We found that regions of high GC content were consistently more stretched than regions of high AT content between pairs of labels varying in size between 2.5 kbp and 500 kbp. We measured that for every 1% increase in GC content there was roughly a 0.06% increase in stretch. While this effect is small, it is important to take into account differences in stretch between AT and GC rich regions to improve the sensitivity of detection of structural variations from genomic variations. NIH Grant: R01-HG006851.

Interglomerular Connectivity within the Canonical and GC-D/Necklace Olfactory Subsystems.

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Cedric R Uytingco

Full Text Available The mammalian main olfactory system contains several subsystems that differ not only in the receptors they express and the glomerular targets they innervate within the main olfactory bulb (MOB, but also in the strategies they use to process odor information. The canonical main olfactory system employs a combinatorial coding strategy that represents odorant identity as a pattern of glomerular activity. By contrast, the "GC-D/necklace" olfactory subsystem-formed by olfactory sensory neurons expressing the receptor guanylyl cyclase GC-D and their target necklace glomeruli (NGs encircling the caudal MOB-is critical for the detection of a small number of semiochemicals that promote the acquisition of food preferences. The formation of these socially-transmitted food preferences requires the animal to integrate information about two types of olfactory stimuli: these specialized social chemosignals and the food odors themselves. However, the neural mechanisms with which the GC-D/necklace subsystem processes this information are unclear. We used stimulus-induced increases in intrinsic fluorescence signals to map functional circuitry associated with NGs and canonical glomeruli (CGs in the MOB. As expected, CG-associated activity spread laterally through both the glomerular and external plexiform layers associated with activated glomeruli. Activation of CGs or NGs resulted in activity spread between the two types of glomeruli; there was no evidence of preferential connectivity between individual necklace glomeruli. These results support previous anatomical findings that suggest the canonical and GC-D/necklace subsystems are functionally connected and may integrate general odor and semiochemical information in the MOB.

Insights into the photocatalytic mechanism of mediator-free direct Z-scheme g-C3N4/Bi2MoO6(010) and g-C3N4/Bi2WO6(010) heterostructures: A hybrid density functional theory study

CSIR Research Space (South Africa)

Opoku, F

2018-01-01

Full Text Available Graphite-like carbon nitride (g-C3N4)-based heterostructures have received much attention due to their prominent photocatalytic activity. The g-C3N4/Bi2WO6 and g-C3N4/Bi2MoO6 heterostructures, which follow a typical hetero-junction charge transfer...

Gas Chromatography-Mass Spectroscopic (GC-MS) Analysis of n ...

African Journals Online (AJOL)

1Department of Pharmacognosy and Phytotherapy, 2Department of Pharmaceutics and Pharmaceutical Technology, University of Port Harcourt, Nigeria ... tuber-regium (synonym Pleurotus tuber regium) using gas chromatography-mass spectroscopic (GC- ... Department of Plant Science and Biotechnology,. University of ...

Gas Chromatography-Mass Spectroscopic (GC-MS) Analysis of n ...

African Journals Online (AJOL)

tuber-regium (synonym Pleurotus tuber regium) using gas chromatography-mass spectroscopic (GC-. MS) techniques. Methods: The n-hexane extract of the sclerotia ... Soxhlet extraction and analysed using gas chromatography-mass spectroscopic (MS) techniques. ..... Phytochemical composition of Pleurotus tuber regium.

Surface modification of g-C3N4 by hydrazine: Simple way for noble-metal free hydrogen evolution catalysts

KAUST Repository

Chen, Yin

2015-11-02

The graphitic carbon nitride (g-C3N4) usually is thought to be an inert material and it’s difficult to have the surface terminated NH2 groups functionalized. By modifying the g-C3N4 surface with hydrazine, the diazanyl group was successfully introduced onto the g-C3N4 surface, which allows the introduction with many other function groups. Here we illustrated that by reaction of surface hydrazine group modified g-C3N4 with CS2 under basic condition, a water electrolysis active group C(=S)SNi can be implanted on the g-C3N4 surface, and leads to a noble metal free hydrogen evolution catalyst. This catalyst has 40% hydrogen evolution efficiency compare to the 3 wt% Pt photo precipitated g-C3N4, with only less than 0.2 wt% nickel.

Surface modification of g-C3N4 by hydrazine: Simple way for noble-metal free hydrogen evolution catalysts

KAUST Repository

Chen, Yin; Lin, Bin; Wang, Hong; Yang, Yong; Zhu, Haibo; Yu, Weili; Basset, Jean-Marie

2015-01-01

The graphitic carbon nitride (g-C3N4) usually is thought to be an inert material and it’s difficult to have the surface terminated NH2 groups functionalized. By modifying the g-C3N4 surface with hydrazine, the diazanyl group was successfully introduced onto the g-C3N4 surface, which allows the introduction with many other function groups. Here we illustrated that by reaction of surface hydrazine group modified g-C3N4 with CS2 under basic condition, a water electrolysis active group C(=S)SNi can be implanted on the g-C3N4 surface, and leads to a noble metal free hydrogen evolution catalyst. This catalyst has 40% hydrogen evolution efficiency compare to the 3 wt% Pt photo precipitated g-C3N4, with only less than 0.2 wt% nickel.

Determinação de substitutos da manteiga de cacau em coberturas de chocolate através da análise de triacilgliceróis Determination of cocoa butter substitutes in coating chocolate.by analysis the triacylglycerol composition

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Valéria Paula Rodrigues MINIM

1999-05-01

Full Text Available A legislação brasileira proíbe a adição de substitutos da manteiga de cacau ao chocolate. O presente trabalho teve como objetivo verificar o padrão de qualidade de coberturas comercializadas na região de Campinas. Para isso, foram analisadas cinco marcas de cobertura de chocolate ao leite e quatro de cobertura de chocolate amargo. Para verificar a possível adição de substitutos determinou-se, por cromatografia gasosa a alta temperatura (CGAT, a composição em triacilgliceróis da gordura extraída e os resultados foram analisados pelo método matemático de Padley & Timms. Não foi detectada a presença de substitutos da manteiga de cacau nas amostras de cobertura de chocolate analisadas.Brazilian regulations prohibit the addition of cocoa butter replacements to chocolate, in total or partial substitution. The objective of the present work was to check the quality standards of four of coating bitter Brasilian chocolate bars and five of coating milk chocolate bars, commercialized in Campinas. In order to check the possible addition of substitutes, the triacylglycerol composition was determined, and the results were analysed by Padley & Timms mathematical method. The triacylglycerol composition of each sample was determined by high temperature gas chromatography (HTGC. The presence of cocoa butter replacements was not detected in the brands of coating chocolate.

Acompanhamento do processo de fermentação para produção de cachaça através de métodos microbiológicos e físico-químicos com diferentes isolados de Saccharomyces cerevisiae

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Thaís Louise Soares

2011-03-01

Full Text Available Com a crescente exigência do mercado consumidor por produtos de melhor qualidade, busca-se o constante aprimoramento da produção de cachaça, uma vez que todas as etapas da cadeia produtiva de bebidas fermento-destiladas são importantes. O objetivo deste trabalho foi acompanhar o processo de fermentação para produção de cachaça, utilizando diferentes isolados de Saccharomyces cerevisiae a partir da quantificação de metabólitos secundários por Cromatografia Gasosa. O acompanhamento do processo deu-se desde o preparo do inóculo até o final do processo fermentativo. O estudo foi conduzido na Universidade Federal de Lavras (UFLA. Foram utilizados 8 isolados de Saccharomyces cerevisiae inoculados em caldo de cana, dos quais foram retiradas amostras durante a fase de crescimento em sistema de batelada alimentada e fermentação. As amostras foram analisadas quanto à taxa de floculação, ºBrix e álcoois superiores. Os parâmetros avaliados apresentaram diferenças para cada isolado. O melhor isolado para a produção de cachaça foi o isolado UFLA CA116 por apresentar alto número de células viáveis, maior taxa de floculação, ausência 1-propanol, presença de 1,3 butanediol.

Atividade antimicrobiana do óleo essencial de rizomas de açafrão (Curcuma longa L. e gengibre (Zingiber officinale Roscoe frente a salmonelas entéricas isoladas de frango resfriado

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C. Majolo

2014-09-01

Full Text Available Objetivou-se com este trabalho identificar, quantificar os constituintes, e avaliar a atividade antibacteriana dos óleos essenciais extraídos de rizomas de açafrão (Curcuma longa L. e gengibre (Zingiber officinale Roscoe cultivados nas condições de Manaus/AM frente a 14 salmonelas entéricas isoladas de frango resfriado. A extração dos óleos essenciais foi realizada utilizando-se aparelho tipo Clevenger e a composição determinada por Cromatografia Gasosa acoplada a Espectrometria de Massas (CG-MS. A atividade antibacteriana foi realizada com o emprego de técnica de microdiluição em caldo. O óleo essencial de gengibre se mostrou expressivamente mais eficiente do que o óleo de açafrão, tanto em termos de ação bacteriostática (concentração inibitória mínima de 2500 a 5000 µg.mL-1 quanto bactericida (concentração bactericida mínima de 5000 a 10000 µg.mL-1 observando-se variação apenas em duas as amostras em termos de resistência a ação bactericida deste óleo. Assim, o óleo essencial de gengibre, representa uma alternativa para o controle de Salmonella enterica, entretanto, demais estudos abordando o sinergismo com alimentos são indicados.

Composição de ácidos graxos do leite materno em mulheres residentes em área distante da costa litorânea brasileira

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Renata Y. Nishimura

2013-06-01

Full Text Available OBJETIVOS: Avaliar a composição de ácidos graxos do leite humano maduro de mulheres residentes em área distante da costa litorânea brasileira. MÉTODOS: Amostras de leite materno maduro foram obtidas de 47 mulheres lactantes com idade entre 18 e 35 anos, que tiveram partos a termo e em aleitamento exclusivo ou predominante. A coleta de leite se deu a partir da 5ª semana pós-parto, por meio de ordenha manual. A composição de ácidos graxos do leite foi determinada por cromatografia gasosa. RESULTADOS: Verificou-se que a concentração de eicosapentaenoico (0,08% foi superior ao observado em estudos brasileiros prévios. Entretanto, o teor de docosahexaenoico (0,09% encontrado no leite humano foi um dos menores já verificados no mundo. O teor de ácidos graxos trans (2,05% foi similar ao relatado em estudos nacionais prévios à obrigatoriedade de declaração do teor deste em rótulos de alimentos, sugerindo que esta medida não surtiu efeito na redução de seu teor na dieta habitual das mulheres. CONCLUSÕES: Baixo teor de docosahexaenoico e elevada concentração de ácidos graxos trans foram verificados no leite materno maduro de mulheres residentes em área distante da costa litorânea brasileira.

CARACTERIZAÇÃO QUÍMICA E ATIVIDADE MUTAGÊNICA DO ÓLEO ESSENCIAL DE Lippia alba

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Thammyres de Assis Alves

2017-01-01

Full Text Available Os óleos essenciais são substâncias voláteis que vêm despertando interesse no setor agrícola, devido o grande potencial que possuem no controle de pragas. Assim, objetivo deste trabalho foi determinar a composição química do óleo essencial de folhas de Lippia alba e avaliar o seu potencial mutagênico. Para isso, o óleo essencial foi obtido por hidrodestilação, utilizando um aparelho do tipo Clevenger, seus constituintes químicos foram analisados por meio da cromatografia em fase gasosa com detector de ionização de chama (CG-DIC e de espectrometria de massas (CG-EM. Os compostos majoritários encontrados foram: geranial (29,83%, neral (20,71% e óxido de cariofileno (19,26%. A toxicidade do óleo essencial de L. alba foi avaliado em sementes de Lactuca sativa. O óleo essencial de L. alba inibiu 100% o crescimento radicular das sementes de L. sativa nas concentrações de 0,720% e 0,360% (m v-1. Nas outras concentrações testadas (0,180%, 0,090%, 0,045%, o óleo essencial apresentou um decréscimo no efeito de inibição conforme diminuição de sua concentração. Logo, o óleo essencial de L. alba possui potencial a ser usado como bioherbicida.

Quantitative analysis of semivolatile organic compounds in selected fractions of air sample extracts by GC/MI-IR spectrometry

International Nuclear Information System (INIS)

Childers, J.W.; Wilson, N.K.; Barbour, R.K.

1990-01-01

The authors are currently investigating the capabilities of gas chromatography/matrix isolation infrared (GC/MI-IR) spectrometry for the determination of semivolatile organic compounds (SVOCs) in environmental air sample extracts. Their efforts are focused on the determination of SVOCs such as alkylbenzene positional isomers, which are difficult to separate chromatographically and to distinguish by conventional electron-impact ionization GC/mass spectrometry. They have performed a series of systematic experiments to identify sources of error in quantitative GC/MI-IR analyses. These experiments were designed to distinguish between errors due to instrument design or performance and errors that arise from some characteristic inherent to the GC/MI-IR technique, such as matrix effects. They have investigated repeatability as a function of several aspects of GC/MI IR spectrometry, including sample injection, spectral acquisition, cryogenic disk movement, and matrix deposition. The precision, linearity, dynamic range, and detection limits of a commercial GC/MI-IR system for target SVOCs were determined and compared to those obtained with the system's flame ionization detector. The use of deuterated internal standards in the quantitative GC/MI-IR analysis of selected fractions of ambient air sample extracts will be demonstrated. They will also discuss the current limitations of the technique in quantitative analyses and suggest improvements for future consideration

UV-light-assisted ethanol sensing characteristics of g-C3N4/ZnO composites at room temperature

Science.gov (United States)

Zhai, Jiali; Wang, Tao; Wang, Chuang; Liu, Dechen

2018-05-01

A highly efficient UV-light-assisted room temperature sensor based on g-C3N4/ZnO composites were prepared by an in situ precipitation method. The thermostability, composition, structure, and morphology properties of the as-prepared g-C3N4/ZnO composites were characterized by TGA, XRD, FT-IR, TEM, and XPS, respectively. And then, we studied the ethanol (C2H5OH) sensing performance of the g-C3N4/ZnO composites at the room temperature. Compared with pure ZnO and g-C3N4, the gas sensing activity of g-C3N4/ZnO composites was greatly improved at room temperature, for example, the g-C3N4/ZnO-8% composites showed an obvious response of 121-40 ppm C2H5OH at room temperature, which was 60 times higher than the pure ZnO based on the sensors under the same condition. The great enhancement of the C2H5OH sensing properties of composites can be understood by the efficient separation of photogenerated charge carriers of g-C3N4/ZnO heterogeneous and the UV-light catalytic effect. Finally, a possible mechanism for the gas sensing activity was proposed.

A novel pseudo-complementary PNA G-C base pair

DEFF Research Database (Denmark)

Olsen, Anne G.; Dahl, Otto; Petersen, Asger Bjørn

2011-01-01

Pseudo-complementary oligonucleotide analogues and mimics provide novel opportunities for targeting duplex structures in RNA and DNA. Previously, a pseudo-complementary A-T base pair has been introduced. Towards sequence unrestricted targeting, a pseudo-complementary G-C base pair consisting...

GC-FID coupled with chemometrics for quantitative and chemical fingerprinting analysis of Alpinia oxyphylla oil.

Science.gov (United States)

Miao, Qing; Kong, Weijun; Zhao, Xiangsheng; Yang, Shihai; Yang, Meihua

2015-01-01

Analytical methods for quantitative analysis and chemical fingerprinting of volatile oils from Alpinia oxyphylla were established. The volatile oils were prepared by hydrodistillation, and the yields were between 0.82% and 1.33%. The developed gas chromatography-flame ionization detection (GC-FID) method showed good specificity, linearity, reproducibility, stability and recovery, and could be used satisfactorily for quantitative analysis. The results showed that the volatile oils contained 2.31-77.30 μL/mL p-cymene and 12.38-99.34 mg/mL nootkatone. A GC-FID fingerprinting method was established, and the profiles were analyzed using chemometrics. GC-MS was used to identify the principal compounds in the GC-FID profiles. The profiles of almost all the samples were consistent and stable. The harvesting time and source were major factors that affected the profile, while the volatile oil yield and the nootkatone content had minor secondary effects. Copyright © 2014 Elsevier B.V. All rights reserved.

Desenvolvimento e validação de um método cromatográfico em fase gasosa para análise da 3,4-metilenodioximetanfetamina (ecstasy e outros derivados anfetamínicos em comprimidos Development and validation of a gas chromatography method for determination of ecstasy and amphetamines derivatives in tablets

Directory of Open Access Journals (Sweden)

Marcelo Carvalho Lasmar

2007-06-01

Full Text Available O uso abusivo das anfetaminas e seus derivados vêm aumentando dramaticamente nos últimos anos em diversas regiões do mundo, notando-se especial utilização do Ecstasy. A análise de amostras da droga apreendidas nas ruas evidenciou, além da presença de MDMA (3,4-metilenodioximetanfetamina, componente principal da droga, outras feniletilaminas, como a MDA (3,4-metilenodioxanfetamina e MDEA (metilenodioximetiletilanfetamina este último também conhecido como a droga Eve, ainda pouco difundida no Brasil. O objetivo do presente trabalho foi desenvolver e validar um método analítico confiável, prático e acessível aos laboratórios de toxicologia, de médio e pequeno porte, no Brasil e em países em desenvolvimento, para identificação separada do MDMA, MDA e MDEA. A cromatografia em fase gasosa utilizando-se coluna capilar e detector de ionização de chama foi a técnica escolhida. O método analítico apresentou para os três analitos de interesse, faixa ampla de linearidade (1,0 a 500,0 µg/mL; limites de quantificação de 1,0 µg/mL e coeficientes de variação intra e interensaio inferiores a 9,5%. Os limites de detecção estabelecidos foram 0,7 µg/mL, 0,8 µg/mL e 0,6 µg/mL, respectivamente para o MDMA, MDA e MDEA. O método foi seletivo na presença de epinefrina, cocaína, anfetamina, ácido acetilsalisílico, metanfetamina, ácido dietilbarbitúrico, p-aminobenzoil dietilbarbitúrico, paracetamol e cafeína.The abusive use of the amphetamine derivative ecsyasy in the world come increasing in the last years. Many tablets samples kept on the streets shown the presence not only of the MDMA- 3,4-methylenedioxymethamphetamine, the main drug component but also of the MDA - 3,4- methylenedioxyamphetamine and MDEA - 3,4-methylenedioxymethylethylamphetamine. The present study sought to develop and validate an analytical method for determination of MDMA, MDA and MDEA in tablets to be accessible for the most small or medium

Analysis of organic micropollutants in drinking water using SPME and GC-MS

International Nuclear Information System (INIS)

Guidotti, M.; Ravaioli, G.

1999-01-01

In this work the purpose was to develop accurate and reproducible methods for the qualitative and quantitative analysis of pesticides/herbicides, phthalates, chlorinated solvents, trihalomethanes, polycyclic aromatic hydrocarbons (PAHs) and chlorophenols in drinking waters, using solid-phase micro extraction and GC-MS techniques. The SPME developed by J. Pawliszyn and co-workers, consists of an fused silica fibre, coated with an appropriate absorbent phase, hosted inside the needle of a holder that looks like a GC-syringe; the needle pierces the septum of a sealed vial and the fibre is lowered, by depressing the plunger of the holder, into the liquid (or in the headspace, if that is the case) that contains the analytes of interest. After a set period of time, necessary to reach the partitioning equilibrium, the fibre is retracted inside the needle, the needle is inserted into the GC injector port and the fibre pushed in the heated injector. Here the compounds of interest (that have adsorbed onto the fibre) are thermally desorbed and analysed by GC-MS. After three minutes the fibre is extracted and is ready for a new analysis. The SPME technique has already found many applications in food and environmental analysis. Many of the analytes investigated in this research are listed Italian legislation as possible pollutants of drinking waters and their presence and concentrations require monitoring. The list of compounds included in this work is reported in Table 1

A quantification method for peroxyacetyl nitrate (PAN) using gas chromatography (GC) with a non-radioactive pulsed discharge detector (PDD)

Science.gov (United States)

Zhang, Lei; Jaffe, Daniel A.; Gao, Xin; McClure, Crystal D.

2018-04-01

In this study, we developed a method for continuous PAN measurements by gas chromatography (GC) with a non-radioactive pulsed discharge detector (PDD). Operational parameters were optimized based on the ratio of peak height over baseline noise (P/N ratio). The GC/PDD system was compared with a traditional radioactive electron-capture detector (ECD). In the lab, the method detection limit (MDL) of the new GC/PDD method (9 pptv) was lower than the radioactive GC/ECD method (15 pptv), demonstrating its excellent potential. The MDL of GC/PDD in the field campaign at the Mt. Bachelor Observatory (MBO) was 23 pptv, higher than in the lab. This was caused in part by the decreased slope of the calibration curve resulting from the low air pressure level at MBO. However, the MDL level of GC/PDD at MBO is still low enough for accurate PAN measurements, although special attention should be paid to its application at high-elevation sites. Observations of PAN were conducted at MBO in the summer of 2016 with the GC/PDD system, and provided more evidence of the performance of the system. PAN was found to be highly correlated with CO. The promising performance of GC/PDD which does not require a radioactive source makes it a useful approach for accurate PAN measurements in the field.

Tile-based Fisher ratio analysis of comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC × GC-TOFMS) data using a null distribution approach.

Science.gov (United States)

Parsons, Brendon A; Marney, Luke C; Siegler, W Christopher; Hoggard, Jamin C; Wright, Bob W; Synovec, Robert E

2015-04-07

Comprehensive two-dimensional (2D) gas chromatography coupled with time-of-flight mass spectrometry (GC × GC-TOFMS) is a versatile instrumental platform capable of collecting highly informative, yet highly complex, chemical data for a variety of samples. Fisher-ratio (F-ratio) analysis applied to the supervised comparison of sample classes algorithmically reduces complex GC × GC-TOFMS data sets to find class distinguishing chemical features. F-ratio analysis, using a tile-based algorithm, significantly reduces the adverse effects of chromatographic misalignment and spurious covariance of the detected signal, enhancing the discovery of true positives while simultaneously reducing the likelihood of detecting false positives. Herein, we report a study using tile-based F-ratio analysis whereby four non-native analytes were spiked into diesel fuel at several concentrations ranging from 0 to 100 ppm. Spike level comparisons were performed in two regimes: comparing the spiked samples to the nonspiked fuel matrix and to each other at relative concentration factors of two. Redundant hits were algorithmically removed by refocusing the tiled results onto the original high resolution pixel level data. To objectively limit the tile-based F-ratio results to only features which are statistically likely to be true positives, we developed a combinatorial technique using null class comparisons, called null distribution analysis, by which we determined a statistically defensible F-ratio cutoff for the analysis of the hit list. After applying null distribution analysis, spiked analytes were reliably discovered at ∼1 to ∼10 ppm (∼5 to ∼50 pg using a 200:1 split), depending upon the degree of mass spectral selectivity and 2D chromatographic resolution, with minimal occurrence of false positives. To place the relevance of this work among other methods in this field, results are compared to those for pixel and peak table-based approaches.

Analysis of canine herpesvirus gB, gC and gD expressed by a recombinant vaccinia virus.

Science.gov (United States)

Xuan, X; Kojima, A; Murata, T; Mikami, T; Otsuka, H

1997-01-01

The genes encoding the canine herpesvirus (CHV) glycoprotein B (gB), gC and gD homologues have been reported already. However, products of these genes have not been identified yet. Previously, we have identified three CHV glycoproteins, gp 145/112, gp80 and gp47 using a panel of monoclonal antibodies (MAbs). To determine which CHV glycoprotein corresponds to gB, gC or gD, the putative genes of gB, gC, and gD of CHV were inserted into the thymidine kinase gene of vaccinia virus LC16mO strain under the control of the early-late promoter for the vaccinia virus 7.5-kilodalton polypeptide. We demonstrated here that gp145/112, gp80 and gp47 were the translation products of the CHV gB, gC and gD genes, respectively. The antigenic authenticity of recombinant gB, gC and gD were confirmed by a panel of MAbs specific for each glycoprotein produced in CHV-infected cells. Immunization of mice with these recombinants produced high titers of neutralizing antibodies against CHV. These results suggest that recombinant vaccinia viruses expressing CHV gB, gC and gD may be useful to develop a vaccine to control CHV infection.

GC-MS quantitation of fragrance compounds suspected to cause skin reactions. 1.

Science.gov (United States)

Chaintreau, Alain; Joulain, Daniel; Marin, Christophe; Schmidt, Claus-Oliver; Vey, Matthias

2003-10-22

Recent changes in European legislation require monitoring of 24 volatile compounds in perfumes as they might elicit skin sensitization. This paper reports a GC-MS quantitation procedure for their determination in fragrance concentrates. GC and MS conditions were optimized for a routine use: analysis within 30 min, solvent and internal standard selection, and stock solution stability. Calibration curves were linear in the range of 2-100 mg/L with coefficients of determination in excess of 0.99. The method was tested using real perfumes spiked with known amounts of reference compounds.

Genuineness assessment of mandarin essential oils employing gas chromatography-combustion-isotope ratio MS (GC-C-IRMS).

Science.gov (United States)

Schipilliti, Luisa; Tranchida, Peter Quinto; Sciarrone, Danilo; Russo, Marina; Dugo, Paola; Dugo, Giovanni; Mondello, Luigi

2010-03-01

Cold-pressed mandarin essential oils are products of great economic importance in many parts of the world and are used in perfumery, as well as in food products. Reconstituted mandarin oils are easy to find on the market; useful information on essential oil authenticity, quality, extraction technique, geographic origin and biogenesis can be attained through high-resolution GC of the volatile fraction, or enantioselective GC, using different chiral stationary phases. Stable isotope ratio analysis has gained considerable interest for the unveiling of citrus oil adulteration, detecting small differences in the isotopic carbon composition and providing plenty of information concerning the discrimination among products of different geographical origin and the adulteration of natural essential oils with synthetic or natural compounds. In the present research, the authenticity of several mandarin essential oils was assessed through the employment of GC hyphenated to isotope ratio MS, conventional GC flame ionization detector, enantioselective GC and HPLC. Commercial mandarin oils and industrial natural (declared as such) mandarin essential oils, characterized by different harvest periods and geographic origins, were subjected to analysis. The results attained were compared with those of genuine cold-pressed Italian mandarin oils, obtained during the 2008-2009 harvest season.

Isolamento, caratterizzazione strutturale e valutazione dell'attività biologica di metaboliti secondari di origine vegetale

OpenAIRE

Incollingo, Filomena

2011-01-01

La tematica di ricerca di questo dottorato si inserisce nell’ambito della chimica delle sostanze naturali. In particolare l’attenzione si è soffermata alle piante officinali e alle piante impiegate nella medicina popolare e alla purificazione e all’isolamento dei metaboliti secondari presenti in maggiore quantità attraverso tecniche cromatografiche quali: cromatografia su colonna, cromatografia su strato sottile, HPLC (high pressure liquid chromatography), DCCC (cromatografia liquida in cont...

Caracterização química do óleo essencial de folhas de goiabeira (Psidium guajava L. e seus efeitos no comportamento da lagarta-do-cartucho do milho Spodoptera frugiperda (J. E. Smith, 1797 (Lepidoptera: Noctuidae Essential oil chemical composition from leaves of guava (Psidium guajava L. and its effects on the fall armyworm Spodoptera frugiperda (J. E. Smith, 1797. (Lepidoptera: Noctuidae behavior

Directory of Open Access Journals (Sweden)

Rafaela Karin Lima

2009-01-01

Full Text Available Nesta pesquisa, objetivou-se a obtenção e caracterização do óleo essencial de folhas da goiabeira Psidium guajava cv. Pedro Sato, e seus possíveis efeitos no comportamento da lagarta-do-cartucho do milho Spodoptera frugiperda. O óleo essencial foi obtido pela técnica "arraste a vapor d'água", utilizando-se de um aparelho de Clevenger modificado e submetido, posteriormente, à análise por cromatografia gasosa acoplada a um espectrômetro de massas CG-EM, a fim de investigar sua composição. Para a avaliação dos efeitos do óleo essencial no comportamento das lagartas de 1º ínstar foram testados quatro tratamentos, dois com o óleo essencial na concentração de 0,01% e 0,001%, diluídos em etanol/água 1:1, e duas testemunhas, uma com água e outra com etanol/água 1:1. Os resultados obtidos mostraram que o óleo essencial de folhas de goiabeira apresenta na sua constituição o α-terpineol (0,9%, 1,8-cineol (7,0%, β-cariofileno (7,2% e o óxido de cariofileno (13,8%. Constatou-se, também, que o óleo essencial demonstrou efeito repelente para a lagarta-do-cartucho na concentração de 0,01%.The aim of this research was to obtain and characterize essential oil from leaves of Psidium guajava cv. Pedro Sato, and its possible effects on fall armyworm Spodoptera frugiperda behavior. The essential oil was obtained through steam distillation, by using a modified Clevenger apparatus, and the chemical composition was later analyzed by gas chromatography coupled to mass spectroscopy GC-MS. In order to evaluate the essential oil effect on the armyworm of 1st instars behavior, four treatments were tested; two with oil at 0.01 and 0.001 % in ethanol/water 1:1 concentration; two controls with water and the other with ethanol/water 1:1. The results showed that the above analyzed essential oil constituted of á-terpineole (0.9%, 1,8-cineole (7.0%, â-caryophyllene (7.2% and the caryophyllene oxide (13.8%. It was also found that the essential

Graphene and g-C3N4 based photocatalysts for NOx removal: A review

Science.gov (United States)

Nikokavoura, Aspasia; Trapalis, Christos

2018-02-01

NOx liberated into atmosphere from automobile exhausts and fossil fuel combustion, comprise the major air pollutants. They are responsible for serious environmental problems such as acid rain, ozone accumulation, haze and photochemical smog. Besides they contribute to the deterioration of human health by causing decrease of the lung function and respiratory problems. The application of photocatalytic methods in order to mitigate the presence of NOx in the atmosphere is preferable as they are environmentally friendly, mild and low cost. Therefore, in this review, the photocatalytic activity of g-C3N4 and graphene based composites towards NOx removal was discussed. NOx oxidation to non volatile nitrates on the surface of graphene and g-C3N4 based photocatalysts has attracted much interest during the last years due to their structures with unique features such as large specific surface area, thermal and chemical stability and enhanced visible light utilization. The formation of 2D-2D intimate heterojunctions between graphene or g-C3N4 and other components ensures the enhanced charge transfer, lifetime of electron/hole pairs and thus photocatalytic activity. The increased visible light harvesting also contributes to their usefulness as effective photocatalytic materials. In the present work, the advantages of these novel photocatalysts and the differences/similarities between them were exhaustively highlighted. The role of graphene as catalyst promoter, electron reservoir, support and photosensitizer in its photocatalytic composites was emphasized. The effect of g-C3N4 doping and copolymerization with metals/semiconductors on its photocatalytic activity towards NOx oxidation was thoroughly discussed. Besides, the preparation methods, photocatalytic efficiencies, type of irradiation, utilization of appropriate cocatalysts, and reaction mechanisms during the photocatalytic NOx removal by graphene and g-C3N4 composies, were summarized. It was demonstrated that in the vast

Analysis of stable isotope assisted metabolomics data acquired by GC-MS

International Nuclear Information System (INIS)

Wei, Xiaoli; Shi, Biyun; Koo, Imhoi; Yin, Xinmin; Lorkiewicz, Pawel; Suhail, Hamid; Rattan, Ramandeep; Giri, Shailendra; McClain, Craig J.

2017-01-01

Stable isotope assisted metabolomics (SIAM) measures the abundance levels of metabolites in a particular pathway using stable isotope tracers (e.g., 13 C, 18 O and/or 15 N). We report a method termed signature ion approach for analysis of SIAM data acquired on a GC-MS system equipped with an electron ionization (EI) ion source. The signature ion is a fragment ion in EI mass spectrum of a derivatized metabolite that contains all atoms of the underivatized metabolite, except the hydrogen atoms lost during derivatization. In this approach, GC-MS data of metabolite standards were used to recognize the signature ion from the EI mass spectra acquired from stable isotope labeled samples, and a linear regression model was used to deconvolute the intensity of overlapping isotopologues. A mixture score function was also employed for cross-sample chromatographic peak list alignment to recognize the chromatographic peaks generated by the same metabolite in different samples, by simultaneously evaluating the similarity of retention time and EI mass spectrum of two chromatographic peaks. Analysis of a mixture of 16 13 C-labeled and 16 unlabeled amino acids showed that the signature ion approach accurately identified and quantified all isotopologues. Analysis of polar metabolite extracts from cells respectively fed with uniform 13 C-glucose and 13 C-glutamine further demonstrated that this method can also be used to analyze the complex data acquired from biological samples. - Highlights: • A signature ion approach is developed for analysis of stable isotope GC-MS data. • GC-MS data of compound standards are used for selection of the signature ion. • Linear regression model is used to deconvolute the overlapping isotopologue peaks. • The developed method was tested by known compounds and biological samples.

Synonymous codon bias and functional constraint on GC3-related DNA backbone dynamics in the prokaryotic nucleoid.

Science.gov (United States)

Babbitt, Gregory A; Alawad, Mohammed A; Schulze, Katharina V; Hudson, André O

2014-01-01

While mRNA stability has been demonstrated to control rates of translation, generating both global and local synonymous codon biases in many unicellular organisms, this explanation cannot adequately explain why codon bias strongly tracks neighboring intergene GC content; suggesting that structural dynamics of DNA might also influence codon choice. Because minor groove width is highly governed by 3-base periodicity in GC, the existence of triplet-based codons might imply a functional role for the optimization of local DNA molecular dynamics via GC content at synonymous sites (≈GC3). We confirm a strong association between GC3-related intrinsic DNA flexibility and codon bias across 24 different prokaryotic multiple whole-genome alignments. We develop a novel test of natural selection targeting synonymous sites and demonstrate that GC3-related DNA backbone dynamics have been subject to moderate selective pressure, perhaps contributing to our observation that many genes possess extreme DNA backbone dynamics for their given protein space. This dual function of codons may impose universal functional constraints affecting the evolution of synonymous and non-synonymous sites. We propose that synonymous sites may have evolved as an 'accessory' during an early expansion of a primordial genetic code, allowing for multiplexed protein coding and structural dynamic information within the same molecular context. © The Author(s) 2014. Published by Oxford University Press on behalf of Nucleic Acids Research.

Rapid analysis for 567 pesticides and endocrine disrupters by GC/MS using deconvolution reporting software

Energy Technology Data Exchange (ETDEWEB)

Wylie, P.; Szelewski, M.; Meng, Chin-Kai [Agilent Technologies, Wilmington, DE (United States)

2004-09-15

More than 700 pesticides are approved for use around the world, many of which are suspected endocrine disrupters. Other pesticides, though no longer used, persist in the environment where they bioaccumulate in the flora and fauna. Analytical methods target only a subset of the possible compounds. The analysis of food and environmental samples for pesticides is usually complicated by the presence of co-extracted natural products. Food or tissue extracts can be exceedingly complex matrices that require several stages of sample cleanup prior to analysis. Even then, it can be difficult to detect trace levels of contaminants in the presence of the remaining matrix. For efficiency, multi-residue methods (MRMs) must be used to analyze for most pesticides. Traditionally, these methods have relied upon gas chromatography (GC) with a constellation of element-selective detectors to locate pesticides in the midst of a variable matrix. GC with mass spectral detection (GC/MS) has been widely used for confirmation of hits. Liquid chromatography (LC) has been used for those compounds that are not amenable to GC. Today, more and more pesticide laboratories are relying upon LC with mass spectral detection (LC/MS) and GC/MS as their primary analytical tools. Still, most MRMs are target compound methods that look for a small subset of the possible pesticides. Any compound not on the target list is likely to be missed by these methods. Using the techniques of retention time locking (RTL) and RTL database searching together with spectral deconvolution, a method has been developed to screen for 567 pesticides and suspected endocrine disrupters in a single GC/MS analysis. Spectral deconvolution helps to identify pesticides even when they co-elute with matrix compounds while RTL helps to eliminate false positives and gives greater confidence in the results.

Potential of gas chromatography-orthogonal acceleration time-of-flight mass spectrometry (GC-oaTOFMS) in flavor research.

Science.gov (United States)

Fay, Laurent B; Newton, Anthony; Simian, Hervé; Robert, Fabien; Douce, David; Hancock, Peter; Green, Martin; Blank, Imre

2003-04-23

Gas chromatography-orthogonal acceleration time-of-flight mass spectrometry (GC-oaTOFMS) is an emerging technique offering a straightforward access to a resolving power up to 7000. This paper deals with the use of GC-oaTOFMS to identify the flavor components of a complex seafood flavor extract and to quantify furanones formed in model Maillard reactions. A seafood extract was selected as a representative example for complex food flavors and was previously analyzed using GC-quadrupole MS, leaving several molecules unidentified. GC-oaTOFMS analysis was focused on these unknowns to evaluate its potential in flavor research, particularly for determining exact masses. N-Methyldithiodimethylamine, 6-methyl-5-hepten-2-one, and tetrahydro-2,4-dimethyl-4H-pyrrolo[2,1-d]-1,3,5-dithiazine were successfully identified on the basis of the precise mass determination of their molecular ions and their major fragments. A second set of experiments was performed to test the capabilities of the GC-oaTOFMS for quantification. Calibration curves were found to be linear over a dynamic range of 10(3) for the quantification of furanones. The quantitative data obtained using GC-oaTOFMS confirmed earlier results that the formation of 4-hydroxy-2,5-dimethyl-3(2H)-furanone was favored in the xylose/glycine model reaction and 2(or 5)-ethyl-4-hydroxy-5(or 2)-methyl-3(2H)-furanone in the xylose/alanine model reaction. It was concluded that GC-oaTOFMS may become a powerful analytical tool for the flavor chemist for both identification and quantification purposes, the latter in particular when combined with stable isotope dilution assay.

A Modified GC-MS Analytical Procedure for Separation and Detection of Multiple Classes of Carbohydrates

Directory of Open Access Journals (Sweden)

Yong-Gang Xia

2018-05-01

Full Text Available A modified GC-MS analytical procedure based on trimethylsilyl-dithioacetal (TMSD derivatization has been established for a simultaneous determination of thirteen carbohydrates. Different from previous approaches, the current GC-MS method was featured by a powerful practicability for simultaneous detection of aldoses, uronic acids, ketoses, and amino sugars; simplifying GC-MS chromatograms and producing a single peak for each derivatized sugar, as well as high resolution, sensitivity, and repeatability. An additional liquid-liquid extraction from derivatization mixtures was performed not only to increase the detection sensitivity of amino sugars but also to decrease the by-products of derivatization. Contrarily, three amino sugars were detected at a very low intensity or not detected at all. The effect of time on monosaccharide- mercaptalated reaction was systematically investigated. The effect of trimethylsilylation on the formation of TMSD was also optimized. The established GC-MS based on TMSD derivatization was suitable for complex carbohydrate analysis and has been successfully applied for the detection of free carbohydrates in water extracts of Anemarrhena asphodeloides roots and determination of monosaccharides in Glossy ganoderma polysaccharides.

Magnetically Separable Fe2O3/g-C3N4 Nanocomposites with Cocoon-Like Shape: Magnetic Properties and Photocatalytic Activities

Science.gov (United States)

Yu, Xiaojia; Yang, Xiaoyu; Li, Guang

2018-01-01

We report magnetically separable Fe2O3/g-C3N4 nanocomposites as a photocatalyst under visible-light irradiation in this study. The Fe2O3/g-C3N4 nanocomposites were synthesized through a two-step hydrothermal method. The Fe2O3 with cocoon-like shape was obviously dispersed on the surface of g-C3N4 with porous and layered nanostructure as seen from micrographs of the particles. Furthermore, the magnetic conversion of the samples was studied via vibrating sample magnetometer technology. It was found that the saturated magnetization Ms of the Fe2O3/g-C3N4 nanoparticles obviously decreased in the presence of g-C3N4, and the photocatalytic activity of the samples investigated by degrading Rhodamine B suggested that the Fe2O3/g-C3N4 photocatalyst was prior to the pure Fe2O3 and g-C3N4 samples. In addition, the magnetically separable ability of Fe2O3/g-C3N4 nanocomposites was efficiently exhibited by an external magnet.

Catalytic pyrolysis of Laminaria japonica over nanoporous catalysts using Py-GC/MS

Directory of Open Access Journals (Sweden)

Jeon Jong-Ki

2011-01-01

Full Text Available Abstract The catalytic pyrolysis of Laminaria japonica was carried out over a hierarchical meso-MFI zeolite (Meso-MFI and nanoporous Al-MCM-48 using pyrolysis gas chromatography/mass spectrometry (Py-GC/MS. The effect of the catalyst type on the product distribution and chemical composition of the bio-oil was examined using Py-GC/MS. The Meso-MFI exhibited a higher activity in deoxygenation and aromatization during the catalytic pyrolysis of L. japonica. Meanwhile, the catalytic activity of Al-MCM-48 was lower than that of Meso-MFI due to its weak acidity.

Rendimento, composição química e atividade antilisterial de óleos essenciais de espécies de Cymbopogon Yield, chemical composition and antilisterial activity of essential oils from Cymbopogon species

Directory of Open Access Journals (Sweden)

M.M.M Oliveira

2011-01-01

Full Text Available Objetivou-se determinar o rendimento, a composição química e avaliar a atividade antilisterial dos óleos essenciais de Cymbopogon citratus (DC. Stapf. (capim-limão e Cymbopogon nardus (L. Rendle (capim-citronela, puros e em combinação. A obtenção dos óleos essenciais foi realizada a partir de folhas frescas, empregando-se a técnica de hidrodestilação e utilizando-se aparelho de Clevenger modificado. Os rendimentos foram calculados a partir da massa obtida na extração e da umidade do material vegetal. A análise qualitativa foi realizada por cromatografia em fase gasosa acoplada à espectrometria de massas e a avaliação dos teores dos constituintes químicos por cromatografia em fase gasosa com detector de ionização de chamas. O efeito bacteriostático de diferentes concentrações dos óleos essenciais, puros e em combinação, foi determinado pela técnica de difusão em ágar. As concentrações mínimas inibitórias (CMIs foram utilizadas na determinação do tempo de ação bactericida. O rendimento, em base seca, foi de 1,39% (v/p para o óleo essencial de C. citratus e de 2,27% (v/p para o óleo essencial de C. nardus. Geranial e neral foram os constituintes majoritários do óleo essencial de C. citratus, enquanto, para C. nardus, foram citronelal, geraniol e citronelol. A maioria das concentrações utilizadas mostrou-se efetiva contra Listeria monocytogenes e observaram-se efeitos bactericidas nas CMIs. Óleos essenciais de C. citratus e C. nardus, puros e em combinação, constituem novas alternativas de antibacterianos naturais a serem utilizados no controle de L. monocytogenes na indústria de alimentos.The aim of this study was to determine the yield and the chemical composition of essential oils from Cymbopogon citratus (DC. Stapf. (lemongrass and Cymbopogon nardus (L. Rendle (citronella, and to evaluate their antilisterial activity when pure and combined. The essential oils were obtained from fresh leaves

Gc/ms analysis of coal tar composition produced from coal

African Journals Online (AJOL)

Coal pyrolysis is one of the significant approaches for the comprehensive utilization ... planigraphy-GC/MS; therefore a satisfactory analytical result obtained, which .... Among the aliphatic group of the coal tar, the proportion of alkene is larger ...

Synthesis of MoS_2/g-C_3N_4 nanosheets as 2D heterojunction photocatalysts with enhanced visible light activity

International Nuclear Information System (INIS)

Li, Juan; Liu, Enzhou; Ma, Yongning; Hu, Xiaoyun; Wan, Jun; Sun, Lin; Fan, Jun

2016-01-01

Graphical abstract: TEM image and schematic diagram of photocatalytic mechanism of 2D MoS_2/g-C_3N_4 composites. - Highlights: • g-C_3N_4 nanosheets coupled with MoS_2 nanosheets as 2D heterojunction photocatalysts were synthesized successfully. • The 2D MoS_2/g-C_3N_4 heterojunctions show higher photocatalytic activity than pure g-C_3N_4. • The photocatalytic mechanism of the 2D MoS_2/g-C_3N_4 heterojunction was described. - Abstract: g-C_3N_4 nanosheets coupled with MoS_2 nanosheets as 2D heteroconjuction were prepared via a facile impregnation and calcination method. The structure characterization clearly indicated that MoS_2 nanosheets were successfully horizontal loaded on g-C_3N_4 nanosheets. The investigation indicated that the formation of 2D heterojunction between the g-C_3N_4 nanosheets and MoS_2 nanosheets promoted the charge transfer and enhanced separation efficiency of photoinduced electron–hole pairs. Furthermore, the measurement of photocatalytic activity for the degradation of rhodamine B and methyl orange revealed that the as-prepared 2D MoS_2/g-C_3N_4 heterojunction exhibited the significantly enhanced photocatalytic activity and considerable stability under visible light irradiation. The 2D MoS_2/g-C_3N_4 heterojunction prepared with 3 wt% of MoS_2 exhibited the optimal photodegradable efficiency. The present work shows that the formation of 2D heterojunction should be a good strategy to design efficient photocatalysts.

Improving g-C3N4 photocatalysis for NOx removal by Ag nanoparticles decoration

International Nuclear Information System (INIS)

Sun, Yanjuan; Xiong, Ting; Ni, Zilin; Liu, Jie; Dong, Fan; Zhang, Wei; Ho, Wing-Kei

2015-01-01

Graphical abstract: Ag/g-C 3 N 4 nanocomposites were prepared via a facile method for enhanced photocatalytic NO x removal due to surface plasmon resonance of Ag. - Highlights: • The Ag/g-C 3 N 4 nanocomposites were prepared using urea as the precursor. • The Ag/g-C 3 N 4 nanocomposites were applied in removal of NO x in air. • The Ag nanoparticles enhanced the photocatalytic activity of g-C 3 N 4 . • The surface plasmon resonance of Ag played a key role in photocatalysis. - Abstract: In order to overcome the intrinsic drawback of pristine g-C 3 N 4 , we prepared g-C 3 N 4 nanosheets with enhanced photocatalytic performance by Ag nanoparticles decoration using urea as the precursor. It was revealed that the monodispersed Ag nanoparticles were deposited on the surface of g-C 3 N 4 nanosheets. The Ag/g-C 3 N 4 nanocomposites were applied in removal of NO x in air under visible light irradiation. The results showed that the decoration of Ag nanoparticles not only enhanced the photocatalytic activity of g-C 3 N 4 nanosheets, but also benefited the oxidation of NO to final products. The increased visible light absorption arising from the surface plasmon resonance of Ag and improved separation and transfer of photoinduced carriers over Ag/g-C 3 N 4 composites were demonstrated by the UV–vis diffuse reflectance spectra and photoluminescence spectra, respectively. It was therefore proposed that the enhanced photocatalytic activity of Ag/g-C 3 N 4 composites could be attributed to the extended light response range and enhanced charge separation due to the introduction of Ag nanoparticles.

Interface engineered construction of porous g-C3N4/TiO2 heterostructure for enhanced photocatalysis of organic pollutants

Science.gov (United States)

Li, Ya-Nan; Chen, Zhao-Yang; Wang, Min-Qiang; Zhang, Long-zhen; Bao, Shu-Juan

2018-05-01

A porous g-C3N4/TiO2 with hierarchical heterostructure has been successfully fabricated through a in situ assembling of small needle-like TiO2 on the surface of ultrathin g-C3N4 sheets. The ultrathin g-C3N4 sheets with carbon vacancies and rich hydroxyl groups were found to facilitate the nucleation and in situ growth of TiO2 and also to modulate the surface chemical activity of the g-C3N4/TiO2 hierarchical heterostructure. The as-designed photocatalytic heterojunction degraded Acid Orange with 82% efficiency after 10 min under simulated solar light, and possessed excellent cycle stability. Relative physical characterizations and photochemical experiments reveal that engineering the interface/surface of g-C3N4 plays a vital role in effectively constructing heterostructures of g-C3N4/TiO2, thus realizing efficient photoinduced electron-hole separation during photocatalytic process.

Exponential decay of GC content detected by strand-symmetric substitution rates influences the evolution of isochore structure.

Science.gov (United States)

Karro, J E; Peifer, M; Hardison, R C; Kollmann, M; von Grünberg, H H

2008-02-01

The distribution of guanine and cytosine nucleotides throughout a genome, or the GC content, is associated with numerous features in mammals; understanding the pattern and evolutionary history of GC content is crucial to our efforts to annotate the genome. The local GC content is decaying toward an equilibrium point, but the causes and rates of this decay, as well as the value of the equilibrium point, remain topics of debate. By comparing the results of 2 methods for estimating local substitution rates, we identify 620 Mb of the human genome in which the rates of the various types of nucleotide substitutions are the same on both strands. These strand-symmetric regions show an exponential decay of local GC content at a pace determined by local substitution rates. DNA segments subjected to higher rates experience disproportionately accelerated decay and are AT rich, whereas segments subjected to lower rates decay more slowly and are GC rich. Although we are unable to draw any conclusions about causal factors, the results support the hypothesis proposed by Khelifi A, Meunier J, Duret L, and Mouchiroud D (2006. GC content evolution of the human and mouse genomes: insights from the study of processed pseudogenes in regions of different recombination rates. J Mol Evol. 62:745-752.) that the isochore structure has been reshaped over time. If rate variation were a determining factor, then the current isochore structure of mammalian genomes could result from the local differences in substitution rates. We predict that under current conditions strand-symmetric portions of the human genome will stabilize at an average GC content of 30% (considerably less than the current 42%), thus confirming that the human genome has not yet reached equilibrium.

Mechanistic Insight into Bunyavirus-Induced Membrane Fusion from Structure-Function Analyses of the Hantavirus Envelope Glycoprotein Gc.

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Pablo Guardado-Calvo

2016-10-01

Full Text Available Hantaviruses are zoonotic viruses transmitted to humans by persistently infected rodents, giving rise to serious outbreaks of hemorrhagic fever with renal syndrome (HFRS or of hantavirus pulmonary syndrome (HPS, depending on the virus, which are associated with high case fatality rates. There is only limited knowledge about the organization of the viral particles and in particular, about the hantavirus membrane fusion glycoprotein Gc, the function of which is essential for virus entry. We describe here the X-ray structures of Gc from Hantaan virus, the type species hantavirus and responsible for HFRS, both in its neutral pH, monomeric pre-fusion conformation, and in its acidic pH, trimeric post-fusion form. The structures confirm the prediction that Gc is a class II fusion protein, containing the characteristic β-sheet rich domains termed I, II and III as initially identified in the fusion proteins of arboviruses such as alpha- and flaviviruses. The structures also show a number of features of Gc that are distinct from arbovirus class II proteins. In particular, hantavirus Gc inserts residues from three different loops into the target membrane to drive fusion, as confirmed functionally by structure-guided mutagenesis on the HPS-inducing Andes virus, instead of having a single "fusion loop". We further show that the membrane interacting region of Gc becomes structured only at acidic pH via a set of polar and electrostatic interactions. Furthermore, the structure reveals that hantavirus Gc has an additional N-terminal "tail" that is crucial in stabilizing the post-fusion trimer, accompanying the swapping of domain III in the quaternary arrangement of the trimer as compared to the standard class II fusion proteins. The mechanistic understandings derived from these data are likely to provide a unique handle for devising treatments against these human pathogens.

Effects of oxaliplatin and oleic acid Gc-protein-derived macrophage-activating factor on murine and human microglia.

Science.gov (United States)

Branca, Jacopo J V; Morucci, Gabriele; Malentacchi, Francesca; Gelmini, Stefania; Ruggiero, Marco; Pacini, Stefania

2015-09-01

The biological properties and characteristics of microglia in rodents have been widely described, but little is known about these features in human microglia. Several murine microglial cell lines are used to investigate neurodegenerative and neuroinflammatory conditions; however, the extrapolation of the results to human conditions is frequently met with criticism because of the possibility of species-specific differences. This study compares the effects of oxaliplatin and of oleic acid Gc-protein-derived macrophage-activating factor (OA-GcMAF) on two microglial cell lines, murine BV-2 cells and human C13NJ cells. Cell viability, cAMP levels, microglial activation, and vascular endothelial growth factor (VEGF) expression were evaluated. Our data demonstrate that oxaliplatin induced a significant decrease in cell viability in BV-2 and in C13NJ cells and that this effect was not reversed with OA-GcMAF treatment. The signal transduction pathway involving cAMP/VEGF was activated after treatment with oxaliplatin and/or OA-GcMAF in both cell lines. OA-GcMAF induced a significant increase in microglia activation, as evidenced by the expression of the B7-2 protein, in BV-2 as well as in C13NJ cells that was not associated with a concomitant increase in cell number. Furthermore, the effects of oxaliplatin and OA-GcMAF on coculture morphology and apoptosis were evaluated. Oxaliplatin-induced cell damage and apoptosis were nearly completely reversed by OA-GcMAF treatment in both BV-2/SH-SY5Y and C13NJ/SH-SY5Y cocultures. Our data show that murine and human microglia share common signal transduction pathways and activation mechanisms, suggesting that the murine BV-2 cell line may represent an excellent model for studying human microglia. © 2015 Wiley Periodicals, Inc.

Using systematic and comparative GC/MS and GC/FID data to identify the source of an unknown oil on contaminated birds

International Nuclear Information System (INIS)

Wang, Z.; Fingas, M.; Landriault, M.; Sigouin, L.; Feng, Y.

1996-01-01

A method to identify and differentiate spilled oil and petroleum products was developed. In January 1996, four birds covered with an unknown oil were found near Larchipel-de-Mingan National Park in Quebec. Environment Canada wanted to know if the oil came from a leak in a barge which was grounded on Anticosti Island. To do so, it was necessary to determine the nature of the oil, the type of petroleum hydrocarbons, the age, the weathering and degradation extent of the spilled oil, and changes in oil character since the occurrence of any possible spill. The analytical approach to determine the source of the unknown oil was described. The analysis of individual aliphatic, aromatic, and biomarker hydrocarbons were made with the use of gas chromatography/mass spectroscopy (GC/MS), and gas chromatography/flame ionization detector (GC/FID). Pattern recognition plot analysis was also used in determining the source of the oil. It was concluded that the residual oil on the birds was not from the suspected barge oil, and was most probably old, highly weathered, somewhat biodegraded bunker type oil. 23 refs., 5 tabs., 7 figs

EVALUACIÓN DE PLAGUICIDAS 0RGAN0CL0RAD0S POR HS-SPME - GC/ECD EN LECHE PASTEURIZADA COMERCIALIZADA EN LA CIUDAD DE CARTAGENA (COLOMBIA A AVALIAQÁO DOS PESTICIDAS ORGANOCLORADOS POR HS-SPME - GC/ECD EM LEITE PASTEURIZADO COMERCIALIZADAS NA CIDADE CARTAGENA (COLOMBIA EVALUATION OF PESTICIDES BY HS-SPME ORGANOCHLORINE - GC / ECD IN PASTEURIZED MILK MARKETED IN THE CITY CARTAGENA (COLOMBIA

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DENILES DEL CARMEN DE ARCO R

2011-12-01

Full Text Available Los plaguicidas han sido utilizados en todo el mundo desde mediados del siglo XX, en campañas de Salud Pública y en prácticas agrícolas. Los Plaguicidas Organoclorados (POCs presentan mayor impacto sobre el ambiente porque no son biodegradables, son lipofílicos, tienen gran movilidad por todo el planeta y gran tendencia a la bioacumulación, através de la cadena trófica. Con el objetivo de identificar y cuantificar plaguicidas organoclorados en leche entera pasteurizada de dos marcas (A y B, que se comercializan en la ciudad de Cartagena de Indias, se realizó la presente investigación, utilizando Microextracción en Fase Sólida en Espacio de Cabeza y Cromatografía de Gases con Detector de Captura de Electrones (HS-SPME-GC/ECD. Fueron analizadas 36 muestras (n=36, 18 de cada marca. El 100% de las muestras (n=36 resultaron positivas para el plaguicida lindano (γ-HCH, superando el Límite Máximo Residual (LMR de 0,01 mg/kg, establecido por la Food and Agriculture Organization y la Organización Mundial de la Salud (FAO/OMS. Las concentraciones promedio de lindano obtenidas para la marca A fueron de 0,042 mg/kg ± 0,003 y 0,062 ± 0,0016 mg/kg (base grasa para la marca B, no superando la Ingesta Diaria Admisible (IDA de 0,001 mg/kg de peso corporal.Os pesticidas têm sido usados em todo o mundo desde meados do século XX, as campanhas de saúde pública e práticas agrícolas. Os inseticidas organoclorados (AP têm maior impacto sobre o meio ambiente porque não são biodegradáveis, são lipofílicas, têm grande mobilidade ao redor do mundo e maior tendencia para a bioacumulação através da cadeia alimentar. A fim de identificar e quantificar pesticidas organoclorados em leite integral, duas marcas (A e B, comercializada na cidade de Cartagena das Índias, a presente investigação foi realizada por cromatografia em Fase Sólida, Microextração Headspace Gás com Detector de Captura de Elétrons(HS-SPME-GC/ECD. 36 amostras foram

Rapid Quantification of N-Methyl-2-pyrrolidone in Polymer Matrices by Thermal Desorption-GC/MS.

Science.gov (United States)

Kim, Young-Min; Kim, Jae Woo; Moon, Hye Mi; Lee, Min-Jin; Hosaka, Akihiko; Watanabe, Atsushi; Teramae, Norio; Park, Young-Kwon; Myung, Seung-Woon

2017-01-01

Analysis of a residual solvent in polymeric materials has become an important issue due to the increased regulations and standards for its use. N-Methyl-2-pyrrolidone (NMP) is a solvent widely used in many industries and restricted as one of the chemicals under EU REACH regulations due to its potential harmful effects. In this study, thermal desorption-gas chromatography/mass spectrometry (TD-GC/MS) is applied for the quantitative analysis of NMP with the use of a polymer-coated sample cup. By using the polymer-coated sample cup, the vaporization of NMP was prevented during waiting time before TD-GC/MS analysis. The calibration curve for the TD method showed good linearity (correlation coefficient, r 2 = 0.9998) and precision values (below 5.3% RSD). NMP recovery rates in different polymer matrices (PS, PMMA and PVC) were in the range of 98.8 to 106.6% with RSD values below 5.0%. The quantification result (600 mg NMP/kg PVC) for the blind NMP carrying sample in a PVC matrix by TD-GC/MS was higher than that (532 mg NMP/kg PVC) by solvent extraction-GC/MS method.

Monoterpene separation by coupling proton transfer reaction time-of-flight mass spectrometry with fastGC.

Science.gov (United States)

Materić, Dušan; Lanza, Matteo; Sulzer, Philipp; Herbig, Jens; Bruhn, Dan; Turner, Claire; Mason, Nigel; Gauci, Vincent

2015-10-01

Proton transfer reaction mass spectrometry (PTR-MS) is a well-established technique for real-time analysis of volatile organic compounds (VOCs). Although it is extremely sensitive (with sensitivities of up to 4500 cps/ppbv, limits of detection monoterpenes, which belong to the most important plant VOCs, still cannot be distinguished so more traditional technologies, such as gas chromatography mass spectrometry (GC-MS), have to be utilised. GC-MS is very time consuming (up to 1 h) and cannot be used for real-time analysis. Here, we introduce a sensitive, near-to-real-time method for plant monoterpene research-PTR-MS coupled with fastGC. We successfully separated and identified six of the most abundant monoterpenes in plant studies (α- and β-pinenes, limonene, 3-carene, camphene and myrcene) in less than 80 s, using both standards and conifer branch enclosures (Norway spruce, Scots pine and black pine). Five monoterpenes usually present in Norway spruce samples with a high abundance were separated even when the compound concentrations were diluted to 20 ppbv. Thus, fastGC-PTR-ToF-MS was shown to be an adequate one-instrument solution for plant monoterpene research.

An evaluation of microcult g.c. in venereal disease clinics

DEFF Research Database (Denmark)

Nielsen, A O; Andersen, Klaus Ejner

1977-01-01

Microcult G.C. is a kit for cultivation and identification of Neisseria gonorrhoeae. ue of this kit was compared with the cultivation and identification methods of the Neisseria Department, Statens Seruminstitut, Copenhagen (WHO collaborating center for reference and research in gonococci). The i...

SPME GC/MS determination of organochlorine pesticides in water samples

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Yerbolat Sailaukhanuly

2013-05-01

Full Text Available Headspace solid phase microextraction (HS-SPME in combination with gas chromatography and mass-spectrometry (GC/MS was studied for analysis of water samples. The organochlorine pesticides (OCPs, p,p'-DDT, p,p'-DDD, and p,p'-DDE were collected and analyzed by GC/MS. To select of effective fiber coatings four types of SPME fibers were examined and compared. The parameters effecting the efficiency of HS-SPME such as extraction and pre-incubation time and extraction temperature, effect of solvent nature, ionic strength were studied to obtain optimal parameters. The method was developed using spiked water samples in a concentration range  10 - 500 ng/L. The calibration curve was linear over the studied concentration range with r≥0.9925. The detection limits varied from 1.57 to 2.08 ng/L. An authentic water samples from contaminated lake with OCPs were analyzed by developed method.

Determination of Propofol by GC/MS and Fast GC/MS-TOF in Two Cases of Poisoning.

Science.gov (United States)

Procaccianti, Paolo; Farè, Fiorenza; Argo, Antonella; Casagni, Eleonora; Arnoldi, Sebastiano; Facheris, Sara; Visconti, Giacomo Luca; Roda, Gabriella; Gambaro, Veniero

2017-11-01

Two cases of suspected acute and lethal intoxication caused by propofol were delivered by the judicial authority to the Department of Sciences for Health Promotion and Mother-Child Care in Palermo, Sicily. In the first case a female nurse was found in a hotel room, where she lived with her mother; four 10 mg/mL vials and two 20 mg/mL vials of propofol were found near the decedent along with syringes and needles. In the second case a male nurse was found in the operating room of a hospital, along with a used syringe. In both cases a preliminary systematic and toxicological analysis indicated the presence of propofol in the blood and urine. As a result, a method for the quantitative determination of propofol in biological fluids was optimized and validated using a liquid-liquid extraction protocol followed by GC/MS and fast GC/MS-TOF. In the first case, the concentration of propofol in blood was determined to be 8.1 μg/mL while the concentration of propofol in the second case was calculated at 1.2 μg/mL. Additionally, the tissue distribution of propofol was determined for both cases. Brain and liver concentrations of propofol were, respectively, 31.1 and 52.2 μg/g in Case 1 and 4.7 and 49.1 μg/g in Case 2. Data emerging from the autopsy findings, histopathological exams as well as the toxicological results aided in establishing that the deaths were due to poisoning, however, the manner of death in each were different: homicide in Case 1 and suicide in Case 2. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

A scanning point source for quality control of FOV uniformity in GC-PET imaging

International Nuclear Information System (INIS)

Bergmann, H.; Minear, G.; Dobrozemsky, G.; Nowotny, R.; Koenig, B.

2002-01-01

Aim: PET imaging with coincidence cameras (GC-PET) requires additional quality control procedures to check the function of coincidence circuitry and detector zoning. In particular, the uniformity response over the field of view needs special attention since it is known that coincidence counting mode may suffer from non-uniformity effects not present in single photon mode. Materials and methods: An inexpensive linear scanner with a stepper motor and a digital interface to a PC with software allowing versatile scanning modes was developed. The scanner is used with a source holder containing a Sodium-22 point source. While moving the source along the axis of rotation of the GC-PET system, a tomographic acquisition takes place. The scan covers the full axial field of view of the 2-D or 3-D scatter frame. Depending on the acquisition software, point source scanning takes place continuously while only one projection is acquired or is done in step-and-shoot mode with the number of positions equal to the number of gantry steps. Special software was developed to analyse the resulting list mode acquisition files and to produce an image of the recorded coincidence events of each head. Results: Uniformity images of coincidence events were obtained after further correction for systematic sensitivity variations caused by acquisition geometry. The resulting images are analysed visually and by calculating NEMA uniformity indices as for a planar flood field. The method has been applied successfully to two different brands of GC-PET capable gamma cameras. Conclusion: Uniformity of GC-PET can be tested quickly and accurately with a routine QC procedure, using a Sodium-22 scanning point source and an inexpensive mechanical scanning device. The method can be used for both 2-D and 3-D acquisition modes and fills an important gap in the quality control system for GC-PET

Supercritical fluid chromatography-A Hybrid of GC and LC

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Neha Sethi

2010-01-01

Full Text Available High performance specifications and unique functionality of chromatographic techniques is a demand of pharmaceutical industry and research. This leads to the origin of Supercritical Fluid Chromatography (SFC. It is a rapidly expanding analytical technique. The main feature that differentiates SFC from other chromatographic techniques is the replacement of either the liquid or gas mobile phase with a supercritical fluid mobile phase. It is considered a hybrid of GC and LC technique. High diffusion coefficient and low viscosity of supercritical fluids is responsible for high speed analysis, high efficiency and high sensitivity. Low mobile-phase flow rate, density programming and compatability with GC and LC detectors make SFC a versatile chromatographic technique in analytical re-search and development. It has a unique characteristic of analyzing thermo labile or non-volatile substances. This review highlights the role of supercritical fluid chromatography in the separation of polymers, thermally labile pesticides, fatty acids, metal chelates and organometallic compounds, chiral and achiral molecules, identification and analysis of polar samples, explosives, drugs of abuse and application of SFC in forensic science (fingerprint-ing.

Construction of g-C_3N_4/Al_2O_3 hybrids via in-situ acidification and exfoliation with enhanced photocatalytic activity

International Nuclear Information System (INIS)

Wang, Xiao-jing; Liu, Chao; Li, Xu-li; Li, Fa-tang; Li, Yu-pei; Zhao, Jun; Liu, Rui-hong

2017-01-01

Highlights: • Ultrathin g-C_3N_4/Al_2O_3 hybrids are prepared via in-situ reaction. • The structure modification role of in-situ formed HNO_3 for g-C_3N_4 is found. • The ultrathin g-C_3N_4 nanosheets are formed by the acidified melamine and Al(OH)_3. • In-situ calcination of melamine and Al(OH)_3 benefits the contact of C_3N_4 and Al_2O_3. • The activity of g-C_3N_4/Al_2O_3 is 16.6 times that of pristine g-C_3N_4 in degrading RhB. - Abstract: Homogeneous ultrathin g-C_3N_4 nanosheets/Al_2O_3 heterojunctions are synthesized using melamine and Al(NO_3)_3 via in-situ reaction and the following thermal polymerization approach. The in-situ reaction between melamine and Al(NO_3)_3 results in the existence of HNO_3-acidified melamine and Al(OH)_3 aggregates via the hydrolysis of Al(NO_3)_3. After thermal polymerization, the aggregates are converted to g-C_3N_4/Al_2O_3 composites. The thermal polymerization of acidified melamine and the support effect of aluminum hydroxide for g-C_3N_4 during the calcination process lead to highly dispersed amrophous Al_2O_3 on ultrathin g-C_3N_4 nanosheets, which is beneficial for the separation of photogenerated electron-hole pairs in the heterojunction. The degradation rate for Rhodamine B (RhB) over the most activie sample is 16.6 times than that of pristine g-C_3N_4 under visible light irradiation, which can be attributed to the high specific surface area, highly dispersion of amorphous Al_2O_3 on ultrathin g-C_3N_4 nanosheet, and the effective electrons transfer from g-C_3N_4 to the amorphous Al_2O_3.

Enhanced visible-light photocatalytic decomposition of 2,4-dichlorophenoxyacetic acid over ZnIn_2S_4/g-C_3N_4 photocatalyst

International Nuclear Information System (INIS)

Qiu, Pengxiang; Yao, Jinhua; Chen, Huan; Jiang, Fang; Xie, Xianchuan

2016-01-01

Highlights: • A novel flower-on-sheet ZnIn_2S_4/g-C_3N_4 nanocomposite was synthesized. • ZnIn_2S_4/g-C_3N_4 showed high visible light catalytic activity for 2,4-D degradation. • The photocatalytic degradation pathway of 2,4-D was investigated. - Abstract: ZnIn_2S_4/g-C_3N_4 heterojunction photocatalyst was successfully synthesized via a simple hydrothermal method and applied to visible-light photocatalytic decomposition of 2,4-dichlorophenoxyacetic acid (2,4-D) from aqueous phase. The flower-like ZnIn_2S_4 particles were dispersed on the surface of g-C_3N_4 nanosheets in the ZnIn_2S_4/g-C_3N_4 composite. The composite showed higher separation rate of electron-hole pairs as compared to ZnIn_2S_4 and g-C_3N_4. Consequently, the ZnIn_2S_4/g-C_3N_4 composite exhibited enhanced visible light photocatalytic decomposition efficiency of 2,4-D, within 20% ZnIn_2S_4/g-C_3N_4 composite owning the highest photocatalytic efficiency and initial rate. The initial rates of 2,4-D degradation on g-C_3N_4, ZnIn_2S_4, and 20% ZnIn_2S_4/g-C_3N_4 were 1.23, 0.57 and 3.69 mmol/(g_c_a_t h), respectively. The h"+ and O_2"·"− were found to be the dominant active species for 2,4-D decomposition. The photocatalytic degradation pathways of 2,4-D by ZnIn_2S_4/g-C_3N_4 under visible light irradiation were explored. The ZnIn_2S_4/g-C_3N_4 composite displayed high photostability in recycling tests, reflecting its promising potential as an effective visible light photocatalyst for 2,4-D treatment.

Effect of paricalcitol and GcMAF on angiogenesis and human peripheral blood mononuclear cell proliferation and signaling.

Science.gov (United States)

Pacini, Stefania; Morucci, Gabriele; Punzi, Tiziana; Gulisano, Massimo; Ruggiero, Marco; Amato, Marcello; Aterini, Stefano

2012-01-01

In addition to its role in calcium homeostasis and bone mineralization, vitamin D is involved in immune defence, cardiovascular function, inflammation and angiogenesis, and these pleiotropic effects are of interested in the treatment of chronic kidney disease. Here we investigated the effects of paricalcitol, a nonhypercalcemic vitamin D analogue, on human peripheral blood mononuclear cell proliferation and signaling, and on angiogenesis. These effects were compared with those of a known inhibitor of angiogenesis pertaining to the vitamin D axis, the vitamin D-binding protein-derived Gc-macrophage activating factor (GcMAF). Since the effects of vitamin D receptor agonists are associated with polymorphisms of the gene coding for the receptor, we measured the effects of both compounds on mononuclear cells harvested from subjects harboring different BsmI polymorphisms. Paricalcitol inhibited mononuclear cell viability with the bb genotype showing the highest effect. GcMAF, on the contrary, stimulated cell proliferation, with the bb genotype showing the highest stimulatory effect. Both compounds stimulated 3'-5'-cyclic adenosine monophosphate formation in mononuclear cells with the highest effect on the bb genotype. Paricalcitol and GcMAF inhibited the angiogenesis induced by proinflammatory prostaglandin E1. Polymorphisms of the vitamin D receptor gene, known to be associated with the highest responses to vitamin D receptor agonists, are also associated with the highest responses to GcMAF. These results highlight the role of the vitamin D axis in chronic kidney disease, an axis which includes vitamin D, its receptor and vitamin D-binding protein-derived GcMAF.

Identification of irradiated chicken by GC/MS determination of radiation-induced volatile from the lipids

International Nuclear Information System (INIS)

Spiegelberg, A.; Helde, L.; Boegl, K.W.

1991-01-01

For the detection of irradiated meat, a procedure is reported which involves high vacuum distillation of the separated fat and analysis by gas chromatography/mass spectrometry (GC/MS) of hydrocarbons. This equipment was well sulted for the method described in this report for the detection of irradiated chicken by separating the volatiles from the lipid fraction and further identification by GC/MS. The results are based on investigations of 7 types of whole frozen chicken 2 types of frozen chicken thigh, and 1 type of frozen chicken. The results demonstrate that irradiated chicken can be monitored by cold-finger high-vacuum distillation-and further GC/MS-Identification of the major hydrocarbons formed during the radiolysis of lipids. The detection of these compounds was simplified by Single Ion Monitoring. 4 figs., 20 refs

Forensic Characterization of Liquor Samples by Gas Chromatography-Mass Spectrometry (GC-MS – A Review

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Praveen K. Yadav

2017-12-01

Full Text Available Alcohol is a subject of forensic research across the world. The forensic characterization of alcoholic beverages is required in cases of death and crimes due to alcohol consumption. In many cases, determining the geographic origin becomes a very important part of the investigation. Therefore, it is important to develop more sensitive methods for the analysis of alcoholic beverages. In this review, an attempt has been made to summarize the work accomplished so far in the field of analysis and detection of alcoholic beverages. In this review, various sample preparation techniques for GC-MS analysis of alcoholic beverages have been discussed along with its applications. GC-MS based analysis is less time consuming, more sensitive and more accurate.   Keywords: Forensic Sciences, Alcoholic beverages, Mortality, Analysis, GC-MS

Gc, gc-ms analysis of lipophilic fractions of aerial parts of fagonia indica burm.f. showing growth inhibitory effect on ht 29 colorectal cancer cells

International Nuclear Information System (INIS)

Farheen, R.; Mahmood, I.

2016-01-01

Fagonia indica Burm.f. is a small genus of herbs and under shrubs. The plant contains potentially active substances and has been used traditionally for the treatment of many illnesses including cancer. Many polar compounds have been reported from this plant but its non-polar constituents have only been rarely studied. In the present studies these constituents of aerial parts of Fagonia indica Burm.f. and its sub fractions showing growth inhibitory effect on HT 29 colorectal cancer cells were analyzed using flame ionization detector (GC-FID) and GC-EIMS analysis. The present studies exhibited the presence of free fatty acids and their esters along with structurally diverse constituents including triterpene, heterocyclic organic compound, aromatics, hydrocarbons, alcohols, lactone and sterols which may be responsible for this activity. The results suggest that the non-polar constituents of F. indica bear a potential of further studies. (author)

Bacteriophage GC1, a Novel Tectivirus Infecting Gluconobacter Cerinus, an Acetic Acid Bacterium Associated with Wine-Making

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Cécile Philippe

2018-01-01

Full Text Available The Gluconobacter phage GC1 is a novel member of the Tectiviridae family isolated from a juice sample collected during dry white wine making. The bacteriophage infects Gluconobacter cerinus, an acetic acid bacterium which represents a spoilage microorganism during wine making, mainly because it is able to produce ethyl alcohol and transform it into acetic acid. Transmission electron microscopy revealed tail-less icosahedral particles with a diameter of ~78 nm. The linear double-stranded DNA genome of GC1 (16,523 base pairs contains terminal inverted repeats and carries 36 open reading frames, only a handful of which could be functionally annotated. These encode for the key proteins involved in DNA replication (protein-primed family B DNA polymerase as well as in virion structure and assembly (major capsid protein, genome packaging ATPase (adenosine triphosphatase and several minor capsid proteins. GC1 is the first tectivirus infecting an alphaproteobacterial host and is thus far the only temperate tectivirus of gram-negative bacteria. Based on distinctive sequence and life-style features, we propose that GC1 represents a new genus within the Tectiviridae, which we tentatively named “Gammatectivirus”. Furthermore, GC1 helps to bridge the gap in the sequence space between alphatectiviruses and betatectiviruses.

An oxygen-vacancy-rich Z-scheme g-C3N4/Pd/TiO2 heterostructure for enhanced visible light photocatalytic performance

Science.gov (United States)

Guo, Yanru; Xiao, Limin; Zhang, Min; Li, Qiuye; Yang, Jianjun

2018-05-01

An oxygen-vacancy-rich Z-scheme g-C3N4/Pd/TiO2 ternary nanocomposite was fabricated using nanotubular titanic acid as precursors via a simple photo-deposition of Pd nanoparticles and calcination process. The prepared nanocomposites were investigated by X-ray diffraction, transmission electron microscopy, X-ray photoelectron spectroscopy, and UV-visible diffuse reflectance spectroscopy, respectively. For g-C3N4/TiO2 binary nanocomposites, at the optimal content of g-C3N4 (2%), the apparent photocatalytic activity of 2%g-C3N4/TiO2 was 9 times higher than that of pure TiO2 under visible-light illumination. After deposition of Pd (1 wt%) at the contact interface between g-C3N4 and TiO2, the 2%g-C3N4/Pd/TiO2 ternary nanocomposites demonstrated the highest visible-light-driven photocatalytic activity for the degradation of gaseous propylene, which was 16- and 2-fold higher activities than pure TiO2 and 2%g-C3N4/TiO2, respectively. The mechanism for the enhanced photocatalytic performance of the g-C3N4/Pd/TiO2 photo-catalyst is proposed to be based on the efficient separation of photo-generated electron-hole pairs through Z-scheme system, in which uniform dispersity of Pd nanoparticles at contact interface between g-C3N4 and TiO2 and oxygen vacancies promote charge separation.

SPE-GC/FTD determination of N-methyl-2-pyrrolidone and its metabolites in urine.

Science.gov (United States)

Kubota, Ryuichi; Endo, Yoko; Takeuchi, Akito; Inoue, Yoshinori; Ogata, Hiroko; Ogawa, Masanori; Nakagawa, Tomoo; Onda, Nobuhiko; Endo, Ginji

2007-07-01

An analytical method using a combination of solid-phase extraction (SPE) and gas chromatography with a flame thermionic detector (GC/FTD) was developed for determination of N-methyl-2-pyrrolidone (NMP), N-methylsuccinimide (MSI), and 2-hydroxy-N-methylsuccinimide (2-HMSI) in human urine. The SPE cartridge of poly(divinylbenzene/hydroxymethacrylate) used was directly loaded with urine sample, followed by elution with methyl isobutyl ketone (MIBK) and subsequent centrifugation, and the supernatant was injected into the capillary GC using a DB1701. This method allowed efficient separation of NMP, MSI, and 2-HMSI, which were nearly free of interference by other GC peaks arising from urine. Recoveries of NMP, MSI, and 2-HMSI from the SPE cartridge were about 98, 101, and 67%, respectively, with limits of detection of 0.04, 0.02, and 0.06 mg/L, respectively, which met the regulatory requirements. The present method was used for assay in biological monitoring of workers exposed to NMP in their occupational environment.

Surface modification of TiO2 with g-C3N4 for enhanced UV and visible photocatalytic activity

International Nuclear Information System (INIS)

Lei, Juying; Chen, Ying; Shen, Fan; Wang, Lingzhi; Liu, Yongdi; Zhang, Jinlong

2015-01-01

Highlights: • g-C 3 N 4 /TiO 2 was prepared by a one-step preparation under mild conditions. • Photocatalysts showed excellent activity under both UV and visible light. • A neat surface modification process is proved, excluding influence of N doping. • Two photocatalytic mechanisms under different wavelengths are proposed. • A wide range of available wavelengths would greatly improve practicability of TiO 2 . - Abstract: g-C 3 N 4 modified TiO 2 composites were prepared through a simple calcination process of anatase and cyanamide. The as-prepared samples were characterized by X-ray diffraction (XRD), diffuse reflectance spectrophotometry (DRS), fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), thermogravimetry differential thermal analysis (TG–DTA) and X-ray photoelectron spectroscopy (XPS), proving a successful modification of TiO 2 with g-C 3 N 4 . Photodegradation of acid orange 7 (AO7) was used to evaluate the photocatalytic activities of the composites, showing excellent activity of them under both visible and UV light. In addition, base treatment was then introduced to investigate the interaction between g-C 3 N 4 and TiO 2 . After removing the g-C 3 N 4 modified on TiO 2 by base, no nitrogen doping is found in TiO 2 lattice, demonstrating the g-C 3 N 4 was surface attached on TiO 2 and attributing all improvement of photocatalytic activity of g-C 3 N 4 /TiO 2 composite to the synergy between the two semiconductors

Construction of g-C3N4/CeO2/ZnO ternary photocatalysts with enhanced photocatalytic performance

Science.gov (United States)

Yuan, Yuan; Huang, Gui-Fang; Hu, Wang-Yu; Xiong, Dan-Ni; Zhou, Bing-Xin; Chang, Shengli; Huang, Wei-Qing

2017-07-01

Promoting the spatial separation of photoexcited charge carriers is of paramount significance for photocatalysis. In this work, binary g-C3N4/CeO2 nanosheets are first prepared by pyrolysis and subsequent exfoliation method, then decorated with ZnO nanoparticles to construct g-C3N4/CeO2/ZnO ternary nanocomposites with multi-heterointerfaces. Notably, the type-II staggered band alignments existing between any two of the constituents, as well as the efficient three-level transfer of electron-holes in unique g-C3N4/CeO2/ZnO ternary composites, leads to the robust separation of photoexcited charge carriers, as verified by its photocurrent increased by 8 times under visible light irradiation. The resulting g-C3N4/CeO2/ZnO ternary nanocomposites unveil appreciably increased photocatalytic activity, faster than that of pure g-C3N4, ZnO and g-C3N4/CeO2 by a factor of 11, 4.6 and 3.7, respectively, and good stability toward methylene blue (MB) degradation. The remarkably enhanced photocatalytic activity of g-C3N4/CeO2/ZnO ternary heterostructures can be interpreted in terms of lots of active sites of nanosheet shapes and the efficient charge separation owing to the resulting type-II band alignment with more than one heterointerface and the efficient three-level electron-hole transfer. A plausible mechanism is also elucidated via active species trapping experiments with various scavengers, which indicating that the photogenerated holes and •OH radicals play a crucial role in photodegradation reaction under visible light irradiation. This work suggest that the rational design and construction of type II multi-heterostructures is powerful for developing highly efficient and reusable visible-light photocatalysts for environmental purification and energy conversion.

Constructing effective photocatalytic purification system with P-introduced g-C3N4 for elimination of UO22+

Science.gov (United States)

Wu, Xi; Jiang, Shujuan; Song, Shaoqing; Sun, Chuanzhi

2018-02-01

Due to the inherent defects of precursor molecular structure, the limited effect of structure in the formed g-C3N4 will weaken the extension of delocalization of π electrons between the adjacent tri-s-triazine or heptazine units of g-C3N4, which thus leads to poor visible-light absorption, low utilization efficiency of charge carrier. Herein, P-introduced g-C3N4 (PC3N4) photocatalysts were constructed by partially replacing C with tributyl phosphate as precursor, and the as-designed PC3N4 photocatalysts were used to eliminate aqueous uranyl ion by photocatalytic reduction technology under visible-light irradiation. Experimental and DFT revealed that introduction of P into g-C3N4 significantly modified its electronic structure, as reflected by the narrowed band gap, enhanced visible-light absorption as well as improved transfer capability of photogenerated charge. Therefore, photocatalytic activity of PC3N4 was much better than that of pristine g-C3N4 and conventional reducing-type photocatalysts. This study suggests an efficient strategy for construct effective visible-light-responsive photocatalysts for radioactive environmental remediation.

Potential of Transition Metal Atoms Embedded in Buckled Monolayer g-C3N4 as Single-Atom Catalysts

KAUST Repository

Li, Shu-Long; Kan, Xiang; Yin, Hui; Gan, Li-Yong; Schwingenschlö gl, Udo; Zhao, Yong

2017-01-01

We use first-principles calculations to systematically explore the potential of transition metal atoms (Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Ru, Rh, Pd, Ag, Ir, Pt, and Au) embedded in buckled monolayer g-C3N4 as single-atom catalysts. We show that clustering of Sc and Ti on g-C3N4 is thermodynamically impeded and that V, Cr, Mn, and Cu are much less susceptible to clustering than the other TM atoms under investigation. Strong bonding of the transition metal atoms in the cavities of g-C3N4 and high diffusion barriers together are responsible for single-atom fixation. Analysis of the CO oxidation process indicates that embedding of Cr and Mn in g-C3N4 gives rise to promising single-atom catalysts at low temperature.

Potential of Transition Metal Atoms Embedded in Buckled Monolayer g-C3N4 as Single-Atom Catalysts

KAUST Repository

Li, Shu-Long

2017-10-27

We use first-principles calculations to systematically explore the potential of transition metal atoms (Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Ru, Rh, Pd, Ag, Ir, Pt, and Au) embedded in buckled monolayer g-C3N4 as single-atom catalysts. We show that clustering of Sc and Ti on g-C3N4 is thermodynamically impeded and that V, Cr, Mn, and Cu are much less susceptible to clustering than the other TM atoms under investigation. Strong bonding of the transition metal atoms in the cavities of g-C3N4 and high diffusion barriers together are responsible for single-atom fixation. Analysis of the CO oxidation process indicates that embedding of Cr and Mn in g-C3N4 gives rise to promising single-atom catalysts at low temperature.

Statistical model for classifying the feeding systems of Iberian pigs through Gas Chromatography (GC-FID and Isotope Ratio Mass Spectrometry (GC-C-IRMS

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García-Casco, J. M.

2013-04-01

Full Text Available In the present work we have analyzed a total of 734 subcutaneous fat samples from Iberian pigs with different feeding systems for fattening (“Bellota”, “Recebo”, “Campo” and “Cebo” over three consecutive years, 2009-2011. Lipids were extracted from the subcutaneous fat on the rump, and after esterification, they were analyzed by Gas Chromatography (GC-FID and Gas Chromatography- Combustion-Isotope Ratio Mass Spectrometry (GC-C-IRMS. Mean fatty acids and isotope ratios show that there are differences according to the year and feeding systems, two factors that should be taken into account when classifying the animals. The application of different prediction models based on Discriminant analysis has allowed us to establish a method for the classification of animals according to the feeding system type, with a correct percentage of 85% using three or four classification categories (Bellota, Recebo, Campo and/or Cebo and 91% using only two categories, Cebo and Bellota. This model could provide the basis for appropriate classification of Iberian pigs according to their feeding regime.En el presente trabajo se han analizado un total de 734 muestras de tejido subcutáneo de cerdos ibéricos con distintos tipos de alimentación de engorde (Bellota, Recebo, Cebo y Campo a lo largo de tres años consecutivos, 2009-2011. Se han extraído los lípidos de la grasa subcutánea de rabadilla, y después de su esterificación, se han analizado por Cromatografía de gases (GC-FID y por Espectrometría de masas de relaciones isotópicas (GC-C-IRMS. Las medias de los ácidos grasos y de las relaciones isotópicas muestran que existen diferencias según el año y tipo de alimentación, factores que deberían tenerse en cuenta a la hora de clasificar los animales. La aplicación de distintos modelos de predicción basados en análisis discriminante permite establecer un método para la clasificación de los animales según el tipo de alimentación, con

Separation and identification of picogram levels of dioxins and PCBs by GC/cryogenic trapping FTIR

Science.gov (United States)

Johnson, David J.; Powell, Jay R.; Krishnan, K.

1994-01-01

Capillary gas chromatography/mass spectrometry (GC/MS) has routinely been used by the analytical chemist to separate and identify low levels of environmentally important compounds. A GC/Cryogenic Trapping Fourier Transform Infrared Spectrometer (Tracer) provides the sensitivity of the GC/MS with the added capability of differentiating between compounds of the same mass. In this work, the Tracer was utilized to study low levels of six Polychlorinated Biphenyls (PCBs), eight Chlorinated Dibenzo-p-Doxins and Norflurazon. In all cases, picogram levels of these compounds were easily detected from `on the fly' generated IR chromatograms. Since the separated compounds eluting from the capillary column are cryogenically trapped onto a moving liquid nitrogen cooled ZnSe crystal, excellent signal-to- noise spectra of these same compounds may be collected after the run by returning to the same areas of deposition and signal averaging.

Changes in the molecular composition of crude oils during their preparation for GC and GC-MS analyses

Energy Technology Data Exchange (ETDEWEB)

Ahmed, M.; George, S.C. [CSIRO Petroleum, North Ryde, NSW (Australia)

2004-02-01

Rotary evaporation and nitrogen blowing are the two frequently used procedures in organic geochemistry laboratories to prepare crude oils and extractable organic matter for gas chromatography (GC) and GC-mass spectrometry (GC-MS) analyses. In this work, the effects of these preparatory procedures on the molecular composition have been comprehensively assessed for the first time, by evaporating 34 aliquots of North Sea Oil-1 dissolved in dichloromethane under a variety of conditions: (a) rotary evaporation with a reduced pressure of 80 to 60 kpa, and water bath temperatures of 30-60 {sup o}C, (b) nitrogen blowing, with flow rates of 130 to >850 ml/min and heater block temperatures of 30-60 {sup o}C, and (c) open vial evaporation in a refrigerator at 3 {sup o}C and in a fume cupboard at 22 {sup o}C. Analyses of the unaltered original oil, solution and the evaporated oil aliquots for 215 target compounds, from benzene to n-C{sub 32}, indicate that (1)

A weak-light-responsive TiO2/g-C3N4 composite film: photocatalytic activity under low-intensity light irradiation.

Science.gov (United States)

Wang, Peifang; Guo, Xiang; Rao, Lei; Wang, Chao; Guo, Yong; Zhang, Lixin

2018-05-10

A TiO 2 /g-C 3 N 4 composite photocatalytic film was prepared by in situ synthesis method and its photocatalytic capability under weak-visible-light condition was studied. The co-precursor with different ratio of melamine and TiO 2 sol-gel precursor were treated using ultrasonic mixing, physical deposition, and co-sintering method to form the smooth, white-yellow, and compact TiO 2 /g-C 3 N 4 composite films. The prepared TiO 2 /g-C 3 N 4 materials were characterized by SEM, TEM, EDS, XRD, BET, VBXPS, and UV-vis diffuse reflectance spectra. The results of composite showed that TiO 2 and g-C 3 N 4 have close interfacial connections which are favorable to charge transfer between these two semiconductors with suitable band structure, g-C 3 N 4 retard the anatase-to-rutile phase transition of TiO 2 significantly, the specific surface area were increased with g-C 3 N 4 ratio raised. Under weak-light irradiation, composite films photocatalytic experiments exhibited RhB removal efficiency approaching 90% after three recycles. Powders suspension degradation experiments revealed the removal efficiency of TiO 2 /g-C 3 N 4 (90.8%) was higher than pure TiO 2 (52.1%) and slightly lower than pure g-C 3 N 4 (96.6%). By control experiment, the enhanced photocatalysis is ascribed to the combination of TiO 2 and g-C 3 N 4 , which not only produced thin films with greater stability but also formed heterojunctions that can be favorable to charge transfer between these two semiconductors with suitable band structure. This study presents the potential application of photocatalytic film in the wastewater treatment under weak-light situation.

Analysis of the secondary compounds produced by Saccharomyces cerevisiae and wild yeast strains during the production of "cachaça" Análise dos componentes secundários produzidos por Saccharomyces cerevisiae e leveduras selvagens durante a produção de cachaça

Directory of Open Access Journals (Sweden)

Maria Cecília Fachine Dato

2005-03-01

Full Text Available The aim of this study is to compare the composition of "cachaças" produced in 10 fermentation cycles by Saccharomyces cerevisiae (Sc and wild yeast strains [Pichia silvicola (Ps, Pichia anomala 1 (Pa1, Pichia anomala 2 (Pa2 and Dekkera bruxelensis (Db], isolated from distilleries in Jaboticabal - SP, Brazil. The secondary components of the heart fraction were determined by gas chromatography. The levels of secondary components were influenced by the wine pH, which varied among yeast strains. S. cerevisiae showed slightly more secondary components, whereas wild strains produced more higher alcohols. Wild yeast strains were shown to be adequate for the production of a high quality "cachaça".O presente trabalho visou estabelecer uma comparação entre composição de cachaças produzidas por Saccharomyces cerevisiae (Sc e estirpes de leveduras selvagens [Pichia silvicola (Ps, Pichia anomala 1 (Pa1, Pichia anomala 2 (Pa2 e Dekkera bruxelensis (Db], isoladas em destilarias da região de Jaboticabal-SP. Os componentes secundários da fração denominada coração foram determinados por cromatografia gasosa. Os níveis dos componentes secundários foram influenciados pelo pH dos respectivos vinhos, os quais dependem da estirpe de levedura empregada no processo fermentativo. A Saccharomyces cerevisiae apresentou valores ligeiramente superiores de componentes secundários, enquanto as estirpes selvagens produziram maiores teores de álcoois superiores. As estirpes selvagens de leveduras mostraram-se adequadas para obtenção de uma cachaça de boa qualidade.

Composição e fungitoxicidade do óleo essencial de capim citronela em função da adubação orgânica

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Ronice Alves Veloso

2012-12-01

Full Text Available O objetivo deste trabalho foi avaliar a influência da adubação orgânica sobre o teor e a composição do óleo essencial de capim citronela (Cymbopogon nardus, bem como a fungitoxicidade desse óleo ao crescimento micelial dos fungos Didymella bryoniae, Colletotrichum gloeosporioides e Amphobotrys ricini. A extração do óleo essencial foi realizada por hidrodestilação, a partir de plantas cultivadas em quatro doses de adubação orgânica (0, 3, 6 e 9 kg de esterco bovino curtido por cova, e a identificação dos constituintes químicos foi conduzida por cromatografia gasosa/espectrometria de massas. Para avaliar a inibição do crescimento micelial, o experimento foi instalado no delineamento inteiramente casualizado, em arranjo fatorial. Foram testadas sete alíquotas do óleo essencial (0, 5, 10, 15, 20, 25 e 30 µL, em cinco épocas de avaliação, com quatro repetições. O teor de óleo essencial do capim citronela não foi afetado pela adubação orgânica, e o óleo essencial do capim citronela apresentou 24 compostos químicos, entre estes monoterpenos e sesquiterpenos, com maior concentração dos compostos citronelal, β-citronelol, geraniol e elemol. O óleo essencial do capim citronela apresenta maior efeito de inibição a Amphobotrys ricini, em comparação aos fungos Didymella bryoniae e Colletotrichum gloeosporioides.

Perfil lipídico da carne e gordura de suínos alimentados com milheto

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Rodrigo Caetano de Abreu

2014-01-01

Full Text Available O objetivo deste trabalho foi avaliar níveis de milheto na alimentação de suínos na composição lipídica e de colesterol da gordura subcutânea e da carne. Foram utilizados 48 animais, machos castrados, distribuídos em um delineamento experimental de blocos casualizados, com quatro níveis de milheto na dieta (0; 25; 50 e 75%, seis repetições, sendo cada unidade experimental constituída por dois animais. Foram analisados os perfis lipídicos da gordura e da carne através de cromatografia gasosa e a quantidade de colesterol nas amostras de carne foi determinada seguindo a metodologia de extração. O aumento do nível de milheto na dieta dos suínos reduziu (P<0,05 a concentração dos ácidos mirístico, palmítico, palmitoleico, heptadecanoico e aumentou a concentração do ácido linoleico na gordura subcutânea. O nível de inclusão de 50,82% de milheto na dieta possibilita máxima deposição do ácido linolênico na gordura. Os níveis de milheto não modificam o perfil de ácidos graxos e o teor de colesterol na carne suína. O nível de 42,09% de inclusão de milheto na dieta resulta no maior índice trombogênico da carne.

Constituintes voláteis de cafés "gourmet" e mole do cerrado do triângulo mineiro em função da torra

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Nascimento Evandro Afonso do

2003-01-01

Full Text Available Neste trabalho foi estudada a variação da composição dos voláteis de dois cafés "gourmet" e de um café mole em função do grau de torrefação. Os cafés provenientes de Araguari, cerrado do Triângulo Mineiro, foram submetidos à torra americana (grãos marrons claros, média (grãos marrons e forte (grãos pretos e, em seguida, moídos e submetidos a uma destilação por arraste de vapor em contra-corrente com diclorometano. A análise de cromatografia gasosa acoplada à espectrometria de massas (CG-EM dos constituintes voláteis mostrou que piridina, pirazina e derivados, furfural e derivados são os principais constituintes voláteis dos cafés analisados. Mostrou ainda que não é possível diferenciar os três tipos de café pelos compostos dominantes (concentração acima de 1% no aroma. Foi observado também que a torra afeta sensivelmente os resultados, sendo que a torra americana, usada normalmente na prova da xícara para classificação sensorial de cafés, produz alguns voláteis de forte impacto no aroma que não aparecem na torra média nem na forte, além de apresentar concentrações dos componentes mais comuns muito diferentes daquelas observadas nas outras duas torras.

Composição química e avaliação da atividade antibacteriana e toxicidade do óleo essencial de Croton zehntneri (variedade estragol

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José G. M. da Costa

Full Text Available Tendo em vista que bactérias resistentes a antimicrobianos representam um desafio no tratamento de infecções, é notória a necessidade de encontrar novas substâncias com propriedades antimicrobianas para serem utilizadas no combate a esses microrganismos. Este trabalho relata a avaliação da atividade antibacteriana, toxicidade e identificação dos componentes químicos do óleo essencial de Croton zehntneri (variedade estragol, planta utilizada na medicina popular como calmante e estimulante do apetite. A atividade antimicrobiana e a concentração inibitória mínima (CIM foram determinadas pelo método de difusão em discos. A avaliação da toxicidade foi realizada frente à Artemia salina com resultado considerado ativo (CL50 < 100 µg/mL. O óleo essencial das folhas apresentou atividade antibacteriana frente a todas as bactérias testadas exceto contra Salmonella typhimurium, sendo o melhor resultado frente a Shigella flexneri com CIM de 50 µg/mL. A análise da composição química foi obtida por cromatografia gasosa acoplada a espectrometria de massa (CG/EM e permitiu identificar um total de 97,4% dos componentes, com presença majoritária de estragol (76,8%. A presença de tal constituinte nos impulsiona a realização de estudos com outras bactérias, já que o estragol foi anteriormente relatado como sendo responsável por atividades antibacterianas.

Fissuração pelo Hidrogênio em um Aço API 5L X70 Soldado com Eletrodos Celulósicos de Diferentes Níveis de Resistência

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Camila Goes Mattioli

Full Text Available Resumo Aços classificados segundo a norma do American Petroleum Institute (API enfrentam o problema de trincamento a frio decorrente da soldagem. Neste trabalho foi estudado, por meio do ensaio de implante, o efeito da resistência mecânica do metal de solda sobre a susceptibilidade de um aço API-5L-X70 ao trincamento pelo hidrogênio. As soldas foram realizadas com dispositivo de soldagem por gravidade, usando-se dois eletrodos celulósicos, AWS-E6010 e AWS-E8010. O hidrogênio difusível dos eletrodos foi determinado por cromatografia gasosa. Como resultado do ensaio de implante, observou-se uma tendência maior à fissuração quando foi utilizado o eletrodo AWS-E6010. Isso pode ser relacionado à menor resistência mecânica apresentada pela solda resultante do mesmo e ao fato de o eletrodo ser menos ligado. Assim, o metal de solda pode ter se transformado a temperaturas mais elevadas, o que levou a uma maior migração do hidrogênio para a ZTA. Observou-se, ainda, que mesmo as soldas que não falharam no ensaio apresentaram trincas. Isso pode ser devido às condições de resfriamento do cordão que levaram ao aparecimento ilhas com estruturas frágeis e susceptíveis ao trincamento. Para as menores cargas usadas (0,8.σe, contudo, estas trincas não atingiram um tamanho crítico para a ruptura final do pino sendo ensaiado.

Produção de matéria seca e trocas gasosas em cultivares de mamoneira sob níveis de irrigação Dry mass production and gas exchanges in castor bean cultivars under different irrigation levels

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Cley A. S. de Freitas

2011-11-01

Full Text Available Este trabalho teve o objetivo de avaliar os efeitos de cinco níveis de irrigação por gotejamento, em três cultivares de mamoneira (IAC Guarani, Mirante 10 e BRS Paraguaçu mediante a quantificação da produção de matéria seca pelas diferentes partes da planta (limbo foliar, caule e pecíolo e a mensuração das trocas gasosas (fotossíntese, condutância estomática e transpiração. O experimento foi conduzido no campo, na Fazenda Experimental Vale do Curu, Pentecoste, CE, sob delineamento experimental em blocos casualizados com parcelas subdivididas, em esquema fatorial 5 x 3 e com três repetições. Os tratamentos foram cinco lâminas de irrigação (25, 50, 75, 100 e 125% da evaporação do tanque Classe "A" e três cultivares. Os diferentes níveis de irrigação influenciaram as variáveis: massa seca do pecíolo, condutância estomática e fotossíntese; os valores máximos para essas variáveis foram obtidos com o nível de irrigação correspondente a 125% da evaporação no tanque Classe A. Houve uma resposta diferenciada na produção de biomassa e nas trocas gasosas entre as três cultivares avaliadas em todas as variáveis estudadas, exceto na massa seca do pecíolo.This study was aimed at evaluating the effects of five levels of drip irrigation in three castor bean cultivars (IAC Guarani, Mirante 10 and BRS Paraguaçu by measuring the dry mass production by the different plant parts (leaf blade, petiole and plant stem as well as by measuring the gas exchange processes (photosynthesis, stomatal conductance and transpiration. The experiment was conducted in the field, at the Fazenda Experimental, Vale do Curu, Pentecoste, Ceará (Br. The experiment was conducted in a randomized blocks in a 5x3 factorial scheme, in split plots with three repetitions. The treatments were five irrigation levels (25, 50, 75, 100 and 125% of the class "A" pan evaporation (CAE applied to the three cultivars. The different irrigation levels

E. coli mismatch repair enhances AT-to-GC mutagenesis caused by alkylating agents.

Science.gov (United States)

Nakano, Kota; Yamada, Yoko; Takahashi, Eizo; Arimoto, Sakae; Okamoto, Keinosuke; Negishi, Kazuo; Negishi, Tomoe

2017-03-01

Alkylating agents are known to induce the formation of O 6 -alkylguanine (O 6 -alkG) and O 4 -alkylthymine (O 4 -alkT) in DNA. These lesions have been widely investigated as major sources of mutations. We previously showed that mismatch repair (MMR) facilitates the suppression of GC-to-AT mutations caused by O 6 -methylguanine more efficiently than the suppression of GC-to-AT mutations caused by O 6 -ethylguanine. However, the manner by which O 4 -alkyT lesions are repaired remains unclear. In the present study, we investigated the repair pathway involved in the repair of O 4 -alkT. The E. coli CC106 strain, which harbors Δprolac in its genomic DNA and carries the F'CC106 episome, can be used to detect AT-to-GC reverse-mutation of the gene encoding β-galactosidase. Such AT-to-GC mutations should be induced through the formation of O 4 -alkT at AT base pairs. As expected, an O 6 -alkylguanine-DNA alkyltransferase (AGT) -deficient CC106 strain, which is defective in both ada and agt genes, exhibited elevated mutant frequencies in the presence of methylating agents and ethylating agents. However, in the UvrA-deficient strain, the methylating agents were less mutagenic than in wild-type, while ethylating agents were more mutagenic than in wild-type, as observed with agents that induce O 6 -alkylguanine modifications. Unexpectedly, the mutant frequencies decreased in a MutS-deficient strain, and a similar tendency was observed in MutL- or MutH-deficient strains. Thus, MMR appears to promote mutation at AT base pairs. Similar results were obtained in experiments employing double-mutant strains harboring defects in both MMR and AGT, or MMR and NER. E. coli MMR enhances AT-to-GC mutagenesis, such as that caused by O 4 -alkylthymine. We hypothesize that the MutS protein recognizes the O 4 -alkT:A base pair more efficiently than O 4 -alkT:G. Such a distinction would result in misincorporation of G at the O 4 -alkT site, followed by higher mutation frequencies in wild

An Innovative Rapid Method for Analysis of 10 Organophosphorus Pesticide Residues in Wheat by HS-SPME-GC-FPD/MSD.

Science.gov (United States)

Du, Xin; Ren, YongLin; Beckett, Stephen J

2016-01-01

The rapid detection of pesticide residues in wheat has become a top food security priority. A solvent-free headspace solid-phase microextraction (HS-SPME) has been evaluated for rapid screening of organophosphorus pesticide (OPP) residues in wheat with high sensitivity. Individual wheat samples (1.7 g), spiked with 10 OPPs, were placed in a 4 mL sealed amber glass vial and heated at 60°C for 45 min. During this time, the OPP residues were extracted with a 50 μm/30 μm divinylbenzene (DVB)/carboxen (CAR)/plasma desorption mass spectroscopy polydimethylsiloxane (PDMS) fiber from the headspace above the sample. The fiber was then removed and injected into the GC injection port at 250°C for desorption of the extracted chemicals. The multiple residues were identified by a GC mass spectrometer detector (GC-MSD) and quantified with a GC flame photometric detector (GC-FPD). Seven spiked levels of 10 OPPs on wheat were analyzed. The GC responses for a 50 μm/30 μm DVB/CAR/PDMS fiber increased with increasing spiking levels, yielding significant (R(2) > 0.98) linear regressions. The lowest LODs of the multiple pesticide standards were evaluated under the conditions of the validation study in a range of levels from 0 (control) to 100 ng of pesticide residue per g of wheat that separated on a low-polar GC capillary column (Agilent DB-35UI). The results of the HS-SPME method were compared with the QuEChERS AOAC 2007.01 method and they showed several advantages over the latter. These included improved sensitivity, selectivity, and simplicity.

LC clean-up and GC/MS analysis of polycyclic aromatic hydrocarbons in river sediment

International Nuclear Information System (INIS)

Nondek, L.; Kuzilek, M.; Krupicka, S.

1993-01-01

An LC clean-up procedure based upon a complexation between polycyclic aromatic hydrocarbons (PAHs) and silica with chemically bonded 2,4-dinitroaniline has been combined with GC/MS. The LC pre-separation makes it possible to obtain a relatively clean fraction of PAHs free from alkanes, alkylbenzenes and naphthalenes, PCBs, chlorinated pesticides and many other interfering compounds. This fraction has been analyzed using capillary GC and mass selective detector (MSD). Substantial improvement of the MS spectra of PAHs with three or more fused benzene rings is achieved. (orig.)

Use of capillary GC-MS for identification of radiation-induced DNA base damage: Implications for base-excision repair of DNA

International Nuclear Information System (INIS)

Dizdaroglu, M.

1985-01-01

Application of GC-MS to characterization of radiation-induced base products of DNA and DNa base-amino acid crosslinks is presented. Samples of γ-irradiated DNa were hydrolyzed with formic acid, trimethylsilylated and subjected to GC-MS analysis using a fused silica capillary column. Hydrolysis conditions suitable for the simultaneous analysis of the radiation-induced products of all four DNA bases in a single run were determined. The trimethylsilyl derivatives of these products had excellent GC-properties and easily interpretable mass spectra. The complementary use of t-butyldimetylsilyl derivatives was also demonstrated. Moreover, the usefulness of this method for identification of radiation-induced DNA base-amino acid crosslinks was shown using γ-irradiated mixtures of thymine and tyrosine or phenylalanine. Because of the excellent resolving power of capillary GC and the instant and highly sensitive identification by MS, GC-MS is suggested as a suitable technique for identification of altered bases removed from DNA by base-excision repair enzymes

GC-MS and FT-IR analysis of a coastal medicinal plant-Hyptis suaveolens (L. Poit

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Joselin Joseph

2016-05-01

Full Text Available Objective: To investigate the bioactive components of a coastal medicinal plant, Hyptis suaveolens (L. Poit. (H. suaveolens leaves using fourier transform-infrared spectroscopy and gas chromatography-mass spectrometer (GC-MS. Methods: The chemical compositions of the ethanol extract of whole plant of H. suaveolens was investigated using PerkinElmer GC-MS, while the mass spectra of the compounds found in the extract was matched with the National Institute of Standard and Technology library. Results: The results of fourier transform-infrared spectroscopy analysis confirmed the presence of secondary alcohols, phenols, alkanes, alkynes, aromatics, nitro compounds and aliphatic compounds. GC-MS analysis of the ethanolic extract revealed the existence of 30 phytochemical compounds. 5,5-Dimethylimidazolidin-2,4-diamine (20.35% was found to be the major compound. Conclusions: The results of this study offer a platform to use H. suaveolens leaves as herbal alternative for various diseases.

GC-MS and FT-IR analysis of a coastal medicinal plant-Hyptis suaveolens (L.) Poit

Institute of Scientific and Technical Information of China (English)

Joselin Joseph; Solomon Jeeva

2016-01-01

Objective:To investigate the bioactive components of a coastal medicinal plant,Hyptis suaveolens (L.) Poit. (H. suaveolens) leaves using fourier transform-infrared spectroscopy and gas chromatography-mass spectrometer (GC-MS). Methods: The chemical compositions of the ethanol extract of whole plant ofH. suaveolens was investigated using PerkinElmerGC-MS, while the mass spectra of the compounds found in the extract was matched with the National Institute of Standard and Technology library. Results: The results of fourier transform-infrared spectroscopy analysis confirmed the presence of secondary alcohols, phenols, alkanes, alkynes, aromatics, nitro compounds and aliphatic compounds.GC-MS analysis of the ethanolic extract revealed the existence of 30 phytochemical compounds. 5,5-Dimethylimidazolidin-2,4-diamine (20.35%) was found to be the major compound. Conclusions: The results of this study offer a platform to useH. suaveolens leaves as herbal alternative for various diseases.

Trapping hydropyrolysates on silica and their subsequent desorption to facilitate rapid fingerprinting by GC-MS

Energy Technology Data Exchange (ETDEWEB)

Meredith, W.; Russell, C.A.; Cooper, M.; Snape, C.E. [Nottingham Univ. (United Kingdom). Fuel and Energy Centre; Love, G.D. [Newcastle upon Tyne Univ. (United Kingdom). School of Civil Engineering and Geosciences; Fabbri, D. [Universita di Bologna, Ravenna (Italy). Lab. di Chimica Ambientale; Vane, C.H. [British Geological Society, Keyworth (United Kingdom)

2004-01-01

Analytical hydropyrolysis performed under high hydrogen gas pressure (>10 MPa) has been demonstrated to possess the unique ability to release high yields of biomarker hydrocarbons covalently bound within the non-hydrocarbon macromolecular fraction of crude oils and source rocks. This study describes the development of the experimental procedure for trapping the product oils (hydropyrolysates) on silica to facilitate more convenient recovery than conventional collection and to allow analysis by thermal desorption-GC-MS without any prior work-up. Conventionally, the trap has consisted of a stainless steel coil, cooled with dry ice from which the products are recovered in organic solvents. Replacing this with a system in which the hydropyrolysates are adsorbed on a small mass of silica greatly reduces the turn-around time between tests, and aids the recovery and separation of the products. This method has been developed using an oil shale and an oil asphaltene fraction, with the silica trap producing very similar biomarker profiles to that from the conventional trap. The quantitative recovery of hydrocarbons from a light crude oil desorbed from silica under hydropyrolysis conditions demonstrates no significant loss of the high molecular weight n-alkanes (>n-C{sub 10}) for both trapping methods. The use of liquid nitrogen as the trap coolant results in significantly improved recovery of the lower molecular mass constituents. The silica trapping method allows for the hydropyrolysates to be characterised by thermal desorption-GC-MS, which has been investigated both on- and off-line. The oils undergo relatively little cracking during desorption, with similar n-alkane and biomarker profiles being obtained as with normal work-up and GC-MS analysis. Thus, in terms of fingerprinting geomacromolecules, ''hypy-thermal desorption-GC-MS'' appears to have the potential to be developed as an attractive alternative to traditional py-GC-MS. (author)

Preparative Capillary GC for Characterization of Five Dracocephalum Essential Oils from Mongolia, and their Mosquito Larvicidal Activity

Science.gov (United States)

(DF), D. moldavica L. (DM), D. fruticulosum Steph. ex Willd. (DFr) and D. peregrinum L. (DP) were evaluated. Simultaneous GC-FID and GC-MS analyses revealed in the EOs of DR, DF and DM an unidentified compound (1) ([M+122], 5.4%, 57.9% and 74.0%, respectively). Therefore, we aimed to isolate compoun...

Highly Enhanced Photoreductive Degradation of Polybromodiphenyl Ethers with g-C3N4/TiO2 under Visible Light Irradiation

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Weidong Ye

2017-04-01

Full Text Available A series of high activity photocatalysts g-C3N4-TiO2 were synthesized by simple one-pot thermal transformation method and characterized by transmission electron microscopy (TEM, scanning electron microscopy (SEM, X-ray diffraction (XRD, X-ray photoelectron spectroscopy, Brunauer–Emmett–Teller (BET surface area, and ultraviolet–visible diffuse reflectance spectroscopy (UV-Vis-DRS. The g-C3N4-TiO2 samples show highly improved photoreductive capability for the degradation of polybromodiphenyl ethers compared with g-C3N4 under visible light irradiation. Among all the hybrids, 0.02-C3N4-TiO2 with 2 wt % g-C3N4 loaded shows the highest reaction rate, which is 15 times as high as that in bare g-C3N4. The well-matched band gaps in heterojunction g-C3N4-TiO2 not only strengthen the absorption intensity, but also show more effective charge carrier separation, which results in the highly enhanced photoreductive performance under visible light irradiation. The trapping experiments show that holetrapping agents largely affect the reaction rate. The rate of electron accumulation in the conductive band is the rate-determining step in the degradation reaction. A possible photoreductive mechanism has been proposed.

EIA and GC/MS analysis of 8-isoprostane in EBC of children with problematic asthma.

Science.gov (United States)

Carraro, S; Cogo, P E; Isak, I; Simonato, M; Corradi, M; Carnielli, V P; Baraldi, E

2010-06-01

Asthmatic airways are characterised by enhanced oxidative stress, which can be studied by measuring biomarkers, such as 8-isoprostane. The aims of the present study were: 1) to measure the concentrations of 8-isoprostane in exhaled breath condensate (EBC) and urine of children with problematic and well-controlled asthma; 2) to compare the concentrations of 8-isoprostane measured by gas chromatographic/negative ion chemical ionisation mass spectrometry (GC/NICI-MS) and by an enzymatic immunoassay (EIA). We recruited 20 asthmatic allergic children, 13 with well-controlled asthma and seven with problematic asthma. They underwent exhaled nitric oxide measurements and spirometry, and both EBC and urine samples were collected. 8-isoprostane was measured in EBC by GC/NICI-MS and EIA. 8-isoprostane concentrations in EBC were significantly higher in children with problematic asthma than in children with well-controlled asthma (p = 0.01). An acceptable reproducibility emerged between GC/NICI-MS and EIA (coefficient of reproducibility 11.5 pg x mL(-1)). 8-isoprostane levels measured in urine did not correlate with those measured in EBC. We showed that 8-isoprostane in EBC was significantly increased in children with problematic asthma, suggesting a role for oxidative stress in this asthma phenotype. In addition we found an acceptable reproducibility of EIA compared to GC/NICI-MS, even if the latter method had higher accuracy.

Detection of petroleum contamination in river sediments from Quebec City region using GC-IRMS

International Nuclear Information System (INIS)

Rogers, K.M.; Savard, M.M.

1999-01-01

Isotopic analysis by compound specific gas chromatography-isotope ratio mass spectrometry (GC-IRMS) is used to detect and characterize petroleum pollution in surficial sediments along the St Lawrence River, near Quebec City. Unusually mature n-alkane distributions have been found in some recent intertidal sediments in the region. GC-IRMS results suggest that the n-alkanes are not derived from indigenous organic sources because they carry delta 13 C values between -30.0 and -27.0 per mille, as well as very small isotopic differences between odd and even numbered n-alkanes, which are both typically associated with petroleum products. Comparison of these sediments with bunker fuel, an oil used in the shipping industry, has shown a close isotopic correlation in some sites, which is further supported by biomarkers. Overall, the contamination has been dispersed along the river but is generally localized around the industrial region where hydrocarbon transfer from shore storage to ships takes place. This study illustrates how GC-IRMS can be used effectively in the detection and characterization of petroleum pollutants in sediments. (author)

Analysis of miRNA expression profiles in melatonin-exposed GC-1 spg cell line.

Science.gov (United States)

Zhu, Xiaoling; Chen, Shuxiong; Jiang, Yanwen; Xu, Ying; Zhao, Yun; Chen, Lu; Li, Chunjin; Zhou, Xu

2018-02-05

Melatonin is an endocrine neurohormone secreted by pinealocytes in the pineal gland. It exerts diverse physiological effects, such as circadian rhythm regulator and antioxidant. However, the functional importance of melatonin in spermatogenesis regulation remains unclear. The objectives of this study are to: (1) detect melatonin affection on miRNA expression profiles in GC-1 spg cells by miRNA deep sequencing (DeepSeq) and (2) define melatonin affected miRNA-mRNA interactions and associated biological processes using bioinformatics analysis. GC-1 spg cells were cultured with melatonin (10 -7 M) for 24h. DeepSeq data were validated using quantitative real-time reverse transcription polymerase chain reaction analysis (qRT-PCR). A total of 176 miRNA expressions were found to be significantly different between two groups (fold change of >2 or melatonin could regulate the expression of miRNA to perform its physiological effects in GC-1 spg cells. These results should be useful to investigate the biological function of miRNAs regulated by melatonin in spermatogenesis and testicular germ cell tumor. Copyright © 2017 Elsevier B.V. All rights reserved.

Challenges in GC-MS analysis: Case studies on phenibut and ethylphenidate.

Science.gov (United States)

Lee, Hui Zhi Shirley; Ong, Mei Ching; Lim, Jong Lee Wendy; Yap, Tiong Whei Angeline

2017-08-01

The challenges associated with drug analysis using GC-MS such as thermal degradation, cyclisation or unwanted side reactions causing potential erroneous identification have become evident in view of the high surge in new drugs available in the market. Two case studies illustrated how alternative methods or modifications to existing techniques can help to circumvent the limitations. In the first case study, phenibut which is a GABA analogue, cyclises to 4-phenyl-2-pyrrolidinone under thermal conditions. The identification of phenibut was achieved through derivatisation and identification of its TMS derivative. The second case study, thermal degradation was minimised on drugs of interest methylphenidate and ethylphenidate by reducing the injector port temperature to 200°C and maintaining the GC oven temperature at below 190°C in order to prevent thermal degradation of the drugs of interest. Copyright © 2017 Elsevier B.V. All rights reserved.

Molecular cloning, homology modeling and site-directed mutagenesis of vanadium-dependent bromoperoxidase (GcVBPO1) from Gracilaria changii (Rhodophyta).

Science.gov (United States)

Baharum, H; Chu, W-C; Teo, S-S; Ng, K-Y; Rahim, R Abdul; Ho, C-L

2013-08-01

Vanadium-dependent haloperoxidases belong to a class of vanadium enzymes that may have potential industrial and pharmaceutical applications due to their high stability. In this study, the 5'-flanking genomic sequence and complete reading frame encoding vanadium-dependent bromoperoxidase (GcVBPO1) was cloned from the red seaweed, Fracilaria changii, and the recombinant protein was biochemically characterized. The deduced amino acid sequence of GcVBPO1 is 1818 nucleotides in length, sharing 49% identity with the vanadium-dependent bromoperoxidases from Corralina officinalis and Cor. pilulifera, respectively. The amino acid residues associated with the binding site of vanadate cofactor were found to be conserved. The Km value of recombinant GcVBPO1 for Br(-) was 4.69 mM, while its Vmax was 10.61 μkat mg(-1) at pH 7. Substitution of Arg(379) with His(379) in the recombinant protein caused a lower affinity for Br(-), while substitution of Arg(379) with Phe(379) not only increased its affinity for Br(-) but also enabled the mutant enzyme to oxidize Cl(-). The mutant Arg(379)Phe was also found to have a lower affinity for I(-), as compared to the wild-type GcVBPO1 and mutant Arg(379)His. In addition, the Arg(379)Phe mutant has a slightly higher affinity for H2O2 compared to the wild-type GcVBPO1. Multiple cis-acting regulatory elements associated with light response, hormone signaling, and meristem expression were detected at the 5'-flanking genomic sequence of GcVBPO1. The transcript abundance of GcVBPO1 was relatively higher in seaweed samples treated with 50 parts per thousand (ppt) artificial seawater (ASW) compared to those treated in 10 and 30 ppt ASW, in support of its role in the abiotic stress response of seaweed. Copyright © 2013 Elsevier Ltd. All rights reserved.

The in vitro GcMAF effects on endocannabinoid system transcriptionomics, receptor formation, and cell activity of autism-derived macrophages

Science.gov (United States)

2014-01-01

Background Immune system dysregulation is well-recognized in autism and thought to be part of the etiology of this disorder. The endocannabinoid system is a key regulator of the immune system via the cannabinoid receptor type 2 (CB2R) which is highly expressed on macrophages and microglial cells. We have previously published significant differences in peripheral blood mononuclear cell CB2R gene expression in the autism population. The use of the Gc protein-derived Macrophage Activating Factor (GcMAF), an endogenous glycosylated vitamin D binding protein responsible for macrophage cell activation has demonstrated positive effects in the treatment of autistic children. In this current study, we investigated the in vitro effects of GcMAF treatment on the endocannabinoid system gene expression, as well as cellular activation in blood monocyte-derived macrophages (BMDMs) from autistic patients compared to age-matched healthy developing controls. Methods To achieve these goals, we used biomolecular, biochemical and immunocytochemical methods. Results GcMAF treatment was able to normalize the observed differences in dysregulated gene expression of the endocannabinoid system of the autism group. GcMAF also down-regulated the over-activation of BMDMs from autistic children. Conclusions This study presents the first observations of GcMAF effects on the transcriptionomics of the endocannabinoid system and expression of CB2R protein. These data point to a potential nexus between endocannabinoids, vitamin D and its transporter proteins, and the immune dysregulations observed with autism. PMID:24739187

The in vitro GcMAF effects on endocannabinoid system transcriptionomics, receptor formation, and cell activity of autism-derived macrophages.

Science.gov (United States)

Siniscalco, Dario; Bradstreet, James Jeffrey; Cirillo, Alessandra; Antonucci, Nicola

2014-04-17

Immune system dysregulation is well-recognized in autism and thought to be part of the etiology of this disorder. The endocannabinoid system is a key regulator of the immune system via the cannabinoid receptor type 2 (CB2R) which is highly expressed on macrophages and microglial cells. We have previously published significant differences in peripheral blood mononuclear cell CB2R gene expression in the autism population. The use of the Gc protein-derived Macrophage Activating Factor (GcMAF), an endogenous glycosylated vitamin D binding protein responsible for macrophage cell activation has demonstrated positive effects in the treatment of autistic children. In this current study, we investigated the in vitro effects of GcMAF treatment on the endocannabinoid system gene expression, as well as cellular activation in blood monocyte-derived macrophages (BMDMs) from autistic patients compared to age-matched healthy developing controls. To achieve these goals, we used biomolecular, biochemical and immunocytochemical methods. GcMAF treatment was able to normalize the observed differences in dysregulated gene expression of the endocannabinoid system of the autism group. GcMAF also down-regulated the over-activation of BMDMs from autistic children. This study presents the first observations of GcMAF effects on the transcriptionomics of the endocannabinoid system and expression of CB2R protein. These data point to a potential nexus between endocannabinoids, vitamin D and its transporter proteins, and the immune dysregulations observed with autism.

DFT study on the attacking mechanisms of H and OH radicals to G-C and A-T base pairs in water

Energy Technology Data Exchange (ETDEWEB)

Okutsu, N.; Shimamura, K.; Shimizu, E.; Kurita, N., E-mail: kurita@cs.tut.ac.jp [Department of Computer Science and Engineering, Toyohashi University of Technology, Toyohashi, Aichi, 441-8580 (Japan); Shulga, S. [Institute for Food Biotechnology and Genomics, National Academy of Sciences of Ukraine, Kyiv (Ukraine); Danilov, V. I. [Institute of Molecular Biology and Genetics, National Academy of Sciences of Ukraine, Kyiv (Ukraine)

2016-02-01

To elucidate the effect of radicals on DNA base pairs, we investigated the attacking mechanism of OH and H radicals to the G-C and A-T base pairs, using the density functional theory (DFT) calculations in water approximated by the continuum solvation model. The DFT calculations revealed that the OH radical abstracts the hydrogen atom of a NH{sub 2} group of G or A base and induces a tautomeric reaction for an A-T base pair more significantly than for a G-C base pair. On the other hand, the H radical prefers to bind to the Cytosine NH{sub 2} group of G-C base pair and induce a tautomeric reaction from G-C to G*-C*, whose activation free energy is considerably small (−0.1 kcal/mol) in comparison with that (42.9 kcal/mol) for the reaction of an A-T base pair. Accordingly, our DFT calculations elucidated that OH and H radicals have a significant effect on A-T and G-C base pairs, respectively. This finding will be useful for predicting the effect of radiation on the genetic information recorded in the base sequences of DNA duplexes.

DFT study on the attacking mechanisms of H and OH radicals to G-C and A-T base pairs in water

International Nuclear Information System (INIS)

Okutsu, N.; Shimamura, K.; Shimizu, E.; Kurita, N.; Shulga, S.; Danilov, V. I.

2016-01-01

To elucidate the effect of radicals on DNA base pairs, we investigated the attacking mechanism of OH and H radicals to the G-C and A-T base pairs, using the density functional theory (DFT) calculations in water approximated by the continuum solvation model. The DFT calculations revealed that the OH radical abstracts the hydrogen atom of a NH 2 group of G or A base and induces a tautomeric reaction for an A-T base pair more significantly than for a G-C base pair. On the other hand, the H radical prefers to bind to the Cytosine NH 2 group of G-C base pair and induce a tautomeric reaction from G-C to G*-C*, whose activation free energy is considerably small (−0.1 kcal/mol) in comparison with that (42.9 kcal/mol) for the reaction of an A-T base pair. Accordingly, our DFT calculations elucidated that OH and H radicals have a significant effect on A-T and G-C base pairs, respectively. This finding will be useful for predicting the effect of radiation on the genetic information recorded in the base sequences of DNA duplexes

Transfer of the high-GC cyclohexane carboxylate degradation pathway from Rhodopseudomonas palustris to Escherichia coli for production of biotin.

Science.gov (United States)

Bernstein, Jeffrey R; Bulter, Thomas; Liao, James C

2008-01-01

This work demonstrates the transfer of the five-gene cyclohexane carboxylate (CHC) degradation pathway from the high-GC alphaproteobacterium Rhodopseudomonas palustris to Escherichia coli, a gammaproteobacterium. The degradation product of this pathway is pimeloyl-CoA, a key metabolite in E. coli's biotin biosynthetic pathway. This pathway is useful for biotin overproduction in E. coli; however, the expression of GC-rich genes is troublesome in this host. When the native R. palustris CHC degradation pathway is transferred to a DeltabioH pimeloyl-CoA auxotroph of E. coli, it is unable to complement growth in the presence of CHC. To overcome this expression problem we redesigned the operon with decreased GC content and removed stretches of high-GC intergenic DNA which comprise the 5' untranslated region of each gene, replacing these features with shorter low-GC sequences. We show this synthetic construct enables growth of the DeltabioH strain in the presence of CHC. When the synthetic degradation pathway is overexpressed in conjunction with the downstream genes for biotin biosynthesis, we measured significant accumulation of biotin in the growth medium, showing that the pathway transfer is successfully integrated with the host metabolism.

GC Analyses of Salvia Seeds as Valuable Essential Oil Source

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Mouna Ben Taârit

2014-01-01

Full Text Available The essential oils of seeds of Salvia verbenaca, Salvia officinalis, and Salvia sclarea were obtained by hydrodistillation and analyzed by gas chromatography (GC and GC-mass spectrometry. The oil yields (w/w were 0.050, 0.047, and 0.045% in S. verbenaca, S. sclarea, and S. officinalis, respectively. Seventy-five compounds were identified. The essential oil composition of S. verbenaca seeds showed that over 57% of the detected compounds were oxygenated monoterpenes followed by sesquiterpenes (24.04% and labdane type diterpenes (5.61%. The main essential oil constituents were camphor (38.94%, caryophyllene oxide (7.28%, and 13-epi-manool (5.61%, while those of essential oil of S. officinalis were α-thujone (14.77%, camphor (13.08%, and 1,8-cineole (6.66%. In samples of S. sclarea, essential oil consists mainly of linalool (24.25%, α-thujene (7.48%, linalyl acetate (6.90%, germacrene-D (5.88%, bicyclogermacrene (4.29%, and α-copaene (4.08%. This variability leads to a large range of naturally occurring volatile compounds with valuable industrial and pharmaceutical outlets.

Forensic Drug Identification, Confirmation, and Quantification Using Fully Integrated Gas Chromatography with Fourier Transform Infrared and Mass Spectrometric Detection (GC-FT-IR-MS).

Science.gov (United States)

Lanzarotta, Adam; Lorenz, Lisa; Voelker, Sarah; Falconer, Travis M; Batson, JaCinta S

2018-05-01

This manuscript is a continuation of a recent study that described the use of fully integrated gas chromatography with direct deposition Fourier transform infrared detection and mass spectrometric detection (GC-FT-IR-MS) to identify and confirm the presence of sibutramine and AB-FUBINACA. The purpose of the current study was to employ the GC-FT-IR portion of the same instrument to quantify these compounds, thereby demonstrating the ability to identify, confirm, and quantify drug substances using a single GC-FT-IR-MS unit. The performance of the instrument was evaluated by comparing quantitative analytical figures of merit to those measured using an established, widely employed method for quantifying drug substances, high performance liquid chromatography with ultraviolet detection (HPLC-UV). The results demonstrated that GC-FT-IR was outperformed by HPLC-UV with regard to sensitivity, precision, and linear dynamic range (LDR). However, sibutramine and AB-FUBINACA concentrations measured using GC-FT-IR were not significantly different at the 95% confidence interval compared to those measured using HPLC-UV, which demonstrates promise for using GC-FT-IR as a semi-quantitative tool at the very least. The most significant advantage of GC-FT-IR compared to HPLC-UV is selectivity; a higher level of confidence regarding the identity of the analyte being quantified is achieved using GC-FT-IR. Additional advantages of using a single GC-FT-IR-MS instrument for identification, confirmation, and quantification are efficiency, increased sample throughput, decreased consumption of laboratory resources (solvents, chemicals, consumables, etc.), and thus cost.

Characterisation of free and glycosidically bound odourant compounds of Aragonez clonal musts by GC-O.

Science.gov (United States)

Botelho, Goreti; Mendes-Faia, Arlete; Clímaco, Maria Cristina

2010-01-11

To evaluate the potential aroma of Aragonez clonal red musts, several free and glycosidically bound odourant compounds were extracted. Then, the gas chromatography-olfactometry (GC-O) posterior intensity method was used to evaluate their odour intensity and the compounds were identified by gas chromatography-mass spectrometry (GC-MS). A group of eight sniffers evaluated free and bound fractions of Aragonez musts and perceived forty-three and twenty-two odourant peaks respectively. Furaneol (burnt sugar, candy-cotton) and vanillin (vanilla, sweet) were identified in both free and bound fractions of Aragonez musts, indicating their grape-derived origin. Principal component analysis (PCA) was applied to the posterior intensity method data and a relationship between the different odourant compound variables and the free fractions was established. Two principal components (PCs) were found which together explained 100% of the total variance. A large number of potentially important but yet unknown odourants was detected by the GC-O analysis.

Cromatografia em camada delgada para o diagnóstico da intoxicação por aldicarb ("chumbinho" em cães e gatos Thin-layer chromatography for aldicarb poisoning diagnosis in dogs and cats

Directory of Open Access Journals (Sweden)

F.G. Xavier

2007-10-01

Full Text Available Avaliou-se a cromatografia em camada delgada (CCD como método de diagnóstico toxicológico para os casos de intoxicação por aldicarb em cães e gatos, utilizando-se 50 amostras de conteúdo gástrico obtidas durante a necropsia e 50 amostras de alimentos utilizados como iscas para intoxicar criminalmente os animais. Todas as amostras resultaram positivas para o aldicarb, mostrando ser a CCD uma técnica qualitativa eficiente, rápida e de baixo custo, com uso potencial na toxicologia veterinária forense.The present study concerns about the identification of aldicarb residues using thin-layer chromatography (TLC in 50 samples of gastric content obtained from the necropsy of dogs and cats and 50 samples of foods suspected of being used as baits. All samples resulted positive for aldicarb showing that the TLC is an efficient, fast and not expensive qualitative method for the detection of aldicarb, being useful for this purpose in the forensic veterinary toxicology.

California serogroup GC (G1) glycoprotein is the principal determinant of pH-dependent cell fusion and entry

International Nuclear Information System (INIS)

Plassmeyer, Matthew L.; Soldan, Samantha S.; Stachelek, Karen M.; Martin-Garcia, Julio; Gonzalez-Scarano, Francisco

2005-01-01

Members of the California serogroup of orthobunyaviruses, particularly La Crosse (LAC) and Tahyna (TAH) viruses, are significant human pathogens in areas where their mosquito vectors are endemic. Previous studies using wild-type LAC and TAH181/57, a highly neurovirulent strain with low neuroinvasiveness (Janssen, R., Gonzalez-Scarano, F., Nathanson, N., 1984. Mechanisms of bunyavirus virulence. Comparative pathogenesis of a virulent strain of La Crosse and an avirulent strain of Tahyna virus. Lab. Invest. 50 (4), 447-455), have demonstrated that the neuroinvasive phenotype maps to the M segment, the segment that encodes the two viral glycoproteins GN (G2) and GC (G1), as well as a non-structural protein NSm. To further define the role of GN and GC in fusion and entry, we prepared a panel of recombinant M segment constructs using LAC, TAH181/57, and V22F, a monoclonal-resistant variant of LAC with deficient fusion function. These M segment constructs were then tested in two surrogate assays for virus entry: a cell-to-cell fusion assay based on T7-luciferase expression, and a pseudotype transduction assay based on the incorporation of the bunyavirus glycoproteins on an MLV backbone. Both assays demonstrated that GC is the principal determinant of virus fusion and cell entry, and furthermore that the region delineated by amino acids 860-1442, corresponding to the membrane proximal two-thirds of GC, is key to these processes. These results, coupled with structural modeling suggesting homologies between the carboxy region of GC and Sindbis virus E1, suggest that the LAC GC functions as a type II fusion protein

Deficiência hídrica e aplicação de ABA nas trocas gasosas e no acúmulo de flavonoides em calêndula (Calendula officinalis L. = Water deficit and ABA application on leaf gas exchange and flavonoid content in marigold (Calendula officinalis L..

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Ana Cláudia Pacheco

2011-04-01

Full Text Available O objetivo deste trabalho foi avaliar os efeitos da deficiencia hidrica e aplicacao de acido abscisico (ABA sobre aspectos fisiologicos e teor de flavonoides em plantas de calendula. Oexperimento foi instalado em condicoes de casa-de-vegetacao com plantas envasadas. No inicio do florescimento de plantas de calendula, foram aplicados quatro intervalos de suspensao da irrigacao (irrigacao diaria; tres; seis e nove dias sem irrigar, acompanhados por tres doses de ABA (0, 10 e 100 ƒÊM. Avaliou-se o conteudo relativo de agua na folha (CRA e as trocas gasosas, utilizando-se um analisador portatil por infravermelho (A: fotossintese liquida, gs: condutancia estomatica, E: transpiracao, Ci: concentracao intercelular de CO2 e EUA: eficiencia de uso daagua. Aos nove dias sem irrigacao ocorreram reducoes significativas em todas as variaveis de trocas gasosas analisadas, independente da aplicacao de ABA. Concluiu-se que o efeito principal do ABA foi o de causar diminuicao na gs, a qual foi acompanhada de reducao em A somente quando as plantas estavam desidratadas. As intensidades de deficiencia hidrica testadas nao causaram interferencia no acumulo de flavonoides nas inflorescencias. Entretanto, o ABA restringiu a biossintese de flavonoides, tanto nas plantas-controle como nas plantas submetidas a deficiencia hidrica.The goal of this study was to evaluate the effects of water deficit and abscisic acid (ABA application on physiological parameters and flavonoid production in marigold plant. The experiment was performed under nursery conditions with potted plants. It was tested water deficit by withholding water (control . diary irrigation, 3, 6 and9 days without irrigation followed by 3 ABA concentrations (0, 10 e 100 ƒÊM applied in the beginning of blooming. It was evaluated the relative water content and the leaf gas exchange using a portable infrared gas analyzer (A: net photosynthesis, gs: stomatal conductance, E: transpiration, Ci: CO2 intercellular

Improvenments in environmental trace analysis by GC-IR and LC-IR.

NARCIS (Netherlands)

Visser, T.; Vredenbregt, M.J.; Jong, A.P.J.M.; Somsen, G.W.; Hankemeier, T.; Velthorst, N.H.; Gooijer, C.; Brinkman, U.A.T.

1997-01-01

Research has been carried out to enlarge the potential of infrared (IR) spectrometry as a detector in gas and liquid chromatography (GC and LC). The study has been directed to applications in environmental analysis. Examples of recently obtained results are presented. The analyte detectability of

Amino acid analysis in biological fluids by GC-MS

OpenAIRE

Kaspar, Hannelore

2009-01-01

Amino acids are intermediates in cellular metabolism and their quantitative analysis plays an important role in disease diagnostics. A gas chromatography-mass spectrometry (GC-MS) based method was developed for the quantitative analysis of free amino acids as their propyl chloroformate derivatives in biological fluids. Derivatization with propyl chloroformate could be carried out directly in the biological samples without prior protein precipitation or solid-phase extraction of the amino acid...

Desenvolvimento e validação de método analítico para quantificação de diclofenaco de dietilamônio em pele humana por cromatografia líquida de alta eficiência

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JOSé ALEXSANDRO SILVA

2010-06-01

Full Text Available Foi desenvolvido e validado neste estudo um método analítico para quantificação de diclofenaco de dietilamônio em pele humana por cromatografia líquida de alta eficiência, segundo a Resolução 899/2003 da Agência Nacional de Vigilância Sanitária (ANVISA. Empregou-se cromatografia em fase reversa com coluna C18 150 x 4,6 mm, 5 µm Shimpack®, à temperatura de 40 ºC e fase móvel, constituída por mistura de acetonitrila e tampão fosfato de sódio 20 mM pH 3,0 (70:30, v/v com fluxo de 1,2 mL min-1. Os analitos foram detectados por UV a 280 nm e o método foi especifico, preciso, exato, robusto e linear no intervalo de 0,05 a 20 µg mL-1 (R2 = 0,998, mostrando que pode ser utilizado em estudos de penetração cutânea in vitro tendo como modelo de membrana a pele humana. Palavras-chave: Diclofenaco dietilamônio. Retenção cutânea. Validação. ABSTRACT Development and validation of an analytical method for quantitation of diclofenac diethylamine in human skin by high performance liquid chromatography An analytical method has been developed and validated for the quantitation of diclofenac diethylamine (DDA in human skin by high performance liquid chromatography (HPLC, in accordance with Regulation 899/2003 of the National Sanitary Surveillance Agency (ANVISA. The HPLC column was a reversed-phase Shimpack® C18, with a 5 µm particle bed, measuring 150 x 4.6 mm i.d., eluted isocratically at 40C with 20 mM sodium phosphate buffer (pH 3.0:acetonitrile (30:70, v/v, the mobile phase flowing at 1.2 mL min-1. Analytes were measured by a UV detector set at 280 nm. The results revealed that the method was specific, precise, accurate, robust and linear (R2=0.998 in the range from 0.05 to 20 µg mL-1. Therefore, it can safely be used to assess DDA in vitro penetration of human skin in kinetic studies. Keywords: Diclofenac diethylamine. Human skin retention. Validation.

PHYTOCHEMICAL ASSESSMENT ON N-HEXANE EXTRACT AND FRACTIONS OF Marsilea crenata Presl. LEAVES THROUGH GC-MS

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Burhan Ma'arif

2016-08-01

Full Text Available Estrogen deficiency causes various health problems in postmenopausal women, including osteoporosis. Phytoestrogen emerged as a potential alternative of estrogen with minimum side effects. Green clover (Marsilea crenata Presl. is a typical plant in East Java which suspected contains estrogen-like substances. The aim of this research was to report the phytochemical properties of M. crenata using GC-MS as a preliminary study. M. crenata leaves were dried and extracted with n-hexane, then separated using vacuum column chromatography to get four fractions, after that the n-hexane extract and four fractions were identified with GC-MS. The results of GC-MS analysis showed some compounds contained in M. crenata leaves like monoterpenoid, diterpenoid, fatty acid compounds, and other unknown compounds. The results obtained in this research indicated a promising potential of M. crenata as medicinal plants, especially as antiosteoporotic agent.

A fast and simple GC MS method for lignan profiling in Anthriscus sylvestris and biosynthetically related plant species

NARCIS (Netherlands)

Koulman, A; Bos, R; Medarde, M; Pras, N; Quax, WJ

2001-01-01

A new GC-MS method for monitoring lignans was developed to study the variation in plants and elucidate the biosynthetic steps. A simple and fast extraction procedure for lyophilised plant material was developed, giving a lignan-rich extract. A GC-MS method was set up using an apolar WCOT fused

GC – MS Characterization of Degutted White Grubs' Fatty Acids ...

African Journals Online (AJOL)

Fatty acids composition of white grubs examined by GC- MS identified 19 different fatty acids; 11 saturated, 7 monoene and a cyclopropaneoctanoate. The identified ones are Methyl tetradecanoate (C14:0), Methyl dodecanoate (C12:0), Methyl cis – 9 - octadecenote (C18:1), Methyl(7E) – 7 – hexadecenoate (C16:1), Methyl ...

Compound Heterozygosity for Hb Alperton (HBB: c.407C>T) and IVS-I-5 (G>C) (HBB: c.92+5G>C) Mutations Presenting as a Moderate Anemia in an Indian Family.

Science.gov (United States)

Godbole, Koumudi G; Ramachandran, Angelina; Karkamkar, Ashwini S; Dalal, Ashwin B

2018-04-13

While knowledge of HBB gene mutations is necessary for offering prenatal diagnosis (PND) of β-thalassemia (β-thal), a genotype-phenotype correlation may not always be available for rare variants. We present for the first time, genotype-phenotype correlation for a compound heterozygous status with IVS-I-5 (G>C) (HBB: c.92+5G>C) and HBB: c.407C>T (Hb Alperton) mutations on the HBB gene in an Indian family. Hb Alperton is a very rare hemoglobin (Hb) variant with scant published information about its clinical presentation, especially when accompanied with another HBB gene mutation. Here we provide biochemical as well as clinical details of this variant.

Detection of flavonoids in Alpinia purpurata (Vieill. K. Schum. leaves using high-performance liquid chromatography Detecção de flavonóides em folhas de Alpinia purpurata (Vieill. K. Schum. por cromatografia líquida de alta eficiência

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C.P. Victório

2009-01-01

Full Text Available The species Alpinia purpurata is scarcely cited as to ethnopharmacology and phytochemistry. This study aimed to analyze bioactive compounds through high-performance liquid chromatography (HPLC. Hydroalcoholic crude extract was obtained from A. purpurata dried leaves. Folin-Ciocalteau method was used to quantify total phenols, using gallic acid as standard. The obtained result was 15.6 mg GAE g-1. The crude extract was partitioned with the solvents ethyl acetate and butanol, followed by thin-layer chromatography (TLC and HPLC. The flavonoids kaempferol-3-O-glucuronide and rutin were detected at a higher concentration in ethyl acetate and butanolic extracts. The butanolic extract contains the highest flavonoid percentage (94.3%. A. purpurata presents important flavonoids of therapeutic use, already verified for A. zerumbet. This is the first study verifying the presence of flavonoids in A. purpurata extracts.A espécie Alpinia purpurata apresenta poucas citações referentes a etnofarmacologia e fitoquímica. Este estudo propõe a análise de substâncias bioativas através da técnica de cromatografia líquida de alta eficiência (CLAE. O extrato bruto hidroalcóolico foi obtido a partir de folhas secas de A. purpurata. A quantificação de fenóis totais foi realizada pelo método de Folin-Ciocalteau, usando ácido gálico como padrão. Como resultado, foi verificado 15,6 mg EAG g-1. O extrato bruto foi particionado com os solventes acetato de etila e butanol e depois analisado por cromatografia em camada delgada e CLAE. Nos extratos acetato de etila e butanólico foi detectada a presença dos flavonóides kaempferol-3-O-glicuronídeo e rutina, em maior concentração. O extrato butanólico contém a maior porcentagem de flavonóides (94,3%. Esta espécie possui flavonóides importantes no uso terapêutico, já antes verificados para a espécie A. zerumbet. Este é o primeiro trabalho que verifica a presença de flavonóides em extratos de A

Solid phase microextraction headspace sampling of chemical warfare agent contaminated samples : method development for GC-MS analysis

Energy Technology Data Exchange (ETDEWEB)

Jackson Lepage, C.R.; Hancock, J.R. [Defence Research and Development Canada, Medicine Hat, AB (Canada); Wyatt, H.D.M. [Regina Univ., SK (Canada)

2004-07-01

Defence R and D Canada-Suffield (DRDC-Suffield) is responsible for analyzing samples that are suspected to contain chemical warfare agents, either collected by the Canadian Forces or by first-responders in the event of a terrorist attack in Canada. The analytical techniques used to identify the composition of the samples include gas chromatography-mass spectrometry (GC-MS), liquid chromatography-mass spectrometry (LC-MS), Fourier-transform infrared spectroscopy (FT-IR) and nuclear magnetic resonance spectroscopy. GC-MS and LC-MS generally require solvent extraction and reconcentration, thereby increasing sample handling. The authors examined analytical techniques which reduce or eliminate sample manipulation. In particular, this paper presented a screening method based on solid phase microextraction (SPME) headspace sampling and GC-MS analysis for chemical warfare agents such as mustard, sarin, soman, and cyclohexyl methylphosphonofluoridate in contaminated soil samples. SPME is a method which uses small adsorbent polymer coated silica fibers that trap vaporous or liquid analytes for GC or LC analysis. Collection efficiency can be increased by adjusting sampling time and temperature. This method was tested on two real-world samples, one from excavated chemical munitions and the second from a caustic decontamination mixture. 7 refs., 2 tabs., 3 figs.

GC-MS study of Nigella sativa (seeds fatty oil

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Mehta, B. K.

2002-06-01

Full Text Available The GC-MS study of N. sativa (seeds fatty oil revealed the presence of 26 compounds which were identified as methyl hept-6-enoate,1-phenylhepta-2,4-dione, pentadecane, hexadec-1-ene, 1-phenyldecan-2-one, octadec-1-ene, octadecane, methyl pentadecanoate, bis(3-chlorophenyl ketone, diethyl phthalate, ethyl octadec-7-enoate, methyl octadecanoate, tricos-9-ene, octadeca-9,12-dienoic acid, hexadecanoic acid, methyl hexadecanoate, methyl octadec-15-enoate, henicosan-10-one, 2-methyl octadecanoic acid, docos-1-ene, ethyl octadecanoate, methyl octadecanoate, pentacos-5-ene,12-methyltricosane, dibutyl phthalate and 2-methyltetracosane.El estudio por GC-MS del aceite de la semilla de Nigella sativa reveló la presencia de 26 compuestos los cuales fueron identificados como: hept-6-enoato de metilo, 1-fenilhepta-2,4-diona, pentadecano, hexadec-1-eno, 1-fenildecan-2-ona, octadec-1-eno, octadecano, pentadecanoato de metilo, bis(3-clorofenil cetona, ftalato de dietilo, octadec-7-enoato de etilo, octadecanoato de metilo, tricos-9-eno, ácido octadeca-9,12-dienoico, ácido hexadecanoico, hexadecanoato de metilo, octadec-15-enoato de metilo, henicosan-10-ona, ácido 2-metil octadecanoico, docos-1-eno, octadecanoato de etilo, octadecanoato de metilo, pentacos-5-eno, 12-metiltricosano, ftalato de dibutilo y 2-metiltetracosano.

Origin Discrimination of Osmanthus fragrans var. thunbergii Flowers using GC-MS and UPLC-PDA Combined with Multivariable Analysis Methods.

Science.gov (United States)

Zhou, Fei; Zhao, Yajing; Peng, Jiyu; Jiang, Yirong; Li, Maiquan; Jiang, Yuan; Lu, Baiyi

2017-07-01

Osmanthus fragrans flowers are used as folk medicine and additives for teas, beverages and foods. The metabolites of O. fragrans flowers from different geographical origins were inconsistent in some extent. Chromatography and mass spectrometry combined with multivariable analysis methods provides an approach for discriminating the origin of O. fragrans flowers. To discriminate the Osmanthus fragrans var. thunbergii flowers from different origins with the identified metabolites. GC-MS and UPLC-PDA were conducted to analyse the metabolites in O. fragrans var. thunbergii flowers (in total 150 samples). Principal component analysis (PCA), soft independent modelling of class analogy analysis (SIMCA) and random forest (RF) analysis were applied to group the GC-MS and UPLC-PDA data. GC-MS identified 32 compounds common to all samples while UPLC-PDA/QTOF-MS identified 16 common compounds. PCA of the UPLC-PDA data generated a better clustering than PCA of the GC-MS data. Ten metabolites (six from GC-MS and four from UPLC-PDA) were selected as effective compounds for discrimination by PCA loadings. SIMCA and RF analysis were used to build classification models, and the RF model, based on the four effective compounds (caffeic acid derivative, acteoside, ligustroside and compound 15), yielded better results with the classification rate of 100% in the calibration set and 97.8% in the prediction set. GC-MS and UPLC-PDA combined with multivariable analysis methods can discriminate the origin of Osmanthus fragrans var. thunbergii flowers. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

Quantitative analysis of replication-related mutation and selection pressures in bacterial chromosomes and plasmids using generalised GC skew index

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Suzuki Haruo

2009-12-01

Full Text Available Abstract Background Due to their bi-directional replication machinery starting from a single finite origin, bacterial genomes show characteristic nucleotide compositional bias between the two replichores, which can be visualised through GC skew or (C-G/(C+G. Although this polarisation is used for computational prediction of replication origins in many bacterial genomes, the degree of GC skew visibility varies widely among different species, necessitating a quantitative measurement of GC skew strength in order to provide confidence measures for GC skew-based predictions of replication origins. Results Here we discuss a quantitative index for the measurement of GC skew strength, named the generalised GC skew index (gGCSI, which is applicable to genomes of any length, including bacterial chromosomes and plasmids. We demonstrate that gGCSI is independent of the window size and can thus be used to compare genomes with different sizes, such as bacterial chromosomes and plasmids. It can suggest the existence of different replication mechanisms in archaea and of rolling-circle replication in plasmids. Correlation of gGCSI values between plasmids and their corresponding host chromosomes suggests that within the same strain, these replicons have reproduced using the same replication machinery and thus exhibit similar strengths of replication strand skew. Conclusions gGCSI can be applied to genomes of any length and thus allows comparative study of replication-related mutation and selection pressures in genomes of different lengths such as bacterial chromosomes and plasmids. Using gGCSI, we showed that replication-related mutation or selection pressure is similar for replicons with similar machinery.

Pràctiques de tècniques instrumentals separatives (Curs 2012/2013)

OpenAIRE

Maicas i Prieto, Sergi

2013-01-01

El quadernet forma part dels materials docents programats mitjançant l'ajut del Servei de Política Lingüística de la Universitat de València. Cromatografia. La cromatografia en paper és una tècnica analítica que s’utilitza per a la separació i la identificació de mescles que són, o poden ser, de color. Aquest mètode ha estat substituït en gran mesura per la cromatografia de capa fina. Tanmateix, continua sent una poderosa eina per l’ensenyament. En algunes ocasions es realitzen cromatograf...

Probing π-π stacking modulation of g-C3N4/graphene heterojunctions and corresponding role of graphene on photocatalytic activity.

Science.gov (United States)

Ma, Xinguo; Wei, Yang; Wei, Zhen; He, Hua; Huang, Chuyun; Zhu, Yongfa

2017-12-15

The photoelectrochemical properties of g-C 3 N 4 sheet are modified by the π-π stacking interaction with graphene, and the corresponding role of graphene on the surface chemical reactions is investigated by density functional theory. The calculated cohesive energies and the lattice mismatch energies indicate that g-C 3 N 4 and graphene are in parallel contact and can form a stable heterojunction. According to our calculated energy band structures and work functions of g-C 3 N 4 /graphene heterojunctions, the band edge modulations by graphene are discussed and corresponding photoinduced charge transfer processes are analyzed in detail. It is found that the incorporating of graphene into g-C 3 N 4 facilitates the separation of photoinduced e - /h + pairs and the oxidation capacity enhancement of the photoinduced holes with the downshifting of the valence band edge of g-C 3 N 4 layer. It is identified that the inhomogeneous onsite energies between interlayer and the band edge modulations are induced by the inhomogeneous charge redistribution between interlayer caused by graphene. Further, the initial dynamic reaction processes of oxygen atoms in g-C 3 N 4 /graphene heterojunctions also confirm the significant role of graphene on the surface chemical reactions. Copyright © 2017 Elsevier Inc. All rights reserved.

High-performance for hydrogen evolution and pollutant degradation of reduced graphene oxide/two-phase g-C3N4 heterojunction photocatalysts.

Science.gov (United States)

Song, Chengjie; Fan, Mingshan; Shi, Weidong; Wang, Wei

2018-05-01

We have successfully synthesized the composites of two-phase g-C 3 N 4 heterojunction photocatalysts by one-step method. And the reduced graphene oxide/two-phase g-C 3 N 4 heterojunction photocatalyst was fabricated via a facile hydrothermal reduction method. The characterization results indicated that the two-phase g-C 3 N 4 was integrated closely, and the common phenomenon of agglomeration for g-C 3 N 4 was significantly reduced. Moreover, the oxidized graphene was reduced successfully in the composites and the graphene was overlaid on the surface or the interlayers of g-C 3 N 4 heterojunction composite uniformly. In addition, we have carried out the photocatalytic activity experiments by H 2 evolution and rhodamine B removal, tetracycline removal under the visible light irradiation. The results revealed that the composite has improved the separation efficiency a lot than the pure photocatalyst. The photocurrent test demonstrated that the recombination of electrons and holes were efficiently inhibited as well as enhanced the photocatalytic activity. The 0.4% rGO loaded samples, 0.4% rGOCN2, own the best performance. Its rate of H 2 evolution was 15 times as high as that of the pure g-C 3 N 4 .

The GC computer code for flow sheet simulation of pyrochemical processing of spent nuclear fuels

International Nuclear Information System (INIS)

Ahluwalia, R.K.; Geyer, H.K.

1996-01-01

The GC computer code has been developed for flow sheet simulation of pyrochemical processing of spent nuclear fuel. It utilizes a robust algorithm SLG for analyzing simultaneous chemical reactions between species distributed across many phases. Models have been developed for analysis of the oxide fuel reduction process, salt recovery by electrochemical decomposition of lithium oxide, uranium separation from the reduced fuel by electrorefining, and extraction of fission products into liquid cadmium. The versatility of GC is demonstrated by applying the code to a flow sheet of current interest

HS-SPME-GC-MS Analysis of onion (Allium cepa L. and shallot (Allium ascalonicum L.

Directory of Open Access Journals (Sweden)

D’Auria, M.

2017-06-01

Full Text Available The volatile organic compounds of onion and shallot were determined via HS-SPME-GC-MS. The main components were dipropyldisulphide and allylpropyldisulphide. Thiopropanal S-oxide were detected only in onion volatiles. In shallot is interesting the presence of 2-methyl-2-pentenal, a compound with an intense fruity aroma, that can characterize the different aroma between onion and shallot. The SPME-GC-MS analysis of shallot after absorption on the SPME fiber at 50°C showed the presence of new compounds, whose structures have been discussed.

GC/MS analysis of coal tar composition produced from coal pyrolysis

African Journals Online (AJOL)

Coal tar is a significant product generated from coal pyrolysis. A detailed analytical study on its composition and chemical structure will be of great advantage to its further processing and utilization. Using a combined method of planigraphy-gas chromatograph/mass spectroscopy (GC/MS), this work presents a composition ...

PyMS: a Python toolkit for processing of gas chromatography-mass spectrometry (GC-MS data. Application and comparative study of selected tools

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O'Callaghan Sean

2012-05-01

Full Text Available Abstract Background Gas chromatography–mass spectrometry (GC-MS is a technique frequently used in targeted and non-targeted measurements of metabolites. Most existing software tools for processing of raw instrument GC-MS data tightly integrate data processing methods with graphical user interface facilitating interactive data processing. While interactive processing remains critically important in GC-MS applications, high-throughput studies increasingly dictate the need for command line tools, suitable for scripting of high-throughput, customized processing pipelines. Results PyMS comprises a library of functions for processing of instrument GC-MS data developed in Python. PyMS currently provides a complete set of GC-MS processing functions, including reading of standard data formats (ANDI- MS/NetCDF and JCAMP-DX, noise smoothing, baseline correction, peak detection, peak deconvolution, peak integration, and peak alignment by dynamic programming. A novel common ion single quantitation algorithm allows automated, accurate quantitation of GC-MS electron impact (EI fragmentation spectra when a large number of experiments are being analyzed. PyMS implements parallel processing for by-row and by-column data processing tasks based on Message Passing Interface (MPI, allowing processing to scale on multiple CPUs in distributed computing environments. A set of specifically designed experiments was performed in-house and used to comparatively evaluate the performance of PyMS and three widely used software packages for GC-MS data processing (AMDIS, AnalyzerPro, and XCMS. Conclusions PyMS is a novel software package for the processing of raw GC-MS data, particularly suitable for scripting of customized processing pipelines and for data processing in batch mode. PyMS provides limited graphical capabilities and can be used both for routine data processing and interactive/exploratory data analysis. In real-life GC-MS data processing scenarios PyMS performs

Inhibition of the Hantavirus Fusion Process by Predicted Domain III and Stem Peptides from Glycoprotein Gc.

Science.gov (United States)

Barriga, Gonzalo P; Villalón-Letelier, Fernando; Márquez, Chantal L; Bignon, Eduardo A; Acuña, Rodrigo; Ross, Breyan H; Monasterio, Octavio; Mardones, Gonzalo A; Vidal, Simon E; Tischler, Nicole D

2016-07-01

Hantaviruses can cause hantavirus pulmonary syndrome or hemorrhagic fever with renal syndrome in humans. To enter cells, hantaviruses fuse their envelope membrane with host cell membranes. Previously, we have shown that the Gc envelope glycoprotein is the viral fusion protein sharing characteristics with class II fusion proteins. The ectodomain of class II fusion proteins is composed of three domains connected by a stem region to a transmembrane anchor in the viral envelope. These fusion proteins can be inhibited through exogenous fusion protein fragments spanning domain III (DIII) and the stem region. Such fragments are thought to interact with the core of the fusion protein trimer during the transition from its pre-fusion to its post-fusion conformation. Based on our previous homology model structure for Gc from Andes hantavirus (ANDV), here we predicted and generated recombinant DIII and stem peptides to test whether these fragments inhibit hantavirus membrane fusion and cell entry. Recombinant ANDV DIII was soluble, presented disulfide bridges and beta-sheet secondary structure, supporting the in silico model. Using DIII and the C-terminal part of the stem region, the infection of cells by ANDV was blocked up to 60% when fusion of ANDV occurred within the endosomal route, and up to 95% when fusion occurred with the plasma membrane. Furthermore, the fragments impaired ANDV glycoprotein-mediated cell-cell fusion, and cross-inhibited the fusion mediated by the glycoproteins from Puumala virus (PUUV). The Gc fragments interfered in ANDV cell entry by preventing membrane hemifusion and pore formation, retaining Gc in a non-resistant homotrimer stage, as described for DIII and stem peptide inhibitors of class II fusion proteins. Collectively, our results demonstrate that hantavirus Gc shares not only structural, but also mechanistic similarity with class II viral fusion proteins, and will hopefully help in developing novel therapeutic strategies against hantaviruses.

A novel assay of DGAT activity based on high temperature GC/MS of triacylglycerol.

Science.gov (United States)

Greer, Michael S; Zhou, Ting; Weselake, Randall J

2014-08-01

Diacylglycerol acyltransferase (DGAT) catalyzes the final step in the acyl-CoA-dependent biosynthesis of triacylglycerol (TAG), a high-energy compound composed of three fatty acids esterified to a glycerol backbone. In vitro DGAT assays, which are usually conducted with radiolabeled substrate using microsomal fractions, have been useful in identifying compounds and genetic modifications that affect DGAT activity. Here, we describe a high-temperature gas chromatography (GC)/mass spectrometry (MS)-based method for monitoring molecular species of TAG produced by the catalytic action of microsomal DGAT. This method circumvents the need for radiolabeled or modified substrates, and only requires a simple lipid extraction prior to GC. The utility of the method is demonstrated using a recombinant type-1 Brassica napus DGAT produced in a strain of Saccharomyces cerevisae that is deficient in TAG synthesis. The GC/MS-based assay of DGAT activity was strongly correlated with the typical in vitro assay of the enzyme using [1-(14)C] acyl-CoA as an acyl donor. In addition to determining DGAT activity, the method is also useful for determining substrate specificity and selectivity properties of the enzyme.

Total OH reactivity measurements using a new fast Gas Chromatographic Photo-Ionization Detector (GC-PID

Directory of Open Access Journals (Sweden)

V. Sinha

2012-12-01

Full Text Available The primary and most important oxidant in the atmosphere is the hydroxyl radical (OH. Currently OH sinks, particularly gas phase reactions, are poorly constrained. One way to characterize the overall sink of OH is to measure directly the ambient loss rate of OH, the total OH reactivity. To date, direct measurements of total OH reactivity have been either performed using a Laser-Induced Fluorescence (LIF system ("pump-and-probe" or "flow reactor" or the Comparative Reactivity Method (CRM with a Proton-Transfer-Reaction Mass Spectrometer (PTR-MS. Both techniques require large, complex and expensive detection systems. This study presents a feasibility assessment for CRM total OH reactivity measurements using a new detector, a Gas Chromatographic Photoionization Detector (GC-PID. Such a system is smaller, more portable, less power consuming and less expensive than other total OH reactivity measurement techniques.

Total OH reactivity is measured by the CRM using a competitive reaction between a reagent (here pyrrole with OH alone and in the presence of atmospheric reactive molecules. The new CRM method for total OH reactivity has been tested with parallel measurements of the GC-PID and the previously validated PTR-MS as detector for the reagent pyrrole during laboratory experiments, plant chamber and boreal field studies. Excellent agreement of both detectors was found when the GC-PID was operated under optimum conditions. Time resolution (60–70 s, sensitivity (LOD 3–6 s⁻¹ and overall uncertainty (25% in optimum conditions for total OH reactivity were similar to PTR-MS based total OH reactivity measurements. One drawback of the GC-PID system was the steady loss of sensitivity and accuracy during intensive measurements lasting several weeks, and a possible toluene interference. Generally, the GC-PID system has been shown to produce closely comparable results to the PTR-MS and thus in suitable environments (e.g. forests it

Quantificação de sulfonamidas em leite por cromatografia líquida de alta eficiência via azoderivados Sulfonamides quantification in milk by high performace liquid chromatography via azoderivatives

Directory of Open Access Journals (Sweden)

Marcelo Volpatto Marques

2008-12-01

Full Text Available O objetivo deste trabalho foi avaliar uma alternativa para a quantificação simultânea de sulfatiazol, sulfametazina e sulfadimetoxina no leite, na forma de azoderivados, por meio de cromatografia líquida de alta eficiência (CLAE. O isolamento e concentração das sulfas foram conduzidos por extração em fase sólida (C18, com metanol como eluente. Após a extração, os analitos foram transformados em sais de diazônio e submetidos ao acoplamento com resorcinol. Os derivados foram separados e quantificados por CLAE (coluna C8, λ = 430 nm, MeOH/KH2PO4 aq.. Foram obtidas recuperações entre 65 e 78%.The objective of this work was to evaluate an analytical method for the simultaneous measurement of sulfathiazole, sulfamethazine, and sulfadimethoxine in milk, in the form of azoderivatives, through the high performance liquid chromatography (HPLC. The isolation and concentration of sulfas were carried out by solid phase extraction (C18 with methanol as eluent. After extraction, analytes were transformed in diazonium salts and coupled with resorcinol. Derivatives were quantified by HPLC (C8 column, λ = 430 nm, MeOH/KH2PO4 aq. Recoveries were obtainedbetween 65 and 78%.

An efficient top-down approach for the fabrication of large-aspect-ratio g-C3N4 nanosheets with enhanced photocatalytic activities.

Science.gov (United States)

Tong, Jincheng; Zhang, Li; Li, Fei; Li, Mingming; Cao, Shaokui

2015-09-28

Graphitic carbon nitride (g-C3N4) nanosheets with large aspect ratios were fabricated from bulk g-C3N4 through an efficient top-down approach of moderate disintegration-exfoliation using diluted H2SO4 as an "efficient knife". By prior disintegration in a diluted H2SO4 solution, the exfoliation of bulk g-C3N4 was effectively accelerated. The as-prepared g-C3N4 nanosheets possess a two-dimensional (2D) thin-layer structure with seven-atom thickness, a large lateral size of about 1 μm, and a high specific surface area of 80 m(2) g(-1). Compared with the bulk precursor, the g-C3N4 nanosheets showed much higher efficiency of photogenerated charge transfer and separation, and consequently exhibited enhanced photocatalytic activity toward hydrogen evolution and pollutant decomposition under both full-sunlight and visible-light irradiation.

Effects of GC temperature and carrier gas flow rate on on-line oxygen isotope measurement as studied by on-column CO injection.

Science.gov (United States)

Chen, Zhi-Gang; Yin, Xi-Jie; Zhou, Youping

2015-08-01

Although deemed important to δ 18 O measurement by on-line high-temperature conversion techniques, how the GC conditions affect δ 18 O measurement is rarely examined adequately. We therefore directly injected different volumes of CO or CO-N 2 mix onto the GC column by a six-port valve and examined the CO yield, CO peak shape, CO-N 2 separation, and δ 18 O value under different GC temperatures and carrier gas flow rates. The results show the CO peak area decreases when the carrier gas flow rate increases. The GC temperature has no effect on peak area. The peak width increases with the increase of CO injection volume but decreases with the increase of GC temperature and carrier gas flow rate. The peak intensity increases with the increase of GC temperature and CO injection volume but decreases with the increase of carrier gas flow rate. The peak separation time between N 2 and CO decreases with an increase of GC temperature and carrier gas flow rate. δ 18 O value decreases with the increase of CO injection volume (when half m/z 28 intensity is rate. On average, the δ 18 O value of the injected CO is about 1‰ higher than that of identical reference CO. The δ 18 O distribution pattern of the injected CO is probably a combined result of ion source nonlinearity and preferential loss of C 16 O or oxygen isotopic exchange between zeolite and CO. For practical application, a lower carrier gas flow rate is therefore recommended as it has the combined advantages of higher CO yield, better N 2 -CO separation, lower He consumption, and insignificant effect on δ 18 O value, while a higher-than-60 °C GC temperature and a larger-than-100 µl CO volume is also recommended. When no N 2 peak is expected, a higher GC temperature is recommended, and vice versa. Copyright © 2015 John Wiley & Sons, Ltd. Copyright © 2015 John Wiley & Sons, Ltd.

GC-MS Analysis of Insecticidal Essential Oil of Aerial Parts of ...

African Journals Online (AJOL)

Methods: Steam distillation of the aerial parts of P. scandens was carried out using Clavenger apparatus in order to obtain the volatile oils. Gas chromatography/mass spectrometric (GC/MS) analyses (HP-5MS column) of the essential oil were performed and its composition determined. Insecticidal activity of the essential oil ...

GC-MS Quantitation and Identification of Bisphenol-A Isolated from Water

Science.gov (United States)

Mead, Ralph N.; Seaton, Pamela J.

2011-01-01

Isolation and identification of organic compounds is a necessary skill chemistry students must be able to do with proficiency. In this upper-level undergraduate laboratory, students isolate bisphenol-A (BPA; 4-4'-isopropylidenediphenol) from water using solid-phase extraction (SPE) followed by derivatization with analysis by GC-MS. The students…

Compressible and Recyclable Monolithic g-C3N4/Melamine Sponge: A Facile Ultrasonic-coating Approach and Enhanced Visible-light Photocatalytic Activity

Science.gov (United States)

Yang, Ye; Zhang, Qian; Zhang, Ruiyang; Ran, Tao; Wan, Wenchao; Zhou, Ying

2018-05-01

Powdery photocatalysts seriously restrict their practical application due to the difficult recycle and low photocatalytic activity. In this work, a monolithic g-C3N4/melamine sponge (g-C3N4/MS) was successfully fabricated by a cost-effective ultrasonic-coating route, which is easy to achieve the uniform dispersion and firm loading of g-C3N4 on MS skeleton. The monolithic g-C3N4/MS entirely inherits the porous structure of MS and results in a larger specific surface area (SSA) than its powdery counterpart. Benefit from this monolithic structure, g-C3N4/MS gains more exposed active sites, enhanced visible-light absorption and separation of photogenerated carriers, thus achieving noticeable photocatalytic activity on nitric oxide (NO) removal, rhodamine B (RhB) degradation and CO2 reduction. Specifically, NO removal ratio is as high as 78.6% which is 4.5 times higher than that of the powdery g-C3N4, while RhB degradation rate reaches 97.88%, and yield rate of CO and CH4 attains 7.48 and 3.93 μmol g-1 h-1. Importantly, the features of low-density, high porosity, good elasticity and firmness, not only endow g-C3N4/MS with flexibility in various environmental applications, but also make it easy to recycle and stable for long-time application. Our work provides a feasible approach to fabricate novel monolithic photocatalysts with large-scale production and application.

One-pot synthesis of K-doped g-C3N4 nanosheets with enhanced photocatalytic hydrogen production under visible-light irradiation

Science.gov (United States)

Wang, Yanyun; Zhao, Shuo; Zhang, Yiwei; Fang, Jiasheng; Zhou, Yuming; Yuan, Shenhao; Zhang, Chao; Chen, Wenxia

2018-05-01

Graphite carbon nitride (g-C3N4), as a promising low cost, visible light driven conjugated polymer semiconductor photocatalyst, has attracted wide attentions from researchers. However, low light absorption efficiency and inadequate charge separation limit the potential applications of g-C3N4. This paper exhibits K-doped g-C3N4 prepared by a facile thermal polymerization with KBr as the K source. The experiments of photocatalytic hydrogen evolution demonstrate that KBr content strongly affects the activity of the catalyst. XRD, FT-IR, XPS, SEM, TEM, UV-vis diffuse reflectance spectra, photoluminescence (PL) characterization methods are used to study the effects of potassium on the catalyst performance. The results find that K-modified g-C3N4 has a narrower band gap and enhanced light harvesting properties. Moreover, the photocatalytic hydrogen evolution rate (HER) of the optimized K-doped g-C3N4 nanosheets (10 wt % KBr) reaches 1337.2 μmol g-1h-1, which is about 5.6 times in comparison with that of pure g-C3N4 (239.8 μmol g-1h-1). The doping of the potassium may increase the π-conjugated systems and accelerate the electron transport rate, then improve the photocatalytic properties. Based on the results of the analysis, a possible mechanism is proposed.

NO-sGC Pathway Modulates Ca2+ Release and Muscle Contraction in Zebrafish Skeletal Muscle.

Science.gov (United States)

Xiyuan, Zhou; Fink, Rainer H A; Mosqueira, Matias

2017-01-01

Vertebrate skeletal muscle contraction and relaxation is a complex process that depends on Ca 2+ ions to promote the interaction of actin and myosin. This process can be modulated by nitric oxide (NO), a gas molecule synthesized endogenously by (nitric oxide synthase) NOS isoforms. At nanomolar concentrations NO activates soluble guanylate cyclase (sGC), which in turn activates protein kinase G via conversion of GTP into cyclic GMP. Alternatively, NO post-translationally modifies proteins via S-nitrosylation of the thiol group of cysteine. However, the mechanisms of action of NO on Ca 2+ homeostasis during muscle contraction are not fully understood and we hypothesize that NO exerts its effects on Ca 2+ homeostasis in skeletal muscles mainly through negative modulation of Ca 2+ release and Ca 2+ uptake via the NO-sGC-PKG pathway. To address this, we used 5-7 days-post fecundation-larvae of zebrafish, a well-established animal model for physiological and pathophysiological muscle activity. We evaluated the response of muscle contraction and Ca 2+ transients in presence of SNAP, a NO-donor, or L-NAME, an unspecific NOS blocker in combination with specific blockers of key proteins of Ca 2+ homeostasis. We also evaluate the expression of NOS in combination with dihydropteridine receptor, ryanodine receptor and sarco/endoplasmic reticulum Ca 2+ ATPase. We concluded that endogenous NO reduced force production through negative modulation of Ca 2+ transients via the NO-sGC pathway. This effect could be reversed using an unspecific NOS blocker or sGC blocker.

Miniature GC-Minicell Ion Mobility Spectrometer (IMS) for In Situ Measurements in Astrobiology Planetary Missions

Science.gov (United States)

Kojiro, Daniel R.; Stimac, Robert M.; Kaye, William J.; Holland, Paul M.; Takeuchi, Norishige

2006-01-01

Astrobiology flight experiments require highly sensitive instrumentation for in situ analysis of volatile chemical species and minerals present in the atmospheres and surfaces of planets, moons, and asteroids. The complex mixtures encountered place a heavy burden on the analytical instrumentation to detect and identify all species present. The use of land rovers and balloon aero-rovers place additional emphasis on miniaturization of the analytical instrumentation. In addition, smaller instruments, using tiny amounts of consumables, allow the use of more instrumentation and/or ionger mission life for stationary landers/laboratories. The miniCometary Ice and Dust Experiment (miniCIDEX), which combined Gas Chromatography (GC) with helium Ion Mobility Spectrometry (IMS), was capable of providing the wide range of analytical information required for Astrobiology missions. The IMS used here was based on the PCP model 111 IMS. A similar system, the Titan Ice and Dust Experiment (TIDE), was proposed as part of the Titan Orbiter Aerorover Mission (TOAM). Newer GC systems employing Micro Electro- Mechanical System (MEMS) based technology have greatly reduced both the size and resource requirements for space GCs. These smaller GCs, as well as the continuing miniaturization of Astrobiology analytical instruments in general, has highlighted the need for smaller, dry helium IMS systems. We describe here the development of a miniature, MEMS GC-IMS system (MEMS GC developed by Thorleaf Research Inc.), employing the MiniCell Ion Mobility Spectrometer (IMS), from Ion Applications Inc., developed through NASA's Astrobiology Science and Technology Instrument Development (ASTID) Program and NASA s Small Business Innovative Research (SBIR) Program.

Characterization of ion processes in a GC/DMS air quality monitor by integration of the instrument to a mass spectrometer.

Science.gov (United States)

Limero, T F; Nazarov, E G; Menlyadiev, M; Eiceman, G A

2015-02-07

The air quality monitor (AQM), which included a portable gas chromatograph (GC) and a detector was interfaced to a mass spectrometer (MS) by introducing flow from the GC detector to the atmospheric pressure ion source of the MS. This small GC system, with a gas recirculation loop for carrier and detector make-up gases, comprised an inlet to preconcentrate volatile organic compounds (VOCs) in air, a thermal desorber before the GC column, a differential mobility spectrometer (DMS), and another DMS as an atmospheric pressure ionization source for the MS. Return flow to the internally recirculated air system of the AQM's DMS was replenished using purified air. Although ions and unreacted neutral vapors flowed from the detector through Viton® tubing into the source of the MS, ions were not detected in the MS without the auxillary ion source, (63)Ni as in the mobility detector. The GC-DMS-MS instrument provided a 3-D measurement platform (GC, DMS, and MS analysis) to explore the gas composition inside the GC-DMS recirculation loop and provide DMS-MS measurement of the components of a complex VOC mixture with performance significantly enhanced by mass-analysis, either with mass spectral scans or with an extracted ion chromatogram. This combination of a mobility spectrometer and a mass spectrometer was possible as vapors and ions are carried together through the DMS analyzer, thereby preserving the chromatographic separation efficiency. The critical benefit of this instrument concept is that all flows in and through the thoroughly integrated GC-DMS analyzer are kept intact allowing a full measure of the ion and vapor composition in the complete system. Performance has been evaluated using a synthetic air sample and a sample of airborne vapors in a laboratory. Capabilities and performance values are described using results from AQM-MS analysis of purified air, ambient air from a research laboratory in a chemistry building, and a sample of synthetic air of known composition

An automated GC-C-GC-IRMS setup to measure palaeoatmospheric δ13C-CH4, δ15N-N2O and δ18O-N2O in one ice core sample

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P. Sperlich

2013-08-01

Full Text Available Air bubbles in ice core samples represent the only opportunity to study the mixing ratio and isotopic variability of palaeoatmospheric CH4 and N2O. The highest possible precision in isotope measurements is required to maximize the resolving power for CH4 and N2O sink and source reconstructions. We present a new setup to measure δ13C-CH4, δ15N-N2O and δ18O-N2O isotope ratios in one ice core sample and with one single IRMS instrument, with a precision of 0.09, 0.6 and 0.7‰, respectively, as determined on 0.6–1.6 nmol CH4 and 0.25–0.6 nmol N2O. The isotope ratios are referenced to the VPDB scale (δ13C-CH4, the N2-air scale (δ15N-N2O and the VSMOW scale (δ18O-N2O. Ice core samples of 200–500 g are melted while the air is constantly extracted to minimize gas dissolution. A helium carrier gas flow transports the sample through the analytical system. We introduce a new gold catalyst to oxidize CO to CO2 in the air sample. CH4 and N2O are then separated from N2, O2, Ar and CO2 before they get pre-concentrated and separated by gas chromatography. A combustion unit is required for δ13C-CH4 analysis, which is equipped with a constant oxygen supply as well as a post-combustion trap and a post-combustion GC column (GC-C-GC-IRMS. The post-combustion trap and the second GC column in the GC-C-GC-IRMS combination prevent Kr and N2O interferences during the isotopic analysis of CH4-derived CO2. These steps increase the time for δ13C-CH4 measurements, which is used to measure δ15N-N2O and δ18O-N2O first and then δ13C-CH4. The analytical time is adjusted to ensure stable conditions in the ion source before each sample gas enters the IRMS, thereby improving the precision achieved for measurements of CH4 and N2O on the same IRMS. The precision of our measurements is comparable to or better than that of recently published systems. Our setup is calibrated by analysing multiple reference gases that were injected over bubble-free ice samples. We show

VOLATILE ORGANO-METALLOIDS IN BIO-SOLID MATERIALS: ANALYSIS BY VACUUM DISTILLATION-GC/MS

Science.gov (United States)

An analytical method based on vacuum distillation-gas chromatography-mass spectrometry (VD-GC-MS)was developed for determining volatile organo-metalloid contaminants in bio-solid materials. Methodperformance was evaluated for dimethylselenide (DMSe), dimethyldisel...

Gene evolutionary trajectories and GC patterns driven by recombination in Zea mays

Science.gov (United States)

Recombination occurring during meiosis is critical for creating genetic variation and plays an essential role in plant evolution. In addition to creating novel gene combinations, recombination can affect genome structure through altering GC patterns. In maize (Zea mays) and other grasses, another in...

Field Portable GC-MS Unit for Semi-Volatile Compound Analysis in Groundwater

Science.gov (United States)

2011-06-01

the size and power consumption compared to standard GC systems. These modifications to the instrument design all serve to decrease the size and...Environment Mass Spectrometry (HEMS) Conference, September 2007, Cocoa Beach, FL. USEPA. 1998. USEPA Superfund Record of Decision, Milan Army

GC-MS analysis of off-odor volatiles from irradiated pork

International Nuclear Information System (INIS)

Lin Ruotai; Geng Shengrong; Zhang Jinmu; Chen Yuxia; Liu Yangmin; Wang Liping; Wang Hong; Xu Ying; Yao Side

2007-01-01

The main compounds of off-odor volatiles from irradiated refrigerated vacuum-packaged pork were analyzed by gas chromatograph/mass spectrometer (GC-MS). The analytical results showed that the main compounds of off-odor volatiles were dimethyl disulfide, dimethyl sulfide, dimethyl trisulfide, S-methyl thioacetate, and methanethiol. It was proved that the off-odor volatile came from irradiated S-containing amino acid and thiamin. (authors)

Measurement of HDO Products Using GC-TCD: Towards Obtaining Reliable Analytical Data

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Zuas Oman

2018-03-01

Full Text Available This paper reported the method development and validation of a gas chromatography with thermal conductivity detector (GC-TCD method for the measurement of the gaseous products of hydrodeoxygenation (HDO. The method validation parameters include selectivity, precision (repeatability and reproducibility, accuracy, linearity, limit of detection (LoD, limit of quantitation (LoQ, and robustness. The results showed that the developed method was able to separate the target components (H2, CO2, CH4 and CO from their mixtures without any special sample treatment. The validated method was selective, precise, accurate, and robust. Application of the developed and validated GC-TCD method to the measurement of by-product components of HDO of bio-oil revealed a good performance with relative standard deviation (RSD less than 1.0% for all target components, implying that the process of method development and validation provides a trustworthy way of obtaining reliable analytical data.

Active and realistic passive marijuana exposure tested by three immunoassays and GC/MS in urine

International Nuclear Information System (INIS)

Mule, S.J.; Lomax, P.; Gross, S.J.

1988-01-01

Human urine samples obtained before and after active and passive exposure to marijuana were analyzed by immune kits (Roche, Amersham, and Syva) and gas chromatography/mass spectrometry (GC/MS). Seven of eight subjects were positive for the entire five-day test period with one immune kit. The latter correlated with GC/MS in 98% of the samples. Passive inhalation experiments under conditions likely to reflect realistic exposure resulted consistently in less than 10 ng/mL of cannabinoids. The 10-100-ng/mL cannabinoid concentration range essential for detection of occasional and moderate marijuana users is thus unaffected by realistic passive inhalation

Active and realistic passive marijuana exposure tested by three immunoassays and GC/MS in urine

Energy Technology Data Exchange (ETDEWEB)

Mule, S.J.; Lomax, P.; Gross, S.J.

1988-05-01

Human urine samples obtained before and after active and passive exposure to marijuana were analyzed by immune kits (Roche, Amersham, and Syva) and gas chromatography/mass spectrometry (GC/MS). Seven of eight subjects were positive for the entire five-day test period with one immune kit. The latter correlated with GC/MS in 98% of the samples. Passive inhalation experiments under conditions likely to reflect realistic exposure resulted consistently in less than 10 ng/mL of cannabinoids. The 10-100-ng/mL cannabinoid concentration range essential for detection of occasional and moderate marijuana users is thus unaffected by realistic passive inhalation.

On-line coupled LC-LC-GC for irradiation detection in complex lipid matrices

International Nuclear Information System (INIS)

Schulzki, G.; Spiegelberg, A.; Helle, N.; Boegl, K.W.; Schreiber, G.A.

1993-01-01

Since sample preparation with HPLC coupled on-line to the GC has been performed for only a few weeks in our laboratory, the results presented give a first look at what can be done by means of this technique. Even difficult samples as the described fish species, where an unequivocal identification regarding an irradiation treatment seemed to become a hopeless enterprise, could be managed. Because of the greater variety of fatty acids in fish ''new'' radiation-induced hydrocarbons were available. According to the theory of Nawar in addition to 16:2 and 17:2 hydrocarbons we have looked for in irradiated meat, further alkadienes appeared in irradiated fish, which were 14:2, 18:2 and 20:2. Analysis of the alkadiene-fraction, transferred to the GC after a two step LC clean up, resulted in an unequivocal identification of all fish samples as well as the fruits and sponge cake. For fruits and sponge cake the detection limit seems to be clearly below 0.5 kGy. It can further be lowered by increasing the amount of lipid whereas the upper limit for a certain LC column has to be determined. In contrast to these samples only qualitative results were obtained for fish. In the case of sponge cake for the first time irradiation of a component of a heat treated food was detected. Further investigations regarding reproducibility, dose dependence and detection limit have to be done. On-line coupled (LC-)LC-GC was proved to be a highly efficient method for analysis of complex samples. In contrast to off-line Florisil column chromatography only a small part of the initial lipid material is needed because the complete hydrocarbon fraction is transferred on-line to the GC. This offers the possibility to analyze even foods with a low fat content like various seafoods. Classification of the hydrocarbon fraction by a two step LC may facilitate the identification of the radiolytic products also if no mass spectrometric detection system is available. (orig./vhe)

Identification of natural indigo in historical textiles by GC-MS.

Science.gov (United States)

Degani, Laura; Riedo, Chiara; Chiantore, Oscar

2015-02-01

The possibility of successfully applying a common GC-MS procedure for identification in one step of all types of dyes from plants of unknown origin and from historical objects is particularly attractive due to the high separation efficiency of the capillary columns, the MS detection sensitivity and the reproducibility of results. In this work, GC-MS analysis, previously and successfully used for the characterization of anthraquinones, flavonoids and tannins from plant extracts and historical samples, has been tested on indigoid dyestuffs. An analytical procedure based on the silylating agent N,O-bis-(trimethylsilyl)trifluoroacetamide (BSTFA) with 1% trimethylchlorosilane (TMCS) was applied to pure molecules of indigotin and indirubin and to plant extracts of Indigofera tinctoria L. and Isatis tinctoria L. Preliminary tests have been done to establish the chromatographic conditions and the derivatization amounts most suitable for the simultaneous detection of indigoid molecules and of the other natural compounds, such as fatty acids, carboxylic acids and sugars, contained within the plant extracts. In order to assess the capacity and the sensitivity of the analytical procedure in typical archaeometric applications, wool samples dyed in the laboratory with indigo were analysed by mimicking the sample amounts typically available with historical objects. The electron ionization (EI) spectra of the main silylated derivatives of indigoid molecules obtained in this way constitute the necessary data set for the characterization of natural extracts and historical works of art. Subsequently, the procedure has been applied to historical samples for the detection of indigo and of other dyestuffs eventually contained in samples. Additional information, useful for restoration and preservation of works of art, could be also obtained on the nature of stains and smudges present on the sampled textile material. The GC-MS method turns out to be an efficient and fast analytical tool

Cytoadhesion to gC1qR through Plasmodium falciparum erythrocyte membrane protein 1 in severe malaria

DEFF Research Database (Denmark)

Magallón-Tejada, Ariel; Machevo, Sónia; Cisteró, Pau

2016-01-01

Cytoadhesion of Plasmodium falciparum infected erythrocytes to gC1qR has been associated with severe malaria, but the parasite ligand involved is currently unknown. To assess if binding to gC1qR is mediated through the P. falciparum erythrocyte membrane protein 1 (PfEMP1) family, we analyzed...

Supercritical Fluid Chromatography- A Hybrid of GC and LC

Directory of Open Access Journals (Sweden)

Kaushal K Chandrul

2010-03-01

Full Text Available

High performance specifications and unique functionality of chromatographic techniques is a demand of pharmaceutical industry and research. This leads to the origin of Supercritical Fluid Chromatography (SFC. It is a rapidly expanding analytical technique. The main feature that differentiates SFC from other chromatographic techniques is the replacement of either the liquid or gas mobile phase with a supercritical fluid mobile phase. It is considered a hybrid of GC and LC technique. High diffusion coefficient and low viscosity of supercritical fluids is responsible for high speed analysis, high efficiency and high sensitivity. Low mobile-phase flow rate, density programming and compatability with GC and LC detectors make SFC a versatile chromatographic technique in analytical research and development. It has a unique characteristic of analyzing thermo labile or non-volatile substances. This review highlights the role of supercritical fluid chromatography in the separation of polymers, thermally labile pesticides, fatty acids, metal chelates and organometallic compounds, chiral and achiral molecules, identification and analysis of polar samples, explosives, drugs of abuse and application of SFC in forensic science (fingerprinting. 

Enhanced Isotopic Ratio Outlier Analysis (IROA Peak Detection and Identification with Ultra-High Resolution GC-Orbitrap/MS: Potential Application for Investigation of Model Organism Metabolomes

Directory of Open Access Journals (Sweden)

Yunping Qiu

2018-01-01

Full Text Available Identifying non-annotated peaks may have a significant impact on the understanding of biological systems. In silico methodologies have focused on ESI LC/MS/MS for identifying non-annotated MS peaks. In this study, we employed in silico methodology to develop an Isotopic Ratio Outlier Analysis (IROA workflow using enhanced mass spectrometric data acquired with the ultra-high resolution GC-Orbitrap/MS to determine the identity of non-annotated metabolites. The higher resolution of the GC-Orbitrap/MS, together with its wide dynamic range, resulted in more IROA peak pairs detected, and increased reliability of chemical formulae generation (CFG. IROA uses two different 13C-enriched carbon sources (randomized 95% 12C and 95% 13C to produce mirror image isotopologue pairs, whose mass difference reveals the carbon chain length (n, which aids in the identification of endogenous metabolites. Accurate m/z, n, and derivatization information are obtained from our GC/MS workflow for unknown metabolite identification, and aids in silico methodologies for identifying isomeric and non-annotated metabolites. We were able to mine more mass spectral information using the same Saccharomyces cerevisiae growth protocol (Qiu et al. Anal. Chem 2016 with the ultra-high resolution GC-Orbitrap/MS, using 10% ammonia in methane as the CI reagent gas. We identified 244 IROA peaks pairs, which significantly increased IROA detection capability compared with our previous report (126 IROA peak pairs using a GC-TOF/MS machine. For 55 selected metabolites identified from matched IROA CI and EI spectra, using the GC-Orbitrap/MS vs. GC-TOF/MS, the average mass deviation for GC-Orbitrap/MS was 1.48 ppm, however, the average mass deviation was 32.2 ppm for the GC-TOF/MS machine. In summary, the higher resolution and wider dynamic range of the GC-Orbitrap/MS enabled more accurate CFG, and the coupling of accurate mass GC/MS IROA methodology with in silico fragmentation has great

Enhanced Isotopic Ratio Outlier Analysis (IROA) Peak Detection and Identification with Ultra-High Resolution GC-Orbitrap/MS: Potential Application for Investigation of Model Organism Metabolomes.

Science.gov (United States)

Qiu, Yunping; Moir, Robyn D; Willis, Ian M; Seethapathy, Suresh; Biniakewitz, Robert C; Kurland, Irwin J

2018-01-18

Identifying non-annotated peaks may have a significant impact on the understanding of biological systems. In silico methodologies have focused on ESI LC/MS/MS for identifying non-annotated MS peaks. In this study, we employed in silico methodology to develop an Isotopic Ratio Outlier Analysis (IROA) workflow using enhanced mass spectrometric data acquired with the ultra-high resolution GC-Orbitrap/MS to determine the identity of non-annotated metabolites. The higher resolution of the GC-Orbitrap/MS, together with its wide dynamic range, resulted in more IROA peak pairs detected, and increased reliability of chemical formulae generation (CFG). IROA uses two different 13 C-enriched carbon sources (randomized 95% 12 C and 95% 13 C) to produce mirror image isotopologue pairs, whose mass difference reveals the carbon chain length (n), which aids in the identification of endogenous metabolites. Accurate m/z, n, and derivatization information are obtained from our GC/MS workflow for unknown metabolite identification, and aids in silico methodologies for identifying isomeric and non-annotated metabolites. We were able to mine more mass spectral information using the same Saccharomyces cerevisiae growth protocol (Qiu et al. Anal. Chem 2016) with the ultra-high resolution GC-Orbitrap/MS, using 10% ammonia in methane as the CI reagent gas. We identified 244 IROA peaks pairs, which significantly increased IROA detection capability compared with our previous report (126 IROA peak pairs using a GC-TOF/MS machine). For 55 selected metabolites identified from matched IROA CI and EI spectra, using the GC-Orbitrap/MS vs. GC-TOF/MS, the average mass deviation for GC-Orbitrap/MS was 1.48 ppm, however, the average mass deviation was 32.2 ppm for the GC-TOF/MS machine. In summary, the higher resolution and wider dynamic range of the GC-Orbitrap/MS enabled more accurate CFG, and the coupling of accurate mass GC/MS IROA methodology with in silico fragmentation has great potential in

GC Method Validation for the Analysis of Menthol in Suppository Pharmaceutical Dosage Form

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Murad N. Abualhasan

2017-01-01

Full Text Available Menthol is widely used as a fragrance and flavor in the food and cosmetic industries. It is also used in the medical and pharmaceutical fields for its various biological effects. Gas chromatography (GC is considered to be a sensitive method for the analysis of menthol. GC chromatographic separation was developed using capillary column (VF-624 and a flame ionization detector (FID. The method was validated as per ICH guidelines for various parameters such as precision, linearity, accuracy, solution stability, robustness, limit of detection, and quantification. The tested validation parameters were found to be within acceptable limits. The method was successfully applied for the quantification of menthol in suppositories formulations. Quality control departments and official pharmacopeias can use our developed method in the analysis of menthol in pharmaceutical dosage formulation and raw material.

Fatty acid isolation by crystallization of fish oil fractioned by enzymatic hydrolysis

OpenAIRE

Padilha, Márcia Elisa da Silva; Augusto-Ruiz, Walter

2010-01-01

Este trabalho teve por objetivo estabelecer um processo para obter e caracterizar os produtos da cristalização das frações do óleo de pescado hidrolisado com lipase pancreática. A hidrólise enzimática foi realizada em 60 minutos com uma concentração de substrato de 1262 mmols, 38 °C, pH 8 e com uma concentração de extrato enzimático de 7,647 mg.mL-1. Os produtos da hidrólise foram separados por cromatografia em coluna e caracterizados por cromatografia em camada delgada e cromatografia em fas...

Questioning the role of actinfree Gc-Globulin as actin scavenger in neurodegenerative central nervous system disease: relationship to S-100B levels and blood-brain barrier function.

Science.gov (United States)

Gressner, Olav A; Schifflers, Marie-Claire; Kim, Philipp; Heuts, Leo; Lahme, Birgit; Gressner, Axel M

2009-02-01

Preliminary studies report on significantly higher levels of the major cytoskeleton protein actin in CSF of patients with neurodegenerative conditions and that the dynamics of these levels obviously correlates with disease progression and clinical disability. One of the primary functions of actinfree Gc-Globulin is to bind and neutralize extracellular monomeric actin, released into the circulation by necrotic or ruptured cells, and thus ameliorating the clinical outcome in situations of severe organ damage. This is the first study to investigate actinfree Gc-Globulin and S100-B levels (as reliable marker of neurodegeneration) in paired CSF and serum samples of patients with multietiological CNS diseases. 42% of all patients with CNS disease displayed serum concentrations of actinfree Gc-Globulin above the established reference range. CSF concentrations of actinfree Gc-Globulin and S100-B were positively correlated with the severity of blood-brain barrier (BBB) dysfunction. Furthermore, patients with severe BBB dysfunction presented a higher percentage of intrathecal synthesis of actinfree Gc-Globulin compared to patients with mild to moderate dysfunction and to patients with normal BBB function. Representative longitudinal data from selected patients demonstrated an inverse behaviour of actinfree Gc-Globulin and S100-B CSF concentrations, suggesting a consumption of the actin scavenger capacity of Gc-Globulin in times of increased neuronal damage. This presumption was supported by the fact that those conditions associated with a severe neuronal damage, in particular CNS trauma, and highest S100-B concentrations simultaneously displayed lowest actinfree Gc-Globulin levels, and thus residual actin binding capacity of Gc-Globulin. In summary, our data propose a function of actinfree Gc-Globulin also in the clearance of actin filaments from CSF of patients with neuronal damage. However, active recruitment of hepatic derived actinfree Gc-Globulin to the site of CNS

Evaluation of immunogenicity and safety of the new tetanus-reduced diphtheria (Td) vaccines (GC1107) in healthy Korean adolescents: a phase II, double-blind, randomized, multicenter clinical trial.

Science.gov (United States)

Rhim, Jung-Woo; Lee, Kyung-Yil; Kim, Sang-Yong; Kim, Jong-Hyun; Kim, Hyun-Hee; Kim, Hwang Min; Choi, Young-Youn; Ma, Sang-Hyuk; Kim, Dong-Ho; Ahn, Dong Ho; Kang, Jin-Han

2013-04-01

This phase II clinical trial was conducted to compare the immunogenicity and safety of a newly developed tetanus-reduced diphtheria (Td) vaccine (GC1107-T5.0 and GC1107-T7.5) and control vaccine. This study was also performed to select the proper dose of tetanus toxoid in the new Td vaccines. Healthy adolescents aged between 11 and 12 yr participated in this study. A total of 130 subjects (44 GC1107-T5.0, 42 GC1107-T7.5 and 44 control vaccine) completed a single dose of vaccination. Blood samples were collected from the subjects before and 4 weeks after the vaccination. In this study, all subjects (100%) in both GC1107-T5.0 and GC1107-T7.5 groups showed seroprotective antibody levels (≥ 0.1 U/mL) against diphtheria or tetanus toxoids. After the vaccination, the geometric mean titer (GMT) against diphtheria was significantly higher in Group GC1107-T5.0 (6.53) and GC1107-T7.5 (6.11) than in the control group (3.96). The GMT against tetanus was 18.6 in Group GC1107-T5.0, 19.94 in GC1107-T7.5 and 19.01 in the control group after the vaccination. In this study, the rates of local adverse reactions were 67.3% and 59.1% in GC1107-T5.0 and GC1107-7.5, respectively. No significant differences in the number of adverse reactions, prevalence and degree of severity of the solicited and unsolicited adverse reactions were observed among the three groups. Thus, both newly developed Td vaccines appear to be safe and show good immunogenicity. GC1107-T5.0, which contains relatively small amounts of tetanus toxoid, has been selected for a phase III clinical trial.

Steroids from Poison Hemlock (Conium maculatum L.: A GC-MS analysis

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Radulović Niko S.

2011-01-01

Full Text Available The steroid content of Conium maculatum L. (Poison Hemlock, Apiaceae, a well-known weed plant species, was studied herein for the first time. This was achieved by detailed GC-MS analyses of twenty two samples (dichloromethane extracts of different plant organs of C. maculatum at three or four different stages of phenological development, collected from three locations. In total, twenty four different steroids were identified. Six steroids had an ergostane nucleus while the other ones possessed a stigmastane carbon framework. The identity of these compounds was determined by spectral means (MS fragmentation, GC co-injections with authentic standards and chemical transformation (silylation. Steroid compounds were noted to be the main chemical constituents of root extracts (up to 70 % of this plant species in the last phase of development. The predominant ones were stigmasta-5,22- dien-3β-ol (stigmasterol and stigmasta-5-en-3β-ol (β-sitosterol. In an attempt to classify the samples, principal component analysis (PCA and agglomerative hierarchical clustering (AHC were performed using steroid percentages as variables.

Analysis of odorous gases with simultaneous GC-MS and sensory determination

Energy Technology Data Exchange (ETDEWEB)

Orko, I.; Lehtomaeki, J.; Sandell, E.; Arnold, M. [VTT Chemical Technology, Espoo (Finland). Environmental Technology

1995-12-31

Industrial odorous off-gases can consist of hundreds of different compounds giving cause to odour annoyance in the vicinity of the odour-emitting plant. For the identification of the odorous components in the gas, traditional analytical methods are not always sufficient since the odour threshold values cannot often be found in literature. This report describes the development of a GC-MS sniffing port method for identifying odorous compounds in off-gases. In the method the sample is injected into a gas chromatograph and divided into two flows. The compounds in these sample flows are separated in two identical columns and detected simultaneously in a mass spectrometer and by sensory means. The olfactory detections are marked in the iongram and the odorous compounds are identified. Tenax TA adsorbent is generally used for collecting the odorous sample for analysis. The compounds are released from the adsorbent for analysis by thermal desorption. The report also describes a case study where the GC-MS sniffing port method was applied to a gaseous emission from a food factory. Over ten odorous compounds could be identified. (author)

Coffee residues as substrates for aroma production by Ceratocystis fimbriata in solid state fermentation Produção de aromas por Ceratocystis fimbriata em fermentaç��o no estado sólido utilizando resíduos da agroindústria do café como substratos

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Adriane Bianchi Pedroni Medeiros

2003-07-01

Full Text Available The ability of two different strains of Ceratocystis fimbriata for fruity aroma production by solid state fermentation (SSF was tested on coffee pulp and coffee husk complemented with glucose as substrates. Experiments were carried out in 250 mL Erlenmeyer flasks and the experimental conditions were: 70% of initial moisture, 20% of glucose addition and pH 6.0. Aeration was made by passive diffusion through the gauze covering the flasks. Headspace analysis of the culture by gas chromatography (GC showed that 12 compounds were produced with coffee husk. Maximum total volatiles (TV concentration was reached after 72 h of culture with coffee husk as substrate (28 µmol.L-1.g-1. Ethyl acetate, ethanol and acetaldehyde were the major compounds produced, representing 84.7%, 7.6% and 2.0% of TV, respectively. A pre-treatment with heat (100ºC/ 40 min of substrates did not improve TV production. Respirometry analysis was used to determine the growth of the culture by measuring carbon dioxide produced. Results showed that the CO2 production follows the aroma production. This result shows the great potential for the use coffee pulp and coffee husk as substrates to microbial aroma production by solid state fermentation.Neste trabalho duas diferentes cepas de Ceratocystis fimbriata foram testadas para a produção de aromas frutais em fermentação no estado sólido (FES utilizando como substratos casca e polpa de café, suplementados com glicose. Os experimentos foram realizados em frascos Erlenmeyer de 250 mL. As condições experimentais foram: umidade inicial de 70%, adição de 20% de glicose e pH 6,0. Os frascos foram cobertos com gaze e a aeração ocorreu por difusão passiva. A análise do "headspace"da cultura foi feita por cromatografia gasosa e 12 compostos foram detectados utilizando a casca de café. A análise respirométrica foi realizada para o acompanhamento do crescimento do microrganismo pela determinação do dióxido de carbono

Essential oil of Lithraea molleoides (Vell.: chemical composition and antimicrobial activity Óleo essencial de Lithraea molleoides (Vell.: composição química e atividade antimicrobiana

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Mario Tsunezi Shimizu

2006-12-01

�leo essencial nas partes aéreas da planta. A análise do óleo essencial por cromatografia gasosa com espectrometria de massa, mostrou a presença de limoneno (89,89%, alfa-pineno (3,48%, beta-pineno (2,63%, alfa-terpineol (1.27%, mirceno (0,64%, sabineno (0,54%, 4-terpineol (0,28%, canfeno (0,22% e delta-3-careno (0,13%. O óleo essencial foi ativo contra algumas bactérias Gram positivas e leveduras testadas e não apresentou atividade contra bactérias Gram negativas.

Essential oil yield and chemical composition of chamomile [Chamomilla recutita (L. Rauschert] under drying air temperature of 70º C/ Rendimento e composição química do óleo essencial da camomila [Chamomilla recutita (L. Rauschert] submetida à secagem à 70º C

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Edmilson Cezar Paglia

2007-08-01

Full Text Available The drying process under 70º C was periodically monitored, in Campo Largo-PR, in “CHAMEL Ind. e Com. de Produtos Naturais LTDA.”, in the 2004 harvest. Simultaneously to the drying, the substances dragged by the steam of water were recovered by condensation. The hydrodistillation and GC-MS analyses were done in the UFPR Laboratories. A randomized experimental design was used, through polynomials regressions (P£0,01. The reduction of the water content and chamomile essential oil was progressive during the drying process; the reduction of the tenor of essential oil of the chamomile happens in the beginning of the drying; was possible to recover the substances volatilized during under 70º C drying temperature; the aromatic water (condensed composition was: artemisia ketona, bisabolol oxide B, alpha-bisabolol, bisabolene oxide, bisabolol oxide A; the essential oil components concentration of the chamomile, except for the alpha-pinene, were just numerically altered, without peculiar behavior in relation to the conditions of drying time.Com o objetivo de avaliar o rendimento e a composição química do óleo essencial de camomila, monitorouse periodicamente o processo de secagem em camada fixa à 70º C, realizada no município de Campo Largo – PR, num secador da “CHAMEL Ind. e Com. de Produtos Naturais LTDA.”, na safra de 2004. Simultaneamente à secagem, as substâncias arrastadas pelo vapor d’água foram recuperadas por condensação. As determinações analíticas foram realizadas nos Laboratórios de Fitoquímica e de Análises de Combustíveis Automotivos - LACAUT, por meio da hidrodestilação e cromatografia gasosa acoplada à espectrometria de massas. Os dados foram avaliados por meio de regressões polinomiais (P£0,01. A redução do teor de água da camomila foi progressiva durante o processo de secagem; a redução do teor de óleo essencial da camomila ocorreu no início da secagem; é possível recuperar as subst

Identificação dos constituintes químicos da fração volátil da Calendula officinalis produzida no Paraná Chemical compounds of the Calendula officinalis volatile fraction produced in the Paraná State, Brazil

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Zilda Cristiani Gazim

2007-03-01

Full Text Available A Calendula officinalis L., pertence à família Asteraceae, é originária da Europa e está aclimatada na região Sul do Brasil, onde vem crescendo o seu cultivo comercial para fins farmacêuticos e cosméticos. Suas inúmeras propriedades terapêuticas entre as quais antiinflamatória, cicatrizante e anti-séptica, justificam a grande procura desta planta pela população. O presente trabalho compara a composição química da fração volátil da cultura de calêndula aclimatada na região Noroeste do Paraná, com os dados da literatura da cultura na França. As substancias químicas majoritários identificadas por cromatografia gasosa acoplada à espectrometria de massas (CG/MS, nas duas culturas, foram sesquiterpenos hidrocarbonetos e álcoois; d-cadineno (22,53% e a-cadinol (20,40% para a cultura de calêndula produzida na região Noroeste do Paraná, Brasil, e d-cadineno (12,10% e a-cadinol (25,50% distinto do registrado para a cultura de calêndula produzida na região de Massif Central, França. Adicionalmente, para garantir a qualidade da planta na comercialização, foram realizadas análises físico-químicas (perda por secagem = 85,0% e perda por dessecação = 11,6%.Calendula officinalis L., belongs to the Asteraceae family from Europe and is acclimatized in the south region of Brazil where its commercial cultivation has been increasing for pharmaceutical and cosmetic purposes. Its several therapeutic properties (anti-inflammatory, healing, antiseptic justify the great demand for this plant by the population. The present study compares the chemical composition of the volatile fraction of two cultivations of calendula, one from Massif Central, France, and the other acclimatized in the Northeast region of Paraná State, Brazil. Most compounds identified by Gas Chromatography-mass spectrometry (GC-MS in both cultivations included the sesquiterpenes hydrocarbons and alcohols; d-cadinene (22.53% and á-cadinol (20.40% for the

Teor e composição química do óleo essencial de Hyptis marrubioides Epling (Lamiaceae em diferentes genótipos Essential oil content and chemical composition in Hyptis marrubioides Epl. of different genotypes

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P.P. Botrel

2009-01-01

Full Text Available Hyptis marrubioides Epling (hortelã-do-campo é espécie de uso medicinal conhecida pelas suas atividades contra infecções gastrointestinais, infecções de pele, dores e câimbras. Objetivou-se com este trabalho, avaliar o teor e composição química do óleo essencial de H. marrubioides em diferentes genótipos (roxo e branco e partes da planta fresca (folhas, inflorescências e caule. Os genótipos estudados foram identificados através das inflorescências das plantas que apresentam coloração roxa e branca. O delineamento experimental foi inteiramente casualizado, contendo as três partes da planta de ambos os genótipos, perfazendo um fatorial 3x2, com quatro repetições. O óleo essencial foi extraído por hidrodestilação por duas horas e analisado por Cromatografia Gasosa acoplada a Espectrometria de Massas (CG-EM. O maior teor de óleo essencial foi observado na inflorescência do genótipo roxo. A composição do óleo essencial de H. marrubioides variou quantitativamente entre as partes das plantas analisadas e entre os genótipos. O composto α-tujona apresentou a maior porcentagem de área do pico nas inflorescências de genótipo roxo. As porcentagens das plantas com genótipo roxo foram em média superiores às plantas com genótipo branco.Hyptis marrubioides Epling ("hortelã-do-campo" is a medicinal species known for its activities against gastrointestinal and skin infections, pains and cramps. The aim of this work was to evaluate essential oil content and chemical composition in H. marrubioides of different genotypes (purple and white, as well as fresh plant parts (leaves, inflorescences and stem. The studied genotypes were identified based on the inflorescences, which are purple and white. The experimental design was completely randomized, including the three parts of both genotypes, in a 3X2 factorial arrangement, with four replicates. Essential oil was extracted through hydrodistillation for two hours and analyzed

Essential oil yield and composition of ginger (Zingiber officinale Roscoe rhizomes after different drying periods Teor e composição de óleo essencial de rizomas de gengibre (Zingiber officinale Roscoe após diferentes períodos de secagem

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I.C.M Dabague

2011-01-01

Full Text Available Ginger production in Paraná State, Brazil, has predominated in Morretes Municipality, with around 300 ha cultivated area. The aim of this work was to evaluate the essential oil yield and composition of ginger rhizomes produced in Morretes and subjected to different drying periods at room temperature. Experimental design was completely randomized, in a 5x5 factorial arrangement, with four replicates (four plants each, five origins and five drying periods at room temperature (0, 15, 30, 45 and 60 days. The essential oil was extracted by hydrodistillation in a Clevenger-type device for 3h and the constituents were analyzed by gas chromatography-mass spectrometry (GC/MS. The drying of ginger rhizomes at room temperature for up to 60 days decreased the essential oil yield in most origins. Geranial and neral levels were higher in all origins and as drying periods were longer. Geraniol and geranyl acetate levels decreased after drying in all origins, as well as eucalyptol, camphene, zingiberene and β-bisabolene in most origins.A produção de gengibre no Paraná concentra-se no município de Morretes, ocupando uma área de plantio de aproximadamente 300 ha. O objetivo deste trabalho foi avaliar o teor e a composição do óleo essencial de rizomas de gengibre produzidos em Morretes e submetidos a diferentes períodos de secagem em temperatura ambiente. O delineamento experimental foi inteiramente casualizado, em esquema fatorial 5 x 5, com quatro repetições (quatro plantas por repetição, avaliando cinco procedências e cinco períodos de secagem a temperatura ambiente (0, 15, 30, 45 e 60 dias. As extrações de óleo essencial foram realizadas por hidrodestilação em aparelho graduado Clevenger durante três horas e a análise dos constituintes foi realizada por meio de cromatografia em fase gasosa acoplada à espectrometria de massas. A secagem de rizomas de gengibre em temperatura ambiente por até 60 dias resultou na diminuição de teores de

Curso diário e sazonal das trocas gasosas e do potencial hídrico foliar em aceroleiras Daily and seasonal course of gas exchange and leaf water potential in acerola plants

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REJANE JUREMA MANSUR CUSTÓDIO NOGUEIRA

2000-07-01

Full Text Available Este trabalho objetivou avaliar o curso diário e sazonal das trocas gasosas, da temperatura foliar e do potencial hídrico da acerola (Malpighia emarginata D.C., no campo. O experimento realizou-se no município de Paudalho, PE. Os valores da transpiração e do potencial da água foram, de modo geral, mais elevados no início da manhã e no final da tarde; os da resistência difusiva e temperatura foliar foram menores no início da manhã e no final da tarde. Houve uma limitação das trocas gasosas com o ambiente, em decorrência da redução da transpiração nas horas mais quentes do dia, sendo mais acentuada na estação seca e na matriz UFRPE 7. Os valores mínimos do potencial ocorreram na época seca, variando de -3,4 MPa (UFRPE 7 a -4,3 MPa (UFRPE 8, enquanto os valores máximos da resistência variaram de 16,30 s cm-1 (UFRPE 7 a 22,10 s cm-1 (UFRPE 8 na mesma estação. O potencial hídrico e a resistência difusiva mostraram forte correlação com o déficit de pressão de vapor. A maior capacidade fotossintética foi verificada em folhas maduras da matriz UFRPE 8. Os mecanismos fisiológicos apresentados pelas plantas demonstram que elas podem resistir a períodos de estresse hídrico quando estes se manifestam. A matriz UFRPE 8 é mais adaptada a períodos de estiagem do que a UFRPE 7.The daily and seasonal course of the gas exchanges, leaf temperature and water potential of Barbados cherry (Malpighia emarginata D.C. were evaluated under field conditions. The experiment was carried out in Paudalho, Pernambuco State, Brazil. Measurements of photosynthetic capacity in the wet season were also made. Changes in daily and seasonal behavior of gas exchange, water potential, and leaf temperature were observed. The transpiration and water potential measurements were higher at the beginning of the morning and at the end of the afternoon, while those for diffusive resistance and leaf temperature were lower at these same periods of the day

Determination of methylmercury in cryptogams by means of GC-AFS using enzymatic hydrolysis

Czech Academy of Sciences Publication Activity Database

Coufalík, Pavel; Meszarosová, N.; Coufalíková, K.; Zvěřina, O.; Komárek, J.

2018-01-01

Roč. 140 (2018), s. 8-13 ISSN 0026-265X Institutional support: RVO:68081715 Keywords : methylmercury * cryptogam * GC-AFS Subject RIV: CB - Analytical Chemistry, Separation OBOR OECD: Analytical chemistry Impact factor: 3.034, year: 2016

Rational construction of Z-scheme Ag_2CrO_4/g-C_3N_4 composites with enhanced visible-light photocatalytic activity

International Nuclear Information System (INIS)

Luo, Jin; Zhou, Xiaosong; Ma, Lin; Xu, Xuyao

2016-01-01

Highlights: • Novel visible-light driven Ag_2CrO_4/g-C_3N_4 composites were synthesized. • Ag_2CrO_4/g-C_3N_4 exhibited enhanced visible-light photocatalytic activity. • The reasons for the enhanced photocatalytic activity were revealed. - Abstract: Novel visible-light driven Z-scheme Ag_2CrO_4/g-C_3N_4 composites with different contents of Ag_2CrO_4 were fabricated by a facile chemical precipitation method and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), UV–vis diffuse reflectance spectroscopy (UV-vis DRS), photoluminescence (PL) spectroscopy and photoelectrochemical measurements. Compared with individual g-C_3N_4 and Ag_2CrO_4, the Ag_2CrO_4/g-C_3N_4 composites displayed much larger photocatalytic activities for the photocatalytic degradation of methyl orange (MO) solution at room temperature under visible light irradiation (λ > 420 nm). Importantly, the optimum photodegradation rate constant of the Ag_2CrO_4/g-C_3N_4 composite at a theoretical weight content of 8.0% Ag_2CrO_4 for the photodegradation of MO was 0.0068 min"−"1, which was 5.7 and 4.3 times higher than that of pure g-C_3N_4 and Ag_2CrO_4, respectively. Such enormous enhancement in photocatalytic performance was predominantly ascribed to the efficient separation and transfer of photogenerated electrons and holes at the Ag_2CrO_4/g-C_3N_4 interface imparted through the Z-scheme electron transfer. Furthermore, radical trap experiments depicted that both the holes and superoxide radical anions were thought to dominate oxidative species of the Ag_2CrO_4/g-C_3N_4 composite for MO degradation under visible light irradiation. Ultimately, a tentative Z-scheme photodegradation mechanism was proposed. This work may be useful for the rational design of new types of Z-scheme photocatalysts and provide some illuminate insights into the Z-scheme transfer mechanism for application in energy

GC-MS analysis, evaluation of phytochemicals, anti-oxidant, thrombolytic and anti-inflammatory activities of Exacum bicolor

OpenAIRE

Appaji Mahesh Ashwini; Latha Puttarudrappa; Belagumba Vijaykumar Ravi; Mala Majumdar

2015-01-01

The aim of the present study was to investigate the GC-MS analysis, phytochemical screening, anti-oxidant, thrombolytic and anti-inflammatory activities of methanol extract of leaves of Exacum bicolor. FTIR analysis confirmed the presence of alcohol, phenols, alkanes, aromatic compounds, aldehyde and ethers. GC-MS analysis revealed the presence of eight phyto-constituents. The total phenol, flavonoid and alkaloid contents were 18.0 ± 0.2 mg/GAE/g, 13.1 ± 0.4 mg QE/g and 108.0 ± 1.2 mg AE/g re...

Improved solar light stimulated charge separation of g-C3N4 through self-altering acidic treatment

Science.gov (United States)

Leong, Kah Hon; Lim, Ping Feng; Sim, Lan Ching; Punia, Varun; Pichiah, Saravanan

2018-02-01

Herein, we report the use of acid treatment to treat g-C3N4 nanostructured by a direct and facile synthesis route. The adopted treatment enhanced photoactivity of g-C3N4 and reflected in the removal of recalcitrant organic pollutant, Bisphenol A under direct sunlight. A complete removal of Bisphenol A was attained in a short duration (225 min) as compared to pure g-C3N4. The analysis clearly substantiated the robustness of acid exfoliation that promoted a blue shift, extended the conjugated length of its respective conduction and valance band. It also drastically prolonged the recombination rate of charge carriers, by producing excess of unpaired electrons in the conduction band for active radicals' generation. Thus, this new findings could offer a new sight of self-alteration in improving the photoactivity of complex organic pollutants for sustainable environmental remediation.

Speciation of organotin compounds in environmental samples by GC-ICPMS

International Nuclear Information System (INIS)

Vahcic, M.; Milacic, R.; Scancar, J.

2009-01-01

Full text: Analytical procedure using 15 m GC column was applied for simultaneous speciation of OTCs in various environmental samples. Methyl-, butyl-, phenyl- and octyl- tin species were quantitatively determined. different extraction reagents and conditions were studied. OTCs species were derivatized by NaBEt 4 and extracted into isooctane or hexane. The applied analytical procedure considerably shortened analytical time and enabled simultaneous determination of 12 OTCs in environmental samples. (author)

Improving Student Understanding of Qualitative and Quantitative Analysis via GC/MS Using a Rapid SPME-Based Method for Determination of Trihalomethanes in Drinking Water

Science.gov (United States)

Huang, Shu Rong; Palmer, Peter T.

2017-01-01

This paper describes a method for determination of trihalomethanes (THMs) in drinking water via solid-phase microextraction (SPME) GC/MS as a means to develop and improve student understanding of the use of GC/MS for qualitative and quantitative analysis. In the classroom, students are introduced to SPME, GC/MS instrumentation, and the use of MS…

TargetSearch--a Bioconductor package for the efficient preprocessing of GC-MS metabolite profiling data.

Science.gov (United States)

Cuadros-Inostroza, Alvaro; Caldana, Camila; Redestig, Henning; Kusano, Miyako; Lisec, Jan; Peña-Cortés, Hugo; Willmitzer, Lothar; Hannah, Matthew A

2009-12-16

Metabolite profiling, the simultaneous quantification of multiple metabolites in an experiment, is becoming increasingly popular, particularly with the rise of systems-level biology. The workhorse in this field is gas-chromatography hyphenated with mass spectrometry (GC-MS). The high-throughput of this technology coupled with a demand for large experiments has led to data pre-processing, i.e. the quantification of metabolites across samples, becoming a major bottleneck. Existing software has several limitations, including restricted maximum sample size, systematic errors and low flexibility. However, the biggest limitation is that the resulting data usually require extensive hand-curation, which is subjective and can typically take several days to weeks. We introduce the TargetSearch package, an open source tool which is a flexible and accurate method for pre-processing even very large numbers of GC-MS samples within hours. We developed a novel strategy to iteratively correct and update retention time indices for searching and identifying metabolites. The package is written in the R programming language with computationally intensive functions written in C for speed and performance. The package includes a graphical user interface to allow easy use by those unfamiliar with R. TargetSearch allows fast and accurate data pre-processing for GC-MS experiments and overcomes the sample number limitations and manual curation requirements of existing software. We validate our method by carrying out an analysis against both a set of known chemical standard mixtures and of a biological experiment. In addition we demonstrate its capabilities and speed by comparing it with other GC-MS pre-processing tools. We believe this package will greatly ease current bottlenecks and facilitate the analysis of metabolic profiling data.

Synthesis and Enhanced Ethanol Gas Sensing Properties of the g-C3N4 Nanosheets-Decorated Tin Oxide Flower-Like Nanorods Composite

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Yan Wang

2017-09-01

Full Text Available Flower-like SnO2/g-C3N4 nanocomposites were synthesized via a facile hydrothermal method by using SnCl4·5H2O and urea as the precursor. The structure and morphology of the as-synthesized samples were characterized by using the X-ray powder diffraction (XRD, electron microscopy (FESEM and TEM, and Fourier transform infrared spectrometer (FT-IR techniques. SnO2 displays the unique 3D flower-like microstructure assembled with many uniform nanorods with the lengths and diameters of about 400–600 nm and 50–100 nm, respectively. For the SnO2/g-C3N4 composites, SnO2 flower-like nanorods were coupled by a lamellar structure 2D g-C3N4. Gas sensing performance test results indicated that the response of the sensor based on 7 wt. % 2D g-C3N4-decorated SnO2 composite to 500 ppm ethanol vapor was 150 at 340 °C, which was 3.5 times higher than that of the pure flower-like SnO2 nanorods-based sensor. The gas sensing mechanism of the g-C3N4nanosheets-decorated SnO2 flower-like nanorods was discussed in relation to the heterojunction structure between g-C3N4 and SnO2.

GC-Rich Extracellular DNA Induces Oxidative Stress, Double-Strand DNA Breaks, and DNA Damage Response in Human Adipose-Derived Mesenchymal Stem Cells.

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Kostyuk, Svetlana; Smirnova, Tatiana; Kameneva, Larisa; Porokhovnik, Lev; Speranskij, Anatolij; Ershova, Elizaveta; Stukalov, Sergey; Izevskaya, Vera; Veiko, Natalia

2015-01-01

Cell free DNA (cfDNA) circulates throughout the bloodstream of both healthy people and patients with various diseases. CfDNA is substantially enriched in its GC-content as compared with human genomic DNA. Exposure of haMSCs to GC-DNA induces short-term oxidative stress (determined with H2DCFH-DA) and results in both single- and double-strand DNA breaks (comet assay and γH2AX, foci). As a result in the cells significantly increases the expression of repair genes (BRCA1 (RT-PCR), PCNA (FACS)) and antiapoptotic genes (BCL2 (RT-PCR and FACS), BCL2A1, BCL2L1, BIRC3, and BIRC2 (RT-PCR)). Under the action of GC-DNA the potential of mitochondria was increased. Here we show that GC-rich extracellular DNA stimulates adipocyte differentiation of human adipose-derived mesenchymal stem cells (haMSCs). Exposure to GC-DNA leads to an increase in the level of RNAPPARG2 and LPL (RT-PCR), in the level of fatty acid binding protein FABP4 (FACS analysis) and in the level of fat (Oil Red O). GC-rich fragments in the pool of cfDNA can potentially induce oxidative stress and DNA damage response and affect the direction of mesenchymal stem cells differentiation in human adipose-derived mesenchymal stem cells. Such a response may be one of the causes of obesity or osteoporosis.

Trans-acting GC-rich non-coding RNA at var expression site modulates gene counting in malaria parasite.

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Guizetti, Julien; Barcons-Simon, Anna; Scherf, Artur

2016-11-16

Monoallelic expression of the var multigene family enables immune evasion of the malaria parasite Plasmodium falciparum in its human host. At a given time only a single member of the 60-member var gene family is expressed at a discrete perinuclear region called the 'var expression site'. However, the mechanism of var gene counting remains ill-defined. We hypothesize that activation factors associating specifically with the expression site play a key role in this process. Here, we investigate the role of a GC-rich non-coding RNA (ncRNA) gene family composed of 15 highly homologous members. GC-rich genes are positioned adjacent to var genes in chromosome-central gene clusters but are absent near subtelomeric var genes. Fluorescence in situ hybridization demonstrates that GC-rich ncRNA localizes to the perinuclear expression site of central and subtelomeric var genes in trans. Importantly, overexpression of distinct GC-rich ncRNA members disrupts the gene counting process at the single cell level and results in activation of a specific subset of var genes in distinct clones. We identify the first trans-acting factor targeted to the elusive perinuclear var expression site and open up new avenues to investigate ncRNA function in antigenic variation of malaria and other protozoan pathogens. © The Author(s) 2016. Published by Oxford University Press on behalf of Nucleic Acids Research.

Surface reconstruction of titania with g-C3N4 and Ag for promoting efficient electrons migration and enhanced visible light photocatalysis

International Nuclear Information System (INIS)

Leong, Kah Hon; Liu, Sze Ling; Sim, Lan Ching; Saravanan, Pichiah; Jang, Min; Ibrahim, Shaliza

2015-01-01

Graphical abstract: - Highlights: • Visible light responsive TiO 2 was reconstructed with g-C 3 N 4 and Ag by simple route. • g-C 3 N 4 simultaneously promoted electrons migration and tuned energy gap of TiO 2 . • Ag facilitated electron junction and enhanced the visible light through SPR. • Reconstructed TiO 2 showed an excellent photocatalytic performance by removing AMX. - Abstract: The developments of heterogeneous photocatalysts are one among the competent reconstruction approach to enrich the visible light responsiveness of conventional TiO 2 . In the present work the TiO 2 was reconstructed with graphitic carbon nitride (g-C 3 N 4 ) and silver (Ag) to form a ternary (g-C 3 N 4 )–Ag/TiO 2 . The graphitic carbon nitride an intriguing material was prepared through a facile pyrolysis by using urea as a precursor. The silver (Ag) that plays a role as electron-conduction mobiliser in the ternary was synthesised through solar mediated photodeposition method. The synthesised ternary composite characteristics were thoroughly investigated through various physical and chemical analyses. The presence of g-C 3 N 4 in the ternary photocatalysts promoted the formation of interface between the Ag/TiO 2 and g-C 3 N 4 and stimulated the electron transfer between them. These electrons migration acknowledged by the synergic effect prolonged the lifetime of charge carriers. The g-C 3 N 4 also significantly tuned the energy band of conventional TiO 2 . The prepared ternary exhibited significantly high visible light photocatalytic performance by degrading Amoxicillin (AMX) a poor photosensitising pollutant at highest rate.

Avaliação da biodegradação de parafinas e da produção de biosurfactante por Bacillus subtilis na presença de petróleo Evaluation of paraffins biodegradation and biosurfactant production by Bacillus subtilis in the presence of crude oil

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Carmen Lucia Queiroga

2003-12-01

Full Text Available Os experimentos com Bacillus subtilis para avaliação da tensão superficial foram realizados com meio de cultivo contendo como nutrientes básicos 0,4% de ions nitrato e 4% de glicose, na presença de petróleo. A produção de surfactina foi observada pela redução da tensão superficial do meio de cultura fermentado. Surfactina foi isolada a partir do meio de cultura fermentado por B. subtilis, por precipitação ácida seguida de extração com clorofórmio-metanol. A avaliação da composição dos alcanos lineares (parafinas foi realizada por cromatografia gasosa. Observamos uma significativa redução da tensão superficial do meio de cultura indicando que a produção de biosurfactante não foi inibida pela presença de parafina, e que as parafinas leves podem ter sido consumidas.Bacillus subtilis experiments for surface tension evaluation were accomplished with culture medium containing 0.4% nitrate ions and 4% glucose basic nutrient in the presence of crude oil. Surfactin production was observed by surface tension reduction of the culture broth. Surfactin was isolated from Bacillus subtilis fermented broth, by acid-precipitation followed by extraction with chloroform-methanol. Evaluation of the linear alkanes composition was performed by capillary gas chromatography. We observed a significant reduction of the surface tension of the fermented broth indicating that the biosurfactant production was not inhibited by the crude oil presence, and that the light paraffins might have been consumed.

Produção de Biodiesel Metílico de Soja com o Auxílio de um Coletor Solar Sustentável

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Luiz Antonio Pimentel Cavalcanti

2016-06-01

Full Text Available A busca por fontes de energias alternativas tem aumentado substancialmente na última década, devido a expectativa de diminuição gradativa das reservas de petróleo e aumento da preocupação com as questões ambientais. O biodiesel vem se consolidando como potencial substituto para o diesel, porém, um dos gargalos da produção ainda é o custo operacional. Uma alternativa ao processo é utilizar coletores solares para realizar o aquecimento da reação de transesterificação. O presente trabalho propôs a construção de um protótipo de coletor solar constituído de matérias potencialmente recicláveis como garrafas PET e embalagens do tipo Tetra Pak. As garrafas PET foram recortadas na sua parte inferior para um encaixe futuro, tendo como função a proteção da parte absorvedora do painel do protótipo. As embalagens Tetra Pak foram pintadas de preto fosco em apenas um dos lados com intuito de absorver com maior eficiência os raios solares. Após a construção do coletor, foram realizados testes de aquecimento, para verificar se o mesmo forneceria a temperatura mínima desejada para haver a reação de transesterificação. O perfil de ésteres presentes no biodiesel, bem como, o seu teor de éster foram avaliados por cromatografia gasosa e seu valor enquadrado na resolução ANP N° 14 de 2012.

Composição química e toxicidade frente Aedes aegypti L. e Artemia salina Leach do óleo essencial das folhas de Myrcia sylvatica (G. Mey. DC.

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C.S. ROSA

2016-03-01

Full Text Available RESUMO A dengue está entre as doenças virais de propagação vetorial mais importante no mundo, causando sérios impactos de morbidade e mortalidade. Desta forma, o presente trabalho teve como objetivo analisar a composição química e a toxicidade do óleo essencial de Myrcia sylvatica (G. Mey D.C. frente Aedes aegypti e Artemia salina. Folhas de M. sylvatica foram coletadas no Parque Nacional da Chapada das Mesas, no município de Carolina (MA no mês de fevereiro de 2012. O óleo foi obtido por hidrodestilação e sua composição química foi determinada por cromatografia gasosa acoplada à espectrometria de massa (CG/EM. O bioensaio frente Artemia salina e às larvas de 3° estádio de Aedes aegypti foram realizados em diferentes concentrações. Os dados de mortalidade foram avaliados por regressão linear para determinar os valores de CL50. Obteve-se 0,5% de rendimento, sendo o (E-cariofileno o constituinte majoritário. O óleo essencial apresentou uma CL50 = 79,44 µg/mL frente A. salina, sendo considerado altamente tóxico. No entanto, este óleo não demonstrou efeito sobre as larvas de A. aegypti. Considerando que o teste de Artemia salina tem correlação com atividades biológicas de grande interesse terapêutico como antitumoral, o óleo essencial das folhas de M. sylvatica demonstrou potencial para desenvolvimento de produtos farmacêuticos.

Preliminary phytochemical screening, Antibacterial potential and GC-MS analysis of two medicinal plant extracts.

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Vijayaram, Seerangaraj; Kannan, Suruli; Saravanan, Konda Mani; Vasantharaj, Seerangaraj; Sathiyavimal, Selvam; P, Palanisamy Senthilkumar

2016-05-01

The presence study was aimed to catalyze the primary metabolites and their confirmation by using GC-MS analysis and antibacterial potential of leaf extract of two important medicinal plant viz., Eucalyptus and Azadirachta indica. The antibacterial potential of the methanol leaf extract of the studied species was tested against Escherichia coli, Pseudomonas aeruginosa, Klebsiellap neumoniae, Streptococcus pyogens, Staphylococcus aureus using by agar well diffusion method. The higher zone of inhibition (16mm) was observed against the bacterium Pseudomonas aeruginosa at 100μl concentration of methanol leaf extract. Preliminary phytochemical analysis of studied species shows that presence of phytochemical compounds like steroids, phenolic compounds and flavonoids. GC-MS analysis confirms the occurrence of 20 different compounds in the methanol leaf extract of the both studied species.

Supervised Semi-Automated Data Analysis Software for Gas Chromatography / Differential Mobility Spectrometry (GC/DMS) Metabolomics Applications.

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Peirano, Daniel J; Pasamontes, Alberto; Davis, Cristina E

2016-09-01

Modern differential mobility spectrometers (DMS) produce complex and multi-dimensional data streams that allow for near-real-time or post-hoc chemical detection for a variety of applications. An active area of interest for this technology is metabolite monitoring for biological applications, and these data sets regularly have unique technical and data analysis end user requirements. While there are initial publications on how investigators have individually processed and analyzed their DMS metabolomic data, there are no user-ready commercial or open source software packages that are easily used for this purpose. We have created custom software uniquely suited to analyze gas chromatograph / differential mobility spectrometry (GC/DMS) data from biological sources. Here we explain the implementation of the software, describe the user features that are available, and provide an example of how this software functions using a previously-published data set. The software is compatible with many commercial or home-made DMS systems. Because the software is versatile, it can also potentially be used for other similarly structured data sets, such as GC/GC and other IMS modalities.

Metal organic framework g-C3N4/MIL-53(Fe) heterojunctions with enhanced photocatalytic activity for Cr(VI) reduction under visible light

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Huang, Wenyuan; Liu, Ning; Zhang, Xiaodong; Wu, Minghong; Tang, Liang

2017-12-01

In this study, hybrid nanocomposites based on Fe-based MOF and graphitic carbon nitride (g-C3N4) were developed by a facile solvothermal method. The as-prepared materials were characterized by XRD, FESEM, TEM, XPS and PL analysis. It was showed that the introduction of a certain amount of g-C3N4 on the surface of MIL-53(Fe) would improve the separation and migration rate of photo-induced charges, consequently resulting in the boost of photocatalytic efficiency. Compared with g-C3N4 and MIL-53(Fe), the CMFe composites displayed more excellent visible light-resposive photocatalytic activity for the reduction of Cr(VI). The optimal doping content of g-C3N4 in g-C3N4/MIL-53(Fe) composite was determined to be 3.0 wt%, and it showed about 2.1 and 2.0 times as high photocatalytic efficiency for the reduction of Cr(VI) as that of pure g-C3N4 and MIL-53(Fe), respectively. Meanwhile, the composite exhibited good reusability and stability in the process of cyclic experiments. A possible photocatalytic reaction mechanism was also investigated in detail by the related electrochemical analysis.

Role of the NO/sGC/PKG signaling pathway of hippocampal CA1 in morphine-induced reward memory.

Science.gov (United States)

Shen, Fang; Li, Yi-Jing; Shou, Xiao-Jing; Cui, Cai-Lian

2012-09-01

Evidence suggests that the nitric oxide (NO)/soluble guanylyl cyclase (sGC)/cGMP dependent protein kinase (PKG) signaling pathway plays a key role in memory processing, but the actual participation of this signaling cascade in the hippocampal CA1 during morphine-induced reward memory remains unknown. In this study, we investigated the role of the NO/sGC/PKG signaling pathway in the CA1 on morphine-induced reward memory using a conditioned place preference (CPP) paradigm. We found that rats receiving an intraperitoneal (i.p.) injection of 4mg/kg morphine exhibited CPP, whereas rats treated with only 0.2mg/kg morphine failed to produce CPP. Intra-CA1 injection of the neuronal NO synthase (nNOS) inhibitor 7-NI, the sGC inhibitor ODQ or the PKG inhibitor Rp-8-Br-PET-cGMPS had no effect on the acquisition of CPP by 4mg/kg morphine. Intra-CA1 injection of 7-NI blocked the consolidation of CPP induced by 4mg/kg morphine, and this amnesic effect of 7-NI was mimicked by ODQ and Rp-8-Br-PET-cGMPS. Intra-CA1 injection of the NOS substrate L-arg or the sGC activator YC-1 with an ineffective dose of morphine (0.2mg/kg, i.p.) elicited CPP. This response induced by L-arg or YC-1 was reversed by pre-microinjection of Rp-8-Br-PET-cGMPS in the CA1. These results indicated that the activation of the NO/sGC/PKG signaling pathway in the CA1 is necessary for the consolidation of morphine-related reward memory. Copyright © 2012 Elsevier Inc. All rights reserved.

Photocatalytic reduction of CO2 into hydrocarbon solar fuels over g-C3N4-Pt nanocomposite photocatalysts.

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Yu, Jiaguo; Wang, Ke; Xiao, Wei; Cheng, Bei

2014-06-21

Photocatalytic reduction of CO2 into renewable hydrocarbon fuels is an alternative way to develop reproducible energy, which is also a promising way to solve the problem of the greenhouse effect. In this work, graphitic carbon nitride (g-C3N4) was synthesized by directly heating thiourea at 550 °C and then a certain amount of Pt was deposited on it to form g-C3N4-Pt nanocomposites used as catalysts for photocatalytic reduction of CO2 under simulated solar irradiation. The main products of photocatalysis were CH4, CH3OH and HCHO. The deposited Pt acted as an effective cocatalyst, which not only influenced the selectivity of the product generation, but also affected the activity of the reaction. The yield of CH4 first increased upon increasing the amount of Pt deposited on the g-C3N4 from 0 to 1 wt%, then decreased at 2 wt% Pt loading. The production rates of CH3OH and HCHO also increased with the content of Pt increasing from 0 to 0.75 wt% and the maximum yield was observed at 0.75 wt%. The Pt nanoparticles (NPs) could facilitate the transfer and enrichment of photogenerated electrons from g-C3N4 to its surface for photocatalytic reduction of CO2. At the same time, Pt was also used a catalyst to promote the oxidation of products. The transient photocurrent response further confirmed the proposed photocatalytic reduction mechanism of CO2. This work indicates that the deposition of Pt is a good strategy to improve the photoactivity and selectivity of g-C3N4 for CO2 reduction.

Urinary amino acid analysis: a comparison of iTRAQ-LC-MS/MS, GC-MS, and amino acid analyzer.

Science.gov (United States)

Kaspar, Hannelore; Dettmer, Katja; Chan, Queenie; Daniels, Scott; Nimkar, Subodh; Daviglus, Martha L; Stamler, Jeremiah; Elliott, Paul; Oefner, Peter J

2009-07-01

Urinary amino acid analysis is typically done by cation-exchange chromatography followed by post-column derivatization with ninhydrin and UV detection. This method lacks throughput and specificity. Two recently introduced stable isotope ratio mass spectrometric methods promise to overcome those shortcomings. Using two blinded sets of urine replicates and a certified amino acid standard, we compared the precision and accuracy of gas chromatography/mass spectrometry (GC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) of propyl chloroformate and iTRAQ derivatized amino acids, respectively, to conventional amino acid analysis. The GC-MS method builds on the direct derivatization of amino acids in diluted urine with propyl chloroformate, GC separation and mass spectrometric quantification of derivatives using stable isotope labeled standards. The LC-MS/MS method requires prior urinary protein precipitation followed by labeling of urinary and standard amino acids with iTRAQ tags containing different cleavable reporter ions distinguishable by MS/MS fragmentation. Means and standard deviations of percent technical error (%TE) computed for 20 amino acids determined by amino acid analyzer, GC-MS, and iTRAQ-LC-MS/MS analyses of 33 duplicate and triplicate urine specimens were 7.27+/-5.22, 21.18+/-10.94, and 18.34+/-14.67, respectively. Corresponding values for 13 amino acids determined in a second batch of 144 urine specimens measured in duplicate or triplicate were 8.39+/-5.35, 6.23+/-3.84, and 35.37+/-29.42. Both GC-MS and iTRAQ-LC-MS/MS are suited for high-throughput amino acid analysis, with the former offering at present higher reproducibility and completely automated sample pretreatment, while the latter covers more amino acids and related amines.

Improved Separation of Complex Polycyclic Aromatic Hydrocarbon Mixtures Using Novel Column Combinations in GC×GC/ToF-MS

Science.gov (United States)

Manzano, Carlos; Hoh, Eunha; Simonich, Staci L. Massey

2012-01-01

Complex mixtures of polycyclic aromatic hydrocarbons (PAHs) are difficult to resolve because of the high degree of overlap in compound vapor pressures, boiling points and mass spectral fragmentation patterns. The objective of this research was to improve the separation of complex PAH mixtures (including 97 different parent, alkyl-, nitro-, oxy-, thio-, chloro-, bromo-, and high molecular weight PAHs) using GC×GC/ToF-MS by maximizing the orthogonality of different GC column combinations and improving the separation of PAHs from the sample matrix interferences, including unresolved complex mixtures (UCM). Four different combinations of non-polar, polar, liquid crystal and nano-stationary phase columns were tested. Each column combination was optimized and evaluated for orthogonality using a method based on conditional entropy that considers the quantitative peak distribution in the entire two-dimensional space. Finally, an atmospheric particulate matter with diameter column in the first dimension and a 1.2 m × 0.10 mm × 0.10 µm NSP-35 nano-stationary phase column in the second dimension. In addition, the use of this column combination in GC×GC/ToF-MS resulted in significantly shorter analysis times (176 min) for complex PAH mixtures compared to one-dimensional GC/MS (257 min), as well as potentially reduced sample preparation time. PMID:22769970

Sol-gel titania-coated needles for solid phase dynamic extraction-GC/MS analysis of desomorphine and desocodeine.

Science.gov (United States)

Su, Chi-Ju; Srimurugan, Sankarewaran; Chen, Chinpiao; Shu, Hun-Chi

2011-01-01

Novel sol-gel titania film coated needles for solid-phase dynamic extraction (SPDE)-GC/MS analysis of desomorphine and desocodeine are described. The high thermal stability of titania film permits efficient extraction and analysis of poorly volatile opiate drugs. The influences of sol-gel reaction time, coating layer, extraction and desorption time and temperature on the SPDE needle performance were investigated. The deuterium labeled internal standard was introduced either during the extraction of analyte or directly injected to GC after the extraction process. The latter method was shown to be more sensitive for the analysis of water and urine samples containing opiate drugs. The proposed conditions provided a wide linear range (from 5-5000 ppb), and satisfactory linearity, with R(2) values from 0.9958 to 0.9999, and prominent sensitivity, LOQs (1.0-5.0 ng/g). The sol-gel titania film coated needle with SPDE-GC/MS will be a promising technique for desomorphine and desocodeine analysis in urine.

GC/MS determination of monosaccharides in yogurt products

International Nuclear Information System (INIS)

Nam, Sang Kyu; Cheong, Won Jo

2000-01-01

Yogurt products are known to be effective for enhancing health and preventing diseases such as cancers. Such effects are generally believed to be due to actions of polysaccharides in yogurt products. In this study we have determined compositions of monosaccharides in hydrolysates of commercial yogurt products as the first step of understanding structures of polysaccharides. The yogurt products were ultracentrifuged, filtered, hydrolyzed in 1M sulfuric acid and neutralized. A porting of the solution was taken and evaporated to dryness, derivatized with TMSI (trimethyl- silylimidazole) and analyzed by GC/MS. We found that the monosaccharides were fructose, glucose, and galactose. Their compositions were variant among several yogurt products

GC/MS determination of monosaccharides in yogurt products

Energy Technology Data Exchange (ETDEWEB)

Nam, Sang Kyu; Cheong, Won Jo [Inha Univ., Incheon (Korea, Republic of)

2000-02-01

Yogurt products are known to be effective for enhancing health and preventing diseases such as cancers. Such effects are generally believed to be due to actions of polysaccharides in yogurt products. In this study we have determined compositions of monosaccharides in hydrolysates of commercial yogurt products as the first step of understanding structures of polysaccharides. The yogurt products were ultracentrifuged, filtered, hydrolyzed in 1M sulfuric acid and neutralized. A porting of the solution was taken and evaporated to dryness, derivatized with TMSI (trimethyl- silylimidazole) and analyzed by GC/MS. We found that the monosaccharides were fructose, glucose, and galactose. Their compositions were variant among several yogurt products.

TargetSearch - a Bioconductor package for the efficient preprocessing of GC-MS metabolite profiling data

Science.gov (United States)

2009-01-01

Background Metabolite profiling, the simultaneous quantification of multiple metabolites in an experiment, is becoming increasingly popular, particularly with the rise of systems-level biology. The workhorse in this field is gas-chromatography hyphenated with mass spectrometry (GC-MS). The high-throughput of this technology coupled with a demand for large experiments has led to data pre-processing, i.e. the quantification of metabolites across samples, becoming a major bottleneck. Existing software has several limitations, including restricted maximum sample size, systematic errors and low flexibility. However, the biggest limitation is that the resulting data usually require extensive hand-curation, which is subjective and can typically take several days to weeks. Results We introduce the TargetSearch package, an open source tool which is a flexible and accurate method for pre-processing even very large numbers of GC-MS samples within hours. We developed a novel strategy to iteratively correct and update retention time indices for searching and identifying metabolites. The package is written in the R programming language with computationally intensive functions written in C for speed and performance. The package includes a graphical user interface to allow easy use by those unfamiliar with R. Conclusions TargetSearch allows fast and accurate data pre-processing for GC-MS experiments and overcomes the sample number limitations and manual curation requirements of existing software. We validate our method by carrying out an analysis against both a set of known chemical standard mixtures and of a biological experiment. In addition we demonstrate its capabilities and speed by comparing it with other GC-MS pre-processing tools. We believe this package will greatly ease current bottlenecks and facilitate the analysis of metabolic profiling data. PMID:20015393

TargetSearch - a Bioconductor package for the efficient preprocessing of GC-MS metabolite profiling data

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Lisec Jan

2009-12-01

Full Text Available Abstract Background Metabolite profiling, the simultaneous quantification of multiple metabolites in an experiment, is becoming increasingly popular, particularly with the rise of systems-level biology. The workhorse in this field is gas-chromatography hyphenated with mass spectrometry (GC-MS. The high-throughput of this technology coupled with a demand for large experiments has led to data pre-processing, i.e. the quantification of metabolites across samples, becoming a major bottleneck. Existing software has several limitations, including restricted maximum sample size, systematic errors and low flexibility. However, the biggest limitation is that the resulting data usually require extensive hand-curation, which is subjective and can typically take several days to weeks. Results We introduce the TargetSearch package, an open source tool which is a flexible and accurate method for pre-processing even very large numbers of GC-MS samples within hours. We developed a novel strategy to iteratively correct and update retention time indices for searching and identifying metabolites. The package is written in the R programming language with computationally intensive functions written in C for speed and performance. The package includes a graphical user interface to allow easy use by those unfamiliar with R. Conclusions TargetSearch allows fast and accurate data pre-processing for GC-MS experiments and overcomes the sample number limitations and manual curation requirements of existing software. We validate our method by carrying out an analysis against both a set of known chemical standard mixtures and of a biological experiment. In addition we demonstrate its capabilities and speed by comparing it with other GC-MS pre-processing tools. We believe this package will greatly ease current bottlenecks and facilitate the analysis of metabolic profiling data.

cIMP synthesized by sGC as a mediator of hypoxic contraction of coronary arteries.

Science.gov (United States)

Chen, Zhengju; Zhang, Xu; Ying, Lei; Dou, Dou; Li, Yanhui; Bai, Yun; Liu, Juan; Liu, Limei; Feng, Han; Yu, Xiaoxing; Leung, Susan Wai-Sum; Vanhoutte, Paul M; Gao, Yuansheng

2014-08-01

cGMP is considered the only mediator synthesized by soluble guanylyl cyclase (sGC) in response to nitric oxide (NO). However, purified sGC can synthesize several other cyclic nucleotides, including inosine 3',5'-cyclic monophosphate (cIMP). The present study was designed to determine the role of cIMP in hypoxic contractions of isolated porcine coronary arteries. Vascular responses were examined by measuring isometric tension. Cyclic nucleotides were assayed by HPLC tandem mass spectroscopy. Rho kinase (ROCK) activity was determined by measuring the phosphorylation of myosin phosphatase target subunit 1 using Western blot analysis and an ELISA kit. The level of cIMP, but not that of cGMP, was elevated by hypoxia in arteries with, but not in those without, endothelium [except if treated with diethylenetriamine (DETA) NONOate]; the increases in cIMP were inhibited by the sGC inhibitor 1H-[1,2,4]oxadiazolo[4,3,-a]quinoxalin-1-one (ODQ). Hypoxia (Po2: 25-30 mmHg) augmented contractions of arteries with and without endothelium if treated with DETA NONOate; these hypoxic contractions were blocked by ODQ. In arteries without endothelium, hypoxic augmentation of contraction was also obtained with exogenous cIMP. In arteries with endothelium, hypoxic augmentation of contraction was further enhanced by inosine 5'-triphosphate, the precursor for cIMP. The augmentation of contraction caused by hypoxia or cIMP was accompanied by increased phosphorylation of myosin phosphatase target subunit 1 at Thr(853), which was prevented by the ROCK inhibitor Y-27632. ROCK activity in the supernatant of isolated arteries was stimulated by cIMP in a concentration-dependent fashion. These results demonstrate that cIMP synthesized by sGC is the likely mediator of hypoxic augmentation of coronary vasoconstriction, in part by activating ROCK. Copyright © 2014 the American Physiological Society.

GC-Rich Extracellular DNA Induces Oxidative Stress, Double-Strand DNA Breaks, and DNA Damage Response in Human Adipose-Derived Mesenchymal Stem Cells

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Svetlana Kostyuk

2015-01-01

Full Text Available Background. Cell free DNA (cfDNA circulates throughout the bloodstream of both healthy people and patients with various diseases. CfDNA is substantially enriched in its GC-content as compared with human genomic DNA. Principal Findings. Exposure of haMSCs to GC-DNA induces short-term oxidative stress (determined with H2DCFH-DA and results in both single- and double-strand DNA breaks (comet assay and γH2AX, foci. As a result in the cells significantly increases the expression of repair genes (BRCA1 (RT-PCR, PCNA (FACS and antiapoptotic genes (BCL2 (RT-PCR and FACS, BCL2A1, BCL2L1, BIRC3, and BIRC2 (RT-PCR. Under the action of GC-DNA the potential of mitochondria was increased. Here we show that GC-rich extracellular DNA stimulates adipocyte differentiation of human adipose-derived mesenchymal stem cells (haMSCs. Exposure to GC-DNA leads to an increase in the level of RNAPPARG2 and LPL (RT-PCR, in the level of fatty acid binding protein FABP4 (FACS analysis and in the level of fat (Oil Red O. Conclusions. GC-rich fragments in the pool of cfDNA can potentially induce oxidative stress and DNA damage response and affect the direction of mesenchymal stem cells differentiation in human adipose—derived mesenchymal stem cells. Such a response may be one of the causes of obesity or osteoporosis.

GcSTUA, an APSES transcription factor, is required for generation of appressorial turgor pressure and full pathogenicity of Glomerella cingulata.

Science.gov (United States)

Tong, XingZhang; Zhang, Xiuwen; Plummer, Kim M; Stowell, Kathryn M; Sullivan, Patrick A; Farley, Peter C

2007-09-01

Glomerella cingulata, which infects a number of different hosts, gains entry to the plant tissue by means of an appressorium. Turgor pressure generated within the appressorium forces a penetration peg through the plant cuticle. A visible lesion forms as the fungus continues to grow within the host. A G. cingulata homolog (GcSTUA) of the genes encoding Asm1, Phd1, Sok2, Efg1, and StuA transcription factors in Magnaporthe grisea and other fungi was cloned and shown to be required for infection of intact apple fruit and penetration of onion epidermal cells. Mobilization of glycogen and triacylglycerol during formation of appressoria by the GcSTUA deletion mutant appeared normal and melanization of the maturing appressoria was also indistinguishable from that of the wild type. However, GcSTUA was essential for the generation of normal turgor pressure within the appressorium. As is the case for its homologs in other fungi, GcSTUA also was required for the formation of aerial hyphae, efficient conidiation, and the formation of perithecia (sexual reproductive structures).

Characterization of volatile profile from ten different varieties of Chinese jujubes by HS-SPME/GC-MS coupled with E-nose.

Science.gov (United States)

Chen, Qinqin; Song, Jianxin; Bi, Jinfeng; Meng, Xianjun; Wu, Xinye

2018-03-01

Volatile profile of ten different varieties of fresh jujubes was characterized by HS-SPME/GC-MS (headspace solid phase micro-extraction combined with gas chromatography-mass spectrometry) and E-nose (electronic nose). GC-MS results showed that a total of 51 aroma compounds were identified in jujubes, hexanoic acid, hexanal, (E)-2-hexenal, (Z)-2-heptenal, benzaldehyde and (E)-2-nonenal were the main aroma components with contributions that over 70%. Differentiation of jujube varieties was conducted by cluster analysis of GC-MS data and principal component analysis & linear discriminant analysis of E-nose data. Both results showed that jujubes could be mainly divided into two groups: group A (JZ, PDDZ, JSXZ and LWZZ) and group B (BZ, YZ, MZ, XZ and DZ). There were significant differences in contents of alcohols, acids and aromatic compounds between group A and B. GC-MS coupled with E-nose could be a fast and accurate method to identify the general flavor difference in different varieties of jujubes. Copyright © 2017 Elsevier Ltd. All rights reserved.

High-throughput investigation of polymerization kinetics by online monitoring of GPC and GC

NARCIS (Netherlands)

Hoogenboom, R.; Fijten, M.W.M.; Abeln, C.H.; Schubert, U.S.

2004-01-01

Gel permeation chromatography (GPC) and gas chromatography (GC) were successfully introduced into a high-throughput workflow. The feasibility and limitations of online GPC with a high-speed column was evaluated by measuring polystyrene standards and comparison of the results with regular offline GPC

Dualism of gene GC content and CpG pattern in regard to expression in the human genome: magnitude versus breadth.

Science.gov (United States)

Vinogradov, Alexander E

2005-12-01

In this article, I show that, in the human genome, the GC content in genes (but not the CpG island in the promoter) is related to the maximum level of gene expression among tissues, whereas the promoter CpG island and gene CpG level are more strongly related to the breadth of expression among tissues. The relevance of gene GC content to expression cannot be a consequence (i.e. a byproduct) of transcription because it does not correlate with expression in the germline. The variation of GC content and CpG level can determine the characteristics of gene expression in a synergistic interplay with transcription-factor-binding sites (mediated by chromatin condensation).

Automated GC-MS analysis of free amino acids in biological fluids.

Science.gov (United States)

Kaspar, Hannelore; Dettmer, Katja; Gronwald, Wolfram; Oefner, Peter J

2008-07-15

A gas chromatography-mass spectrometry (GC-MS) method was developed for the quantitative analysis of free amino acids as their propyl chloroformate derivatives in biological fluids. Derivatization with propyl chloroformate is carried out directly in the biological samples without prior protein precipitation or solid-phase extraction of the amino acids, thereby allowing automation of the entire procedure, including addition of reagents, extraction and injection into the GC-MS. The total analysis time was 30 min and 30 amino acids could be reliably quantified using 19 stable isotope-labeled amino acids as internal standards. Limits of detection (LOD) and lower limits of quantification (LLOQ) were in the range of 0.03-12 microM and 0.3-30 microM, respectively. The method was validated using a certified amino acid standard and reference plasma, and its applicability to different biological fluids was shown. Intra-day precision for the analysis of human urine, blood plasma, and cell culture medium was 2.0-8.8%, 0.9-8.3%, and 2.0-14.3%, respectively, while the inter-day precision for human urine was 1.5-14.1%.

Determinação de herbicidas usados no cultivo de arroz irrigado na região sul do estado de Santa Catarina através da SPME-GC-ECD Determination of herbicides used in irrigated rice cultivation in the south of Santa Catarina using SPME-GC-ECD

Directory of Open Access Journals (Sweden)

Léa L. F. Costa

2008-01-01

Full Text Available Evaluation of the pollution by the herbicides alachlor, propanil and atrazine in water samples from four rivers in the cities of Turvo and Meleiro, south of Santa Catarina State, was made using the SPME-GC-ECD method. The proposed method was optimized and validated. The correlation coefficients were higher than 0.997 and linear ranges of the analytical curves were 0.1-4; 0.1-2.5 and 0.1-5 µg L-1 for atrazine, alachlor and propanil, respectively. The herbicides were quantified by GC-ECD and identified by GC-MS. Both of the selected rivers presented contamination by at least one of the studied herbicides.

Postirradiation examination data report for gap conductance test series. Test GC 2-1

International Nuclear Information System (INIS)

Murdock, B.A.

1978-02-01

The results of the postirradiation examination of four boiling water reactor type, zircaloy-clad, UO 2 -fueled rods tested in the Power Burst Facility are discussed. These rods were employed in Gap Conductance Test GC 2-1 which was performed to obtain experimental data from which test fuel rod gap conductance values could be determined by both the steady state ∫kdT and the power oscillation methods. The postirradiation examination results provided in the document will aid in interpreting the experimental data obtained during Test GC 2-1 and in evaluating the effect of fuel behavior on the fuel rod thermal response and interpreted gap conductances. Fuel rod fill gas composition and pressure are discussed. Measurements of fuel pellet-cladding gap and fuel crack areas are presented. The fuel structure is analyzed. Test rod instrumentation and power profiles are examined to better evaluate the test conditions

[GC-MS analysis of volatile constituents from five different kinds of Chinese eaglewood].

Science.gov (United States)

Mei, Wen-Li; Zeng, Yan-Bo; Liu, Jun; Dai, Hao-Fu

2007-05-01

Volatile oils of five different kinds of Chinese eaglewood were extracted with aether at room temperature. The chemical constituents and relative contents of the volatile oils were analysed by GC-MS. It showed that all the five volatile oils were mainly composed of sesquiterpenes, aromatic constituents and fatty acids. Several sesquiterpenes, such as hinesol, nootkatone, valerenic acid, velleral, guaiol, gamma-gurjunene, gamma-selinene, viridiflorol, isoaromadendrene epoxide, valencene, alpha-costol et. al., together with several aromatic constituents, 2,4-di-tert-butylphenol,4-methyl-2,6-di-tert-butylphenol, phenylpropionic acid, 1-(benzyloxy)-8-naphthol, anisylacetone, et. al. were found in the volatile oils of Chinese eaglewood for the first time. The samilarities and differences of the volatile oils from the five kinds of Chinese eaglewood were compared. It suggested that the quality of Chinese eaglewood could be evaluated by GC-MS analyse of the volatile oil.

Determination of pesticides in fruits and vegetables using acetonitrile extraction and GC/MS technique

International Nuclear Information System (INIS)

Hussain, Z.

2010-01-01

A selection of oranges, guava and spinach were purchased from the local markets of Lahore, Pakistan. Extraction of the samples was carried out using an acetonitrile/toluene extraction procedure to determine the residual concentration of pesticides which may have been used during seasonal growth. Gas chromatography/mass spectrometry (GC/MS) was used for quantitative and confirmatory analysis of GC-amenable pesticides. The data obtained was compared with that of a referenced pesticide by matching molecular weight to a library of known pesticides. For comparison the same non-sprayed fruits/vegetable were extracted as a control reference. Factors studied were retention time, elution time, relative abundance and molecular weight. The results showed that low molecular weight pesticides were eluted before the high molecular weight pesticides. Pesticides identified included crotoxyphos, fenoxycarb and methoxyfenozide. (author)

Detection limits in the chromatographic element trace analysis - quantitative TLC, HPLC and GC with the example of beryllium acetylacetonate

International Nuclear Information System (INIS)

Schwedt, G.

1981-01-01

Chromatographic analyses of beryllium acetylacetonate are carried out in synthetic solutions within the nano- and picogram range of beryllium. For thin-layer chromatography (TLC) normal and silanized silica gel is used, for high-performance liquid chromatography (HPLC) silica gel of 7 μm particles, for gas chromatography (GC) silicone SE-30 as stationary phase. Visual evaluation and remission measurements in TLC, UV-254 nm absorption measurements in HPLC and measurements with a FID in GC are employed for the determination of the calibration curves. A calibration curve through the origin and a detection limit of 150 pg Be determinable form are received by HPLC only. For trace analyses by GC a new definition of a detection limit for the evaluation of substance peaks on a solvent tailing is suggested. (orig.) [de

Fabrication of flower-like direct Z-scheme β-Bi2O3/g-C3N4 photocatalyst with enhanced visible light photoactivity for Rhodamine B degradation

Science.gov (United States)

Zhang, Liping; Wang, Guohong; Xiong, Zhenzhong; Tang, Hua; Jiang, Chuanjia

2018-04-01

A combined hydrothermal-calcination approach is developed to synthesize hierarchical β-Bi2O3/g-C3N4 direct Z-scheme photocatalyst with enhanced visible light photoactivity for Rhodamine B (RhB) degradation. First, Bi2O2CO3 microflowers were hydrothermally prepared using Bi(NO3)3·5H2O as feedstocks, and then a series of β-Bi2O3/g-C3N4 direct Z-scheme photocatalysts were synthesized via a facile calcination method using Bi2O2CO3 and g-C3N4 as precursors. The samples were systematically characterized by various characterization technologies including X-ray diffraction, scanning and transmission electron microscopes, Fourier transform infrared spectroscopy and N2 absorption-desorption equipment. It was found that the g-C3N4 content in the precursors played a key role in affecting the photocatalytic activity of the final products. The β-Bi2O3/g-C3N4 heterojunction exhibited higher photocatalytic activity than single active components (β-Bi2O3 and g-C3N4), indicating the presence of a synergistic effect between two active components in β-Bi2O3/g-C3N4 heterojunction. Among all as-prepared catalysts, the 70 wt.% g-C3N4/Bi2O2CO3 exhibits the highest activity for RhB degradation, and the apparent reaction rate constant k (42.2 × 10-3 min-1) is 3.1 and 1.7 times as high as that of pure β-Bi2O3 (13.5 × 10-3 min-1) and g-C3N4 (25.2 × 10-3 min-1), respectively. The enhanced photocatalytic performance of β-Bi2O3/g-C3N4 heterostructure photocatalysts is mainly due to the high surface area, closely contacted interfaces between the β-Bi2O3 and g-C3N4 component, and the formation of direct Z-scheme structure in the β-Bi2O3/g-C3N4 composites.

Facile synthesis of Fe3O4/g-C3N4/HKUST-1 composites as a novel biosensor platform for ochratoxin A.

Science.gov (United States)

Hu, Shuisheng; Ouyang, Wenjun; Guo, Longhua; Lin, Zhenyu; Jiang, Xiaohua; Qiu, Bin; Chen, Guonan

2017-06-15

A fluorescent biosensor for ochratoxin A was fabricated on the basis of a new nanocomposite (Fe 3 O 4 /g-C 3 N 4 /HKUST-1 composites). Fe 3 O 4 /g-C 3 N 4 /HKUST-1 was synthesized in this work for the first time, which combined HKUST-1 with g-C 3 N 4 to improve its chemical stability. Fe 3 O 4 /g-C 3 N 4 /HKUST-1 composites have strong adsorption capacity for dye-labeled aptamer and are able to completely quench the fluorescence of the dye through the photoinduced electron transfer (PET) mechanism. In the presence of ochratoxin A (OTA), it can bind with the aptamer with high affinity, causing the releasing of the dye-labeled aptamer from the Fe 3 O 4 /g-C 3 N 4 /HKUST-1 and therefore results in the recovery of fluorescence. The fluorescence intensity of the biosensor has a linear relationship with the OTA concentration in the range of 5.0-160.0ng/mL. The LOD of sensor is 2.57ng/mL (S/N=3). This fluorescence sensor based on the Fe 3 O 4 /g-C 3 N 4 /HKUST-1 composites has been applied to detect OTA in corn with satisfying results. Copyright © 2016. Published by Elsevier B.V.

Estimation of Environment-Related Properties of Chemicals for Design of Sustainable Processes: Development of Group-Contribution+ (GC+) Property Models and Uncertainty Analysis

Science.gov (United States)

The aim of this work is to develop group-contribution+ (GC+) method (combined group-contribution (GC) method and atom connectivity index (CI) method) based property models to provide reliable estimations of environment-related properties of organic chemicals together with uncert...

GC/MS-based profiling of amino acids and TCA cycle-related molecules in ulcerative colitis.

Science.gov (United States)

Ooi, Makoto; Nishiumi, Shin; Yoshie, Tomoo; Shiomi, Yuuki; Kohashi, Michitaka; Fukunaga, Ken; Nakamura, Shiro; Matsumoto, Takayuki; Hatano, Naoya; Shinohara, Masakazu; Irino, Yasuhiro; Takenawa, Tadaomi; Azuma, Takeshi; Yoshida, Masaru

2011-09-01

The roles that amino acids play in immunity and inflammation are well defined, and the relationship between inflammatory bowel disease (IBD) and certain amino acids has recently attracted attention. In this study, the levels of amino acids and trichloroacetic acid (TCA) cycle-related molecules in the colonic tissues and sera of patients with ulcerative colitis (UC) were profiled by gas chromatography/mass spectrometry (GC/MS), with the aim of evaluating whether the clinical state induced by UC leads to variations in the amino acid profile. Colonic biopsy samples from 22 UC patients were used, as well as serum samples from UC patients (n = 13), Crohn's disease (CD) patients (n = 21), and healthy volunteers (n = 17). In the GC/MS-based profiling of amino acids and TCA cycle-related molecules, lower levels of 16 amino acids and 5 TCA cycle-related molecules were observed in the colonic lesion tissues of the UC patients, and the serum profiles of amino acids and TCA cycle-related molecules of the UC patients were different from those of the CD patients and healthy volunteers. Our study raises the possibility that GC/MS-based profiling of amino acids and TCA cycle-related molecules is a useful early diagnostic tool for UC.

Determination of six phthalates in polypropylene consumer products by sonication-assisted extraction/ GC-MS methods

International Nuclear Information System (INIS)

Wei, Chong Kian; Fung, Loke Chui; Pang, Michelle

2011-01-01

Studies on determination of six kinds of phthalates, for example dimethyl phthalate (DMP), diethyl phthalate (DEP), dibutyl phthalate (DBP), benzyl butyl phthalate (BBP), di-(2-ethylhexyl) phthalate (DEHP), and di-n-octyl phthalate (DnOP), in three kinds of plastic containers for food use, including food container, instant noodle cup and snack container, by gas chromatography in combination with mass spectrometry detector (GC-MS) in electronic ionization mode with selected-ion monitoring (SIM) acquisition method (GC-MS(EI-SIM)) have been carried out. Extraction, clean-up and analysis methods have been developed and optimized. Determination of samples were performed after sonication-assisted extraction with 1:9 toluene and dichloromethane, clean-up with Bio-Beads S-X8 gel-permeation column and analyzed by GC-MS methods. The characteristic ions, 163, 194 for DMP; 149, 177, 222 for DEP; 149, 233, 251 for DBP; 91, 149, 206 for BBP; 149, 176, 193 for DEHP; 149, 167, 279 for DNOP were chosen for quantitative studies. These techniques are possible to detect phthalates at the level of 1-70 mg/ kg. The overall recoveries were 79.2-91.1 % with relative standard deviation (R.S.D.) values at 3.1-11.3 %. Only DEHP was detected in the studied samples. (author)

Urinary Amino Acid Analysis: A Comparison of iTRAQ®-LC-MS/MS, GC-MS, and Amino Acid Analyzer

Science.gov (United States)

Kaspar, Hannelore; Dettmer, Katja; Chan, Queenie; Daniels, Scott; Nimkar, Subodh; Daviglus, Martha L.; Stamler, Jeremiah; Elliott, Paul; Oefner, Peter J.

2009-01-01

Urinary amino acid analysis is typically done by cation-exchange chromatography followed by post-column derivatization with ninhydrin and UV detection. This method lacks throughput and specificity. Two recently introduced stable isotope ratio mass spectrometric methods promise to overcome those shortcomings. Using two blinded sets of urine replicates and a certified amino acid standard, we compared the precision and accuracy of gas chromatography/mass spectrometry (GC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) of propyl chloroformate and iTRAQ® derivatized amino acids, respectively, to conventional amino acid analysis. The GC-MS method builds on the direct derivatization of amino acids in diluted urine with propyl chloroformate, GC separation and mass spectrometric quantification of derivatives using stable isotope labeled standards. The LC-MS/MS method requires prior urinary protein precipitation followed by labeling of urinary and standard amino acids with iTRAQ® tags containing different cleavable reporter ions distinguishable by MS/MS fragmentation. Means and standard deviations of percent technical error (%TE) computed for 20 amino acids determined by amino acid analyzer, GC-MS, and iTRAQ®-LC-MS/MS analyses of 33 duplicate and triplicate urine specimens were 7.27±5.22, 21.18±10.94, and 18.34±14.67, respectively. Corresponding values for 13 amino acids determined in a second batch of 144 urine specimens measured in duplicate or triplicate were 8.39±5.35, 6.23±3.84, and 35.37±29.42. Both GC-MS and iTRAQ®-LC-MS/MS are suited for high-throughput amino acid analysis, with the former offering at present higher reproducibility and completely automated sample pretreatment, while the latter covers more amino acids and related amines. PMID:19481989

Highly Efficient Performance and Conversion Pathway of Photocatalytic CH3SH Oxidation on Self-Stabilized Indirect Z-scheme g-C3N4/I3-BiOI.

Science.gov (United States)

Hu, Lingling; He, Huanjunwa; Xia, Dehua; Huang, Yajing; Xu, Jiarong; Li, Haoyue; He, Chun; Yang, Wenjing; Shu, Dong; Wong, Po Keung

2018-05-07

A self-stabilized Z-scheme porous g-C3N4/I3--containing BiOI ultrathin nanosheets (g-C3N4/I3--BiOI) heterojunction photocatalyst with I3-/I- redox mediator was successfully synthesized by a facile solvothermal method coupling with light illumination. The structure and optical properties of g-C3N4/I3--BiOI composites were systematically characterized by means of XRD, SEM, TEM, FT-IR, XPS, N2 adsorption/desorption, UV-vis DRS, PL. The g-C3N4/I3--BiOI composites, with heterojunction between porous g-C3N4 and BiOI ultrathin nanosheets, were firstly applied for the photocatalytic elimination of ppm-leveled CH3SH under LED visible light illumination. The g-C3N4/I3--BiOI heterojunction with 10% g-C3N4 showed a dramatically enhanced photocatalytic activity in removal of CH3SH compared with pure BiOI and g-C3N4, due to its effective interfacial charge transfer and separation. The adsorption and photocatalytic oxidation of CH3SH over g-C3N4/I3--BiOI were deeply explored by in situ DRIFTS, and the intermediates and conversion pathways were elucidated and compared. Furthermore, on the basis of reactive species trapping, ESR and Mott-Schottky experiments, it was revealed that the responsible reactive species for catalytic CH3SH composotion were h+, ·O2- and 1O2, thus, the g-C3N4/I3--BiOI heterojunction followed an indirect all-solid state Z-scheme charge transfer mode with self-stabilized I3-/I- pairs as redox mediator, which could accelerate the separation of photo-generated charge and enhance the redox reaction power of charged carriers simultaneously.

A Simple Method for Measuring Carbon-13 Fatty Acid Enrichment in the Major Lipid Classes of Microalgae Using GC-MS

Science.gov (United States)

Elahee Doomun, Sheik Nadeem; Loke, Stella; O’Callaghan, Sean; Callahan, Damien L.

2016-01-01

A simple method for tracing carbon fixation and lipid synthesis in microalgae was developed using a combination of solid-phase extraction (SPE) and negative ion chemical ionisation gas chromatography mass spectrometry (NCI-GC-MS). NCI-GC-MS is an extremely sensitive technique that can produce an unfragmented molecular ion making this technique particularly useful for stable isotope enrichment studies. Derivatisation of fatty acids using pentafluorobenzyl bromide (PFBBr) allows the coupling of the high separation efficiency of GC and the measurement of unfragmented molecular ions for each of the fatty acids by single quadrupole MS. The key is that isotope spectra can be measured without interference from co-eluting fatty acids or other molecules. Pre-fractionation of lipid extracts by SPE allows the measurement of 13C isotope incorporation into the three main lipid classes (phospholipids, glycolipids, neutral lipids) in microalgae thus allowing the study of complex lipid biochemistry using relatively straightforward analytical technology. The high selectivity of GC is necessary as it allows the collection of mass spectra for individual fatty acids, including cis/trans isomers, of the PFB-derivatised fatty acids. The combination of solid-phase extraction and GC-MS enables the accurate determination of 13C incorporation into each lipid pool. Three solvent extraction protocols that are commonly used in lipidomics were also evaluated and are described here with regard to extraction efficiencies for lipid analysis in microalgae. PMID:27845718

Implementation of AICAR analysis by GC-C-IRMS for anti-doping purposes.

Science.gov (United States)

Buisson, C; Frelat, C; Mongongu, C; Martinat, N; Audran, M

2017-11-01

AICAR (5-aminoimidazole-4-carboxamide-1-β-D-ribofuranoside), is a naturally occurring substance which is part to the World Anti-Doping Agency (WADA) Prohibited List. It is claimed to improve physical performance when administered as a supplement. As for other endogenous compounds such as steroids, the gas chromatography-combustion-isotope ratio mass spectrometry (GC-C-IRMS) analysis remains an efficient tool to differentiate endogenous substances from exogenous ones. A protocol was described in the literature for the analysis of AICAR by GC-C-IRMS. The aim of the present study was to implement this protocol in our laboratory and to propose solutions to avoid the difficulties encountered. The first point discussed in this study is the derivatization step. Due to the structure of the AICAR molecule, conventional derivatization for GC-C-IRMS such as acetylation could not be applied and silylation was preferred. The improvement of the derivatives stability was achieved thanks to several derivatization conditions tested. This adjustment led to a reproducible derivatization pattern with the 3-TMS form as major derivative product. The second point discussed in this study is the diminution of extracts' background noise. Indeed, the implementation of the published protocol was not easy due to high performance liquid chromatography (HPLC) problems encountered when concentrated urine was injected into our system. Also, too many interferences in the endogenous reference compound fractions were observed. The addition of both a wash step before the HPLC purification and a HPLC purification step for the endogenous reference compound (ERC) fraction allowed us to increase the robustness of the method. This study presents the modified protocol compared to the original protocol as well as the evaluation of the whole method performances. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

Efficient Photocatalytic Bilirubin Removal over the Biocompatible Core/Shell P25/g-C3N4 Heterojunctions with Metal-free Exposed Surfaces under Moderate Green Light Irradiation

Science.gov (United States)

Kang, Shifei; Qin, Hengfei; Zhang, Lu; Huang, Yongkui; Bai, Xia; Li, Xi; Sun, Di; Wang, Yangang; Cui, Lifeng

2017-03-01

Highly-monodispersed g-C3N4/TiO2 hybrids with a core/shell structure were synthesized from a simple room temperature impregnation method, in which g-C3N4 was coated through self-assembly on the commercially available Degussa P25 TiO2 nanoparticles. Structural and surface characterizations showed that the presence of g-C3N4 notably affected the light absorption characteristics of TiO2. The g-C3N4/TiO2 heterojunctions with metal-free exposed surfaces were directly used as biocompatible photocatalysts for simulated jaundice phototherapy under low-power green-light irradiation. The photocatalytic activity and stability of g-C3N4/TiO2 were enhanced relative to pure P25 or g-C3N4, which could be ascribed to the effective Z-scheme separation of photo-induced charge carriers in g-C3N4/TiO2 heterojunction. The photoactivity was maximized in the 4 wt.% g-C3N4-coated P25, as the bilirubin removal rate under green light irradiation was more than 5-fold higher than that under the clinically-used blue light without any photocatalyst. This study approves the future applications of the photocatalyst-assisted bilirubin removal in jaundice treatment under moderate green light which is more tolerable by humans.

Analysis of Endocrine Disrupting Pesticides by Capillary GC with Mass Spectrometric Detection

Directory of Open Access Journals (Sweden)

Svetlana Hrouzková

2012-09-01

Full Text Available Endocrine disrupting chemicals, among them many pesticides, alter the normal functioning of the endocrine system of both wildlife and humans at very low concentration levels. Therefore, the importance of method development for their analysis in food and the environment is increasing. This also covers contributions in the field of ultra-trace analysis of multicomponent mixtures of organic pollutants in complex matrices. With this fact conventional capillary gas chromatography (CGC and fast CGC with mass spectrometric detection (MS has acquired a real importance in the analysis of endocrine disrupting pesticide (EDP residues. This paper provides an overview of GC methods, including sample preparation steps, for analysis of EDPs in a variety of matrices at ultra-trace concentration levels. Emphasis is put on separation method, mode of MS detection and ionization and obtained limits of detection and quantification. Analysis time is one of the most important aspects that should be considered in the choice of analytical methods for routine analysis. Therefore, the benefits of developed fast GC methods are important.

Mechanistic Characteristics of Surface Modified Organic Semiconductor g-C3N4 Nanotubes Alloyed with Titania

Directory of Open Access Journals (Sweden)

Lan Ching Sim

2017-01-01

Full Text Available The visible-light-driven photocatalytic degradation of Bisphenol A (BPA was investigated using the binary composite of alkaline treated g-C3N4 (HT-g-C3N4 deposited over commercial TiO2 (Evonik Degussa GmbH, Essen, Germany. The existence and contribution of both TiO2 and g-C3N4/HT-g-C3N4 in the composite was confirmed through various analytical techniques including powder X-ray diffraction (XRD, high-resolution transmission electron microscopy (HRTEM, field emission scanning electron microscopy (FESEM, Fourier transform infrared spectroscopy (FTIR, X-ray photoelectron spectroscopy (XPS, ultraviolet-visible diffuse reflectance spectra (UV-vis-DRS, and photoluminescence (PL analysis. The results showed that the titania in the binary composite exhibited both pure rutile and anatase phases. The morphological analysis indicated that the spongy “morel-like” structure of g-C3N4 turned to nanotube form after alkaline hydrothermal treatment and thereby decreased the specific surface area of HT-g-C3N4. The low surface area of HT-g-C3N4 dominates its promising optical property and effective charge transfer, resulting in a deprived degradation efficiency of BPA two times lower than pure g-C3N4. The binary composite of HT-g-C3N4/TiO2 exhibited excellent degradation efficiency of BPA with 2.16 times higher than the pure HT-g-C3N4. The enhanced photocatalytic activity was mainly due to the promising optical band gap structure with heterojunction interface, favorable specific surface area, and good charge separation.

Mechanistic Characteristics of Surface Modified Organic Semiconductor g-C3N4 Nanotubes Alloyed with Titania

Science.gov (United States)

Sim, Lan Ching; Tan, Wei Han; Leong, Kah Hon; Bashir, Mohammed J. K.; Saravanan, Pichiah; Surib, Nur Atiqah

2017-01-01

The visible-light-driven photocatalytic degradation of Bisphenol A (BPA) was investigated using the binary composite of alkaline treated g-C3N4 (HT-g-C3N4) deposited over commercial TiO2 (Evonik Degussa GmbH, Essen, Germany). The existence and contribution of both TiO2 and g-C3N4/HT-g-C3N4 in the composite was confirmed through various analytical techniques including powder X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), field emission scanning electron microscopy (FESEM), Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), ultraviolet-visible diffuse reflectance spectra (UV-vis-DRS), and photoluminescence (PL) analysis. The results showed that the titania in the binary composite exhibited both pure rutile and anatase phases. The morphological analysis indicated that the spongy “morel-like” structure of g-C3N4 turned to nanotube form after alkaline hydrothermal treatment and thereby decreased the specific surface area of HT-g-C3N4. The low surface area of HT-g-C3N4 dominates its promising optical property and effective charge transfer, resulting in a deprived degradation efficiency of BPA two times lower than pure g-C3N4. The binary composite of HT-g-C3N4/TiO2 exhibited excellent degradation efficiency of BPA with 2.16 times higher than the pure HT-g-C3N4. The enhanced photocatalytic activity was mainly due to the promising optical band gap structure with heterojunction interface, favorable specific surface area, and good charge separation. PMID:28772387

Compound-specific nitrogen and carbon isotope analysis of nitroaromatic compounds in aqueous samples using solid-phase microextraction coupled to GC/IRMS.

Science.gov (United States)

Berg, Michael; Bolotin, Jakov; Hofstetter, Thomas B

2007-03-15

Solid-phase microextraction (SPME) coupled to gas chromatography/isotope ratio mass spectrometry was used to determine the delta15N and delta13C signatures of selected nitroaromatic contaminants such as the explosive 2,4,6-trinitrotoluene (TNT) for derivation of isotopic enrichment factors of contaminant transformation. Parameters for efficient extraction of nitroaromatic compounds (NACs) and substituted anilines from water samples were evaluated by SPME-GC/MS. delta13C signatures determined by SPME-GC/IRMS and elemental analyzer IRMS (EA-IRMS) were in good agreement, generally within +/-0.7 per thousand, except for 2,4-dinitrotoluene (2,4-DNT) and TNT, which showed slight deviations (IRMS were between 73 and 780 microg L-1 and correlated with the extraction efficiencies of the compounds determined by SPME-GC/MS. Nitrogen isotope measurements by SPME-GC/IRMS were of similar precision (standard deviations IRMS within +/-1.3 per thousand (+2.5 per thousand for TNT), but no systematic trend was found for the deviations. LODs of delta15N measurements ranged from 1.6 to 9.6 mg L-1 for nitrotoluenes, chlorinated NACs and DNTs (22 mg L-1 for TNT). The SPME-GC/IRMS method is well suited for the determination of isotopic enrichment factors of various NAC transformation processes and provides so far unexplored possibilities to elucidate behavior and degradation mechanisms of nitroaromatic contaminants in soils and groundwaters.

Photocatalysis and self-cleaning from g-C3N4 coated cotton fabrics under sunlight irradiation

Science.gov (United States)

Fan, Yunde; Zhou, Ji; Zhang, Jin; Lou, Yaqin; Huang, Zhenwu; Ye, Yong; Jia, Li; Tang, Bin

2018-05-01

Graphite-like carbon nitride (g-C3N4) nanosheets have been facilely assembled via electrostatic interaction onto cotton fabrics for achieving multi-functionalities. The surface morphologies, chemical composition and optical features of the g-C3N4-coated fabrics were characterized. The treated cotton fabrics exhibited remarkable photocatalytic degradation activity and superior self-cleaning performance. A complete degradation of Rhodamine B (RhB) and removal of stains were accomplished under simulated sunlight irradiation. More importantly, the modified fabrics can be reused in catalysis reactions with great durability. The practical treatment approach demonstrated from this work has great potential to be applied in textile industry for functional fabrics manufacture.

Computational study on the half-metallicity in transition metal—oxide-incorporated 2D g-C3N4 nanosheets

Science.gov (United States)

Gao, Qian; Wang, Hui-Li; Zhang, Li-Fu; Hu, Shuang-Lin; Hu, Zhen-Peng

2018-06-01

In this study, based on the first-principles calculations, we systematically investigated the electronic and magnetic properties of the transition metal-oxide-incorporated 2D g-C3N4 nanosheet (labeled C3N4-TM-O, TM = Sc-Mn). The results suggest that the TM-O binds to g-C3N4 nanosheets strongly for all systems. We found that the 2D C3N4-TM-O framework is ferromagnetic for TM = Sc, Ti, V, Cr, while it is antiferromagnetic for TM = Mn. All the ferromagnetic systems exhibit the half-metallic property. Furthermore, Monte Carlo simulations based on the Heisenberg model suggest that the Curie temperatures ( T c ) of the C3N4-TM-O (TM = Sc, Ti, V, Cr) framework are 169 K, 68 K, 203 K, and 190 K, respectively. Based on Bader charge analysis, we found that the origin of the half-metallicity at Fermi energy can be partially attributed to the transfer of electrons from TM atoms to the g-C3N4 nanosheet. In addition, we found that not only electrons but also holes can induce half-metallicity for 2D g-C3N4 nanosheets, which may help to understand the origin of half-metallicity for graphitic carbon nitride.

Desenvolvimento de método analítico de cromatografia líquida de alta eficiencia (CLAE para quantificação de lupeol em nanocápsulas poliméricas

Directory of Open Access Journals (Sweden)

Letícia Nasser Naves

2014-08-01

Full Text Available Um método de cromatografia líquida de alta performance simples, exato e preciso foi desenvolvido para a determinação do lupeol em nanocápsulas poliméricas. A separação cromatográfica foi realizada numa coluna Varian C8 (250 mm x 4,6 mm x 5 mm, mantida a 35°C, fase móvel constituída por acetonitrila e metanol acidificado com ácido acético a 0,1% (95:5 v/v, e taxa de fluxo de 1,2 mL/min, com um volume injeção de amostra de 20 µl e detecção UV a 210 nm, com o tempo de eluição de 6,2 min. O método proposto é linear para a faixa de concentração de 10 a 250 μg/ mL com coeficiente de correlação de 0,9996. As análises de exatidão e precisão demonstraram baixos valores de desvio padrão relativo (< 4,2%. A metodologia foi específica, linear, precisa, exata e robusta, se mostrando capaz de ser aplicada para quantificação de lupeol em nanocápsulas poliméricas.

Dereplication of pentacyclic triterpenoids in plants by GC-EI/MS.

Science.gov (United States)

Gu, Jian-Qiao; Wang, Yuehong; Franzblau, Scott G; Montenegro, Gloria; Timmermann, Barbara N

2006-01-01

Three common plant-derived pentacyclic triterpenoids, oleanolic acid (1), betulinic acid (2) and ursolic acid (3), have been found to exhibit moderate anti-tubercular activity in a microplate alamar blue assay. In order to facilitate the discovery of novel anti-tubercular leads with diverse chemical structures, a new and rapid GC-EI/MS method was developed simultaneously and unambiguously to dereplicate 1-3 as their methyl esters with limits of detection of 25.6, 26.9 and 26.8 ng, respectively.

Economics of LNG and pipeline gas export from GC C

International Nuclear Information System (INIS)

White, N.

1995-01-01

This paper briefly reviews the economic and non-economic considerations underlying gas exports from the GC C and the Arabian Peninsula in general. It addresses four themes: policy issues, political risks, technical risks and economics. It examines the distance between the regional resource areas and the major gas markets in the Far East and Europe, and examines the implications for moving gas to those markets in liquid form or by pipeline, in terms of number of LNG vessels required, and capital costs. (Author)

Phytochemical investigation GC-MS analysis and in vitro antimicrobial activity of Coleus forskohlii

Directory of Open Access Journals (Sweden)

Krishnamoorthy Rajkumar

2015-12-01

Full Text Available The aim of this study was to investigate the phytochemical constituents, gas chromatography-mass spectrometry (GC-MS analysis and antimicrobial activity of Coleus forskohlii. The different solvents such as ethanol, chloroform, acetone and aqueous extracts were identified pharmacologically as important bioactive compounds and their antimicrobial properties were studied. In the phytochemical investigation almost all the ethanol extract of leaf, stem and root having secondary metabolites like alkaloids, flavonoids, tannins, saponins, terpenoids, and steroids. The active constituents of the ethanol extract of C. forskohlii root was studied by GC-MS analysis. According to the antimicrobial results ethanol extract of C. froshkolii root showed highest antibacterial activity compared with stem and leaf. The highest antimicrobial activity was observed against Klebsiella pneumonia (19 mm and Candida albicans (16 mm in ethanol extract of root. Among the above extracts of leaf, stem and root, ethanol extract of root having antimicrobial activities due to the presence of phytoconstituents.

Analytical and sensorial characterization of the aroma of wines produced with sour rotten grapes using GC-O and GC-MS: identification of key aroma compounds.

Science.gov (United States)

Barata, André; Campo, Eva; Malfeito-Ferreira, Manuel; Loureiro, Virgílio; Cacho, Juan; Ferreira, Vicente

2011-03-23

In the present work, the aroma profiles of wines elaborated from sound and sour rot-infected grapes as raw material have been studied by sensory analysis, gas chromatography-olfactometry (GC-O), and gas chromatography-mass spectrometry (GC-MS), with the aim of determining the odor volatiles most likely associated with this disease. The effect of sour rot was tested in monovarietal wines produced with the Portuguese red grape variety Trincadeira and in blends of Cabernet Sauvignon and sour rotten Trincadeira grapes. Wines produced from damaged berries exhibited clear honey-like notes not evoked by healthy samples. Ethyl phenylacetate (EPhA) and phenylacetic acid (PAA), both exhibiting sweet honey-like aromas, emerged as key aroma compounds of sour rotten wines. Their levels were 1 order of magnitude above those found in controls and reached 304 and 1668 μg L(-1) of EPhA and PAA, respectively, well above the corresponding odor thresholds. Levels of γ-nonalactone also increased by a factor 3 in sour rot samples. Results also suggest that sour rot exerts a great effect on the secondary metabolism of yeast, decreasing the levels of volatiles related to fatty acids and amino acid synthesis. The highest levels of γ-decalactone of up to 405 μg L(-1) were also found in all of the samples, suggesting that this could be a relevant aroma compound in Trincadeira wine aroma.

Educational Program Improvement in Chemistry Through the Acquisition of GC/MS And FT-NMR Instruments

National Research Council Canada - National Science Library

Anderson, Gloria

1997-01-01

...), Department of Defense. The purpose of this grant was to enable the department to acquire instrumentation necessary for incorporating the theory and practice of Gas Chromatography/Mass Spectrometry (GC/MS...

First detection of an NSAID, flunixin, in sheep's wool using GC-MS

Energy Technology Data Exchange (ETDEWEB)

Richards, Ngaio, E-mail: ngaio.richards@anglia.ac.uk [Life Sciences, Anglia Ruskin University, East Road, Cambridge, CB1 1PT (United Kingdom); Hall, Sarah [Life Sciences, Anglia Ruskin University, East Road, Cambridge, CB1 1PT (United Kingdom); Scott, Karen [Forensic Medicine and Science, University of Glasgow, Glasgow G12 8QQ (United Kingdom); Harrison, Nancy [Life Sciences, Anglia Ruskin University, East Road, Cambridge, CB1 1PT (United Kingdom)

2011-05-15

Exposure to the nonsteroidal anti-inflammatory drug (NSAID) diclofenac resulted in the near extinction of three species of Gyps vultures on the Indian subcontinent. Other NSAIDs present in the environment, including flunixin, may pose a similar risk. In the course of a study to determine the feasibility of detecting NSAIDs in keratinous matrices (i.e., hair, nails and feathers) using GC-MS, wool opportunistically collected from a sheep treated with flunixin was analysed for residues. Flunixin was detected qualitatively in external wool wash and extract samples. While residues of veterinary agents and pesticides have previously been found in sheep's wool, our preliminary investigation provides the first instance of an NSAID being detected in this matrix. Here we provide the sample preparation methods and GC-MS parameters used to enable further refinement as part of ongoing conservation and consumer quality control measures. - Highlights: > In this study we qualitatively detected the NSAID flunixin in sheep's wool using GC-MS. > Potential applications of this technique to the conservation of avian scavengers are outlined. > The quantitative and confirmatory steps required to fully validate the method are also provided. - This is the first time that an NSAID has been investigated or detected in sheep's wool. As such, it details a novel exposure pathway for scavenging species in the environment and offers a potential tool for future monitoring effort in vulture conservation.

Determination of vitamins D2 and D3 in selected food matrices by online high-performance liquid chromatography-gas chromatography-mass spectrometry (HPLC-GC-MS).

Science.gov (United States)

Nestola, Marco; Thellmann, Andrea

2015-01-01

An online normal-phase liquid chromatography-gas chromatography-mass spectrometry (HPLC-GC-MS) method was developed for the determination of vitamins D2 and D3 in selected food matrices. Transfer of the sample from HPLC to GC was realized by large volume on-column injection; detection was performed with a time-of-flight mass spectrometer (TOF-MS). Typical GC problems in the determination of vitamin D such as sample degradation or sensitivity issues, previously reported in the literature, were not observed. Determination of total vitamin D content was done by quantitation of its pyro isomer based on an isotopically labelled internal standard (ISTD). Extracted ion traces of analyte and ISTD showed cross-contribution, but non-linearity of the calibration curve was not determined inside the chosen calibration range by selection of appropriate quantifier ions. Absolute limits of detection (LOD) and quantitation (LOQ) for vitamins D2 and D3 were calculated as approximately 50 and 150 pg, respectively. Repeatability with internal standard correction was below 2 %. Good agreement between quantitative results of an established high-performance liquid chromatography with UV detection (HPLC-UV) method and HPLC-GC-MS was found. Sterol-enriched margarine was subjected to HPLC-GC-MS and HPLC-MS/MS for comparison, because HPLC-UV showed strong matrix interferences. HPLC-GC-MS produced comparable results with less manual sample cleanup. In summary, online hyphenation of HPLC and GC allowed a minimization in manual sample preparation with an increase of sample throughput.

Sequencing and Analysis of the Pseudomonas fluorescens GcM5-1A Genome: A Pathogen Living in the Surface Coat of Bursaphelenchus xylophilus.