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Sample records for cromatografia gasosa gc

  1. Cromatografia gasosa bidimensional abrangente (GC × GC Comprehensive two-dimensional gas chromatography (GC × GC

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    Marcio Pozzobon Pedroso

    2009-01-01

    Full Text Available This paper presents the fundamental principles, instrumentation and selected applications of comprehensive two-dimensional gas chromatography (GC × GC. In this technique, introduced in 1991, two capillary columns are coupled and proper modulating interfaces continuously collect the eluate from the first column, transferring it to the second column. The result is a geometric increment in the chromatographic resolution, ensuring separation of extremely complex mixtures in time periods shorter or comparable to those of analysis using conventional gas chromatography and with better detectabilities and sensitivities.

  2. Caracterização de amostras petroquímicas e derivados utilizando cromatografia gasosa bidimensional abrangente (GCxGC Characterization of petrochemical samples and their derivatives by comprehensive two-dimensional gas chromatography

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    Carin von Mühlen

    2006-07-01

    Full Text Available The goal of this article is to discuss the application of comprehensive two-dimensional gas chromatography (GCxGC to petrochemical samples. The use of GCxGC for petroleum and petroleum derivatives characterization, through group type analysis, or BTEX (benzene, toluene, ethylbenzene, xylenes, total aromatic hydrocarbons, polyaromatic hydrocarbons, sulfur-containing, oxygen-containing, and nitrogen-containing compounds is presented. The capability of GCxGC to provide additional specific chemical information regarding petroleum processing steps, such as dehydrogenation of linear alkanes, the Fischer-Tropsch process, hydrogenation and oligomerization is also described. In addition, GCxGC analyses of petrochemical biomarkers and environmental pollutants derived from petrochemicals are reported.

  3. Uso da cromatografia gasosa bidimensional abrangente (GC×GC na caracterização de misturas biodiesel/diesel: aplicação ao biodiesel de sebo bovino

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    Maria Silvana A Moraes

    2011-01-01

    Full Text Available The growth of biodiesel market and the implementation of regulations related to biodiesel production and biodiesel/diesel blending has encouraged the development of appropriate analytical methods to control the composition of this type of mixture. In this study, an evaluation of the potential of GC×GC for the characterization of samples of beef tallow biodiesel and the composition of blends of biodiesel/diesel is presented. The methodology was applied to beef tallow biodiesel and its mixtures with petrodiesel, ranging from B2 to B50. Results allowed not only the identification and quantification of the biodiesel esters, but also the biodiesel percentage in biodiesel/diesel blends.

  4. Desenvolvimento de metodologia para determinação de 4-cloroanilina em frangos por cromatografia gasosa - espectrometria de massas: análise em tecidos tratados com digluconato de clorhexidina após o processamento térmico Methodology for 4-chloroaniline determination in poultry by GC-MS: analisys in chlorhexidine digluconate treated tissues after termical processing

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    Eduardo Vicente

    2003-12-01

    Full Text Available A degradação do antimicrobiano digluconato de clorhexidina (DGCH durante armazenamento ou processamento térmico pode formar a 4-cloroanilina (CA, um composto potencialmente carcinogênico. Conseqüentemente, o uso deste sanitizante para descontaminação de carcaças de frangos representa uma fonte de risco para o consumidor, devendo ser avaliada a presença da CA no produto tratado. Um método foi desenvolvido para determinação de resíduos de CA em tecidos de frangos. Após a extração com diclorometano, foi feita a limpeza do extrato em cartucho C18 e quantificação por cromatografia gasosa-espectrometria de massas (CG-EM, sem derivação. A recuperação média (89,2% - CV 9,9%. e o limite de detecção (1,8ng/g foram considerados satisfatórios para os propósitos do estudo. Em amostras tratadas com DGCH e não submetidas a processamento térmico, a quantidade de CA detectada foi relativamente baixa, e provavelmente se originou da solução de tratamento. A fritura e a cocção em forno convencional resultaram em níveis elevados de CA, enquanto que a cocção em panela de pressão não alterou os níveis de CA presentes na amostra crua. Em vista destes resultados e, considerando-se o potencial tóxico da CA, recomenda-se que estes dados sejam levados em consideração quando avaliada a utilização de DGCH como sanitizante de carcaças em abatedouros de aves.The degradation of the antimicrobial agent chlorhexidine digluconate (CHDG during storage or thermal process originates 4-chloroaniline (CA, a compound which is potentially carcinogenic. As the use of this sanitizing agent to decontaminate poultry carcasses in processing plants may represent a risk to the consumers, it is important to search for the presence of CA residues in the treated products. A method was developed to quantify CA in poultry tissues. After dichloromethane extraction, the extract was cleaned on a C18 cartridge and the quantitation was performed, without

  5. Identificação de compostos voláteis de maçãs (Malus domestica cultivar Fuji, por cromatografia gasosa-espectrometria de massas

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    JANZANNTTI Natália S.

    2000-01-01

    Full Text Available Os compostos voláteis da maçã cultivar Fuji foram estudados durante 2 anos consecutivos (1994 e 1995. O isolamento dos compostos voláteis da maçã Fuji foi feito utilizando-se uma técnica de enriquecimento dos voláteis do "headspace" em Porapak Q e eluição com hexano. Foram detectados 84 componentes voláteis na maçã Fuji, por cromatografia gasosa de alta resolução, dos quais trinta foram identificados por cromatografia gasosa-espectrometria de massas, aliada aos índices de Kovats. Os compostos majoritários foram os ésteres acetato de butila, acetato de 2-metil butila, acetato de hexila e o terpeno µ-farneseno. A classe química predominante, entre compostos voláteis na maçã Fuji, foi a dos ésteres.

  6. (E-2-Nonenal determination in brazilian beers using headspace solid-phase microextraction and gas chromatographic coupled mass spectrometry (HS-SPME-GC-MS Determinação de (E-2-nonenal em cervejas brasileiras utilizando microextração em fase sólida do headspace e cromatografia gasosa acoplada a espectrometria de massas

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    Rodrigo Scherer

    2010-05-01

    Full Text Available (E-2-nonenal is considered an important off-flavor of beer, related to the flavor of beer staling. In this study, a new method for determination of (E-2-nonenal in beer using headspace solid-phase microextraction and gas chromatographic coupled mass spectrometry (HS-SPME-GC-MS was developed and applied in Brazilian beer samples. The extractions were carried out in CAR-PDMS (carboxen-polydimethylsiloxane fiber and the best results were found with 15 minutes of equilibrium and 90 minutes of extraction at 50 °C. The method was linear in the range from 0.02 to 4.0 μg.L-1 with correlation coefficient of 0.9994. The limits of detection and quantification were 0.01 and 0.02 μg.L-1, respectively. 96.5% of recovery and 4% precision (RSD were obtained in the fortification of beer samples with 2.0 μg.L-1 of (E-2-nonenal. The developed method proved to be simple, efficient and highly sensitive to the determination of this analyte being easily applied in the quality control of the brewery. (E-2-nonenal was found in all beer samples analyzed with levels between 0.17 and 0.42 μg.L-1.O (E-2-nonenal é considerado um importante off-flavor da cerveja, sendo relacionado ao sabor de cerveja envelhecida. Neste estudo, um novo método para determinação de (E-2-nonenal em cerveja usando microextração em fase sólida do headspace e cromatografia a gás acoplada à espectrometria de massa (HS-SPME-GC-MS foi desenvolvido e aplicado em amostras de cerveja brasileira. As extrações foram realizadas utilizando a fibra CAR/PDMS (carboxen/polidimetilsiloxano, com 15 minutos de tempo de equilíbrio e 90 minutos de exposição da fibra a 50 °C. O método foi linear na faixa de 0,02 e 4,0 μg.L-1, com coeficiente de correlação de 0,9994. Os limites de detecção e quantificação foram 0,01 e 0,02 μg.L-1, respectivamente. Foram obtidos 96,5% de recuperação e 4% de variação entre replicatas de amostras de cerveja fortificadas com 2,0 μg.L-1 de (E-2-nonenal. O m

  7. Determinação da relação siringila/guaiacila da lignina em madeiras de eucalipto por pirólise acoplada à cromatografia gasosa e espectrometria de massas (PI CG/EM Determination of the siringyl/guaiacyl ratio in eucalyptus wood by pyrolysis-gas chroma-tography/mass spectrometry (PY-GC/MS

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    Luiz C. A. Barbosa

    2008-01-01

    Full Text Available The use of analytical pyrolysis combined with gas chromatography/mass spectrometry (Py-GC/MS to determine the syringyl/guaiacyl ratio (S/G in lignins from Eucalyptus spp woods was investigated. Sample of E. grandis and "E. urograndis" wood, with and without extractives, were subjected to pyrolysis from 300 ºC to 600 ºC. The products that results from pyrolysis were identified by mass spectrometry and the S/G ratio was determined based on the areas of the peaks corresponding to the guaiacyl and syringyl derivatives. The best S/G estimation is achieved when pyrolysis is carried out at 550 ºC. Extractives and carbohydrate present in the woods do not interfere with the results.

  8. Otimização e validação intralaboratorial de método para análise de resíduos de cloranfenicol em leite caprino por cromatografia gasosa com detecção por captura de elétrons (CG/DCE Optimization and intralaboratorial validation of method for analysis of chloramphenicol residues in goat milk by GC/ECD

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    Jaff R. da Silva

    2010-01-01

    Full Text Available The presence of chloramphenicol residues in goat milk can cause toxic effects in the population. The present work consists of the optimization and validation of analytical methodology for determination of chloramphenicol residues in goat milk by GC/ECD. The extraction was made with ethyl acetate and the clean-up with SPE-C18. The identification was made by comparison of retention time and GC/MS, and the quantification by external standard. The method was selective, linearity (0.998, precise (5.8-13.4%, exact (69.87-73.71% and robust. The LOD and LOQ of method were 0.030 and 0.10 μg/kg, respectively. The method was efficiently for analysis of chloramphenicol in goat milk.

  9. Determinação de efedrinas em urina por cromatografia em fase gasosa (CG/DNP para o controle da dopagem no esporte Gas chromatographic method for the determination of ephedrines in urine for doping control purposes

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    Paula Rodrigues Garcia

    2005-09-01

    Full Text Available Efedrinas são aminas simpatomiméticas componentes de diversas especialidades farmacêuticas, utilizadas no tratamento de doenças respiratórias devido à sua ação descongestionante e broncodilatora. Atualmente, diversos produtos comercializados como suplementos nutricionais contêm efedrinas e são amplamente utilizados no meio esportivo, com o objetivo de facilitar a queima de gorduras e melhorar o desempenho. Entretanto, o uso indiscriminado destas substâncias pode acarretar série de efeitos tóxicos como hipertensão, taquicardia, cefaléia e tremores. Devido à sua ação psicoestimulante, foram incluídas na lista de substâncias proibidas nas atividades esportivas pelo Comitê Olímpico Internacional (COI e estabelecidas concentrações na urina para o controle da dopagem (efedrina e metilefedrina: 10 µg/mL. O presente trabalho teve como objetivo a validação de um método para quantificação de efedrinas, por cromatografia em fase gasosa acoplada a detetor de nitrogênio/fósforo (CG/DNP, em amostras de urina com a finalidade de controle da dopagem. O método consistiu em extração líquido-líquido e posterior derivação das efedrinas com anidrido trifluoroacético, e demonstrou ser simples e prático, apresentando linearidade nas faixas de concentração estudadas. Amostras de urina de voluntários que relataram uso de efedrinas foram submetidas à análise pelo método proposto.Ephedrines are sympathomimetic amines present in many pharmaceutical preparations used in the treatment of respiratory diseases due to their actions against broncospasm and congestion. Nowadays, several products sold as nutritional supplements contain ephedrines and are widely used in a diverse range of sports as weight loss aids and enhancement of athletic performance. However, the abuse of ephedrines may lead to a number of adverse effects including hypertension, headache, tachycardia and seizure. Due to their CNS stimulating action, ephedrines are

  10. Determinação por cromatografia gasosa de açúcares em frutíferas de clima temperado Gas chromatography determination of sugars in temperate-zone fruit trees

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    Alexandre Couto Rodrigues

    2005-04-01

    Full Text Available As frutíferas de clima temperado apresentam o fenômeno da dormência. Na saída da dormência, há a conversão do amido para açúcares solúveis, como substrato para a retomada de crescimento na primavera. Visando à maior compreensão da fisiologia das plantas em respostas a eventos, como as variações climáticas, estresses e problemas de adaptação, desenvolveu-se este trabalho, no Laboratório de Fisiologia Vegetal da Embrapa Clima Temperado, com o objetivo de descrever uma metodologia para a determinação das concentrações dos açúcares solúveis (frutose, sorbitol, alfa-glicose, beta-glicose e sacarose, em tecidos vegetais de frutíferas, via cromatografia gasosa. O cromatógrafo utilizado para as análises dos açúcares por essa metodologia é o GAS CHROMATOGRAPH e a coluna do tipo Packed Column J. K. de 3,2mm de diâmetro por 2m de comprimento, empacotada com Silicone SE-52 Uniport HP 80/100 mesh. Através da cromatografia gasosa, obtêm-se eficiência e resolução cromatográfica, para análises de açúcares solúveis, sendo, desta forma, vantajoso e executável esse tipo de análise pelo método descrito.The temperate-zone deciduous fruit trees present the phenomenon of dormancy. In that period, there is the conversion of the starch in soluble sugars, as substratum for the resumption of growth in the spring. Seeking to better understanding the physiology of the plants in answers to events as the climatic variations, stresses and adaptation problems, this study was done in the Laboratory of Crop Physiology of Embrapa Temperate Climate, with the objective of describing a methodology for determination of concentrations of the soluble sugars (fructose, sorbitol, alpha-glucose, beta-glucose and sucrose, in tissues of fruit tree, through gaseous chromatography. The chromatograph used for the analyses of the sugars was the GAS CHROMATOGRAPH with the column of the type Packed Column J. K. of 3,2mm of diameter for 2m of length

  11. Determinação simultânea dos ácidos hipúrico e metil-hipúrico urinários por métodos cromatográficos: comparação entre cromatografia líquida de alta eficiência e cromatografia gasosa capilar Simultaneous determination of urinary hyppuric and methylhyppuric acids through chromatographic methods: comparation between high performance liquid chromatography and capilary gas chromatography

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    Zelaine Lima Silva

    2002-06-01

    Full Text Available O presente trabalho foi realizado objetivando-se comparar a eficiência de dois métodos analíticos, um por cromatografia líquida de alta eficiência (CLAE e outro por cromatografia em fase gasosa com coluna capilar (CG, na determinação conjunta do ácido hipúrico (AH e ácido metil-hipúrico (AMH em urina de indivíduos expostos ocupacionalmente ao tolueno e xileno. Após a validação analítica foi observado que o método CLAE apresentou melhores precisão intra e interensaio, porcentagem de recuperação e sensibilidade. Amostras de urina de trabalhadores expostos aos dois solventes em fábrica de tintas-látex foram analisadas pelos dois métodos validados e os resultados avaliados estatisticamente. Não se encontrou diferença significativa entre os valores de AH superiores a 1,0 g/g de creatinina, quando determinados pelos dois métodos cromatográficos. Esta similaridade não foi repetida quando os níveis de AH eram inferiores a 1,0 g/g de creatinina. Os valores de AMH nas amostras analisadas estavam, na maioria das vezes, abaixo do limite de deteção, razão pela qual não foi realizada a comparação estatística entre os mesmos.High performance liquid chromatography and capillary gas chromatography were compared for simultaneous measurement of hyppuric and methyl hyppuric acids in urine of workers co-exposed to toluene and xilene. Quantitative advantages offered by HPLC over capillary GC method are observed: better average recovery, wider dynamic interval in calibration curve and lower detection and quantification limits mainly when MHA measurement was performed. No significant difference was found between the values of HA higher than 1.0 g/g creatinine measured by the two chromatographic procedures. Regarding to MHA concentration the methods gave similar results and there was no significant difference between the values.

  12. Gas chromatography and photoacoustic spectroscopy for the assessment of soil greenhouse gases emissions Cromatografia gasosa e espectroscopia fotoacústica para avaliação das emissões de gases de efeito estufa do solo

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    Rodrigo da Silveira Nicoloso

    2013-02-01

    Full Text Available Assessments of soil carbon dioxide (CO2, methane (CH4, and nitrous oxide (N2O emissions are critical for determination of the agricultural practices' potential to mitigate global warming. This study evaluated the photoacoustic spectroscopy (PAS for the assessment of soil greenhouse gases (GHG fluxes in comparison to the standard gas chromatography (GC method. Two long-term experiments with different tillage and cropping systems over a Paleudult were evaluated using static chambers. PAS measurements of CO2 and N2O concentrations showed good relationship and linearity (R2=0.98 and 0.94, respectively with GC results. However, CH4 measurements were significantly affected by air sample moisture which interfered on CH4 detection by PAS. Overestimation of CO2 and N2O concentrations in air samples determined by PAS (14.6 and 18.7%, respectively were also related to sampling moisture. CO2 and N2O fluxes showed good agreement between methods (R2=0.96 and 0.95, respectively, though PAS overestimated fluxes by 18.6 and 13.6% in relation to GC results, respectively. PAS showed good sensitivity and was able to detect CO2 and N2O fluxes as low as 332mg CO2 m-2 h-1 and 21µg N2O m-2 h-1. PAS analyzer should be detailed calibrated to reduce humidity interference on CO2, CH4 and N2O concentrations measurements avoiding overestimation or erroneous determination of soil GHG fluxes.As avaliações das emissões de dióxido de carbono (CO2, metano (CH4 e óxido nitroso (N2O do solo são fundamentais para a determinação do potencial de práticas agrícolas em mitigar o aquecimento global. Este estudo avaliou a espectroscopia fotoacústica (EFA para a determinação dos fluxos de gases de efeito estufa (GEE do solo em comparação com o método padrão de cromatografia gasosa (CG. Dois experimentos de longa duração com diferentes sistemas de preparo do solo e rotação de culturas sobre um Argissolo foram avaliados usando câmaras estáticas. As medidas das

  13. Softwares for comprehensive two-dimensional gas chromatography (GC x GC)

    OpenAIRE

    2010-01-01

    Resumo: A Cromatografia Gasosa Bidimensional Abrangente (GCxGC) é uma técnica analítica capaz de separar e detectar centenas de picos, sendo aplicada a diferentes amostras petroquímicas, ambientais e biológicas. Esta técnica se diferencia da Cromatografia Gasosa (GC) pela utilização de duas colunas cromatográficas de composições e dimensões diferentes conectadas em série e de uma interface para a coleta das frações da primeira coluna e para a reinjeção na segunda em períodos regulares, denomi...

  14. FASES ESTACIONÁRIAS DE LÍQUIDOS IÔNICOS EM CROMATOGRAFIA GASOSA: FUNDAMENTOS, AVANÇOS RECENTES E PERSPECTIVAS

    OpenAIRE

    2016-01-01

    Since their original discovery in 1914, ionic liquids (IL) have been widely examined and explored in chemistry due to their unique physical and chemical properties. Ionic liquids are collectively known as organic salts and have melting points of 100 °C or under. The molten salts most employed in analytical chemistry, including gas chromatography (GC), consist of an organic cation paired with an organic or inorganic anion. This class of materials exhibits negligible vapor pressure and may have...

  15. IDENTIFICAÇÃO DE COMPOSTOS ORGÂNICOS EM LIXIVIADO DE ATERRO SANITÁRIO MUNICIPAL POR CROMATOGRAFIA GASOSA ACOPLADA A ESPECTROMETRIA DE MASSAS

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    Eliane Sloboda Rigobello

    2015-07-01

    Full Text Available The organic compounds present in leachate can contaminate soil, superficial and underground water, and the majority is considered harmful to the environment and human health. The objective of this study was to identify organic compounds present in landfill leachate located in Maringá-PR by gas chromatography coupled to mass spectrometry (GC-MS. The raw leachate was characterized by measurements of pH, Chemical Oxygen Demand (COD, Biochemical Oxygen Demand (BOQ, Dissolved Organic Carbon (DOC, apparent and true colors, turbidity and absorbance at 254 nm. The extraction of organic compounds in leachate was carried out by liquid-liquid extraction (LLE with ethyl acetate and dichloromethane solvents, while varying the pH and ionic strength. The analysis of the leachate by GC-MS showed the presence of compounds considered to have toxic effects on the environment and human health, such as pesticides and phenolic compounds. Several compounds containing oxygenated groups such as carboxylic acids and alcohols were also identified, indicating that it was highly probable that the decomposition of waste in the landfill was in the acidogenic phase.

  16. Determinação da pressão de vapor de compostos orgânicos por cromatografia gasosa Determination of vapor pressure of organic compounds by gas chromatography

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    Fabrício P. Povh

    2006-06-01

    Full Text Available O conhecimento das pressões de vapor dos compostos naturais e suas propriedades críticas, de grande interesse para a extração supercrítica e impregnação de polímeros pelo processo supercrítico, é imprescindível para se fazer a modelagem termodinâmica do equilíbrio de fases. No entanto, a escassez de dados experimentais desses compostos, devida à alta volatilidade, ou facilidade à degradação em temperaturas baixas, requer a utilização de métodos especiais. Neste trabalho, determinaram-se as pressões de vapor da curcumina, nicotina, d-limoneno, beta-mirceno, citronelal e linalol, através de um método que utiliza medidas de tempo de retenção por cromatografia gasosa. Utilizou-se detector de ionização de chama e coluna em fase estacionária não polar, em condições isotérmicas. O método apresenta vantagens em relação a outros métodos, quanto à rapidez de análise, quantidade e repetibilidade das amostras. Para as determinações das pressões de vapor destes compostos naturais requer-se o conhecimento da temperatura normal de ebulição, ou temperatura de fusão e das pressões de vapor dos homólogos dos compostos analisados.The knowledge of the vapor pressures of natural compounds, as well as their critical properties are of great interest for the application of supercritical extraction and supercritical impregnation dye, and necessary for the thermodynamic modeling of equilibria phase. The scarcity of experimental data for these compounds results from their low volatility or easiness to degrade at low temperatures, therefore, requires the use of special methods. In this work, the vapor pressures of curcumin, nicotine, d-limonene, ß-myrcene, citronellal and linalool were determined through a method based on the retention time in a gas chromatographer column. A flame ionization detector and a column with non-polar stationary phase were used, under isothermal conditions. This method has the advantages of giving

  17. FASES ESTACIONÁRIAS DE LÍQUIDOS IÔNICOS EM CROMATOGRAFIA GASOSA: FUNDAMENTOS, AVANÇOS RECENTES E PERSPECTIVAS

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    Leandro W. Hantao

    2016-01-01

    Full Text Available Since their original discovery in 1914, ionic liquids (IL have been widely examined and explored in chemistry due to their unique physical and chemical properties. Ionic liquids are collectively known as organic salts and have melting points of 100 °C or under. The molten salts most employed in analytical chemistry, including gas chromatography (GC, consist of an organic cation paired with an organic or inorganic anion. This class of materials exhibits negligible vapor pressure and may have their properties (e.g.thermal stability and selectivity structurally tuned by imparting different moieties to the cation/anion. Currently, there are an estimated 1018possible combinations of IL. In this context, the prospection of highly selective IL-based stationary phases for gas-liquid chromatography has enabled high peak capacity and efficient separations of many critical pairs in complex samples. In this review, we present and discuss fundamental characteristics of ionic liquids and introduce important solvation models for gas-liquid systems. In addition, recent advances and applications of IL in conventional and multidimensional gas chromatography are outlined.

  18. Determinação de fenol urinário por cromatografia em fase gasosa em trabalhadores que utilizam resinas fenólicas em fundições Determination of urinary phenol by gas chromatography in workers using phenolic resins in foundries

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    Tiago Severo Peixe

    2006-06-01

    Full Text Available O fenol é utilizado na indústria como agente desinfetante no preparo de resinas fenólicas e pigmentos de tintas. Apresenta-se no estado sólido à temperatura ambiente, com coloração fracamente rósea, odor acre e higroscópico. Na exposição ocupacional aguda o composto pode levar a lesões eritematosas e, cronicamente, afetar a maturação celular no compartimento medular ósseo devido à formação de quinonas livres e 1,4-benzoquinona, proveniente do metabolismo hepático da hidroquinona via CYP2E1. A monitorização biológica possui relevância nas situações de exposições ocupacionais. Para tal, utiliza-se o fenol urinário, considerado bioindicador de exposição a este composto. O objetivo do presente trabalho foi validar uma técnica de extração líquido-líquido para quantificar o fenol urinário, por meio da cromatografia em fase gasosa com detetor de ionização por chama (CG/DIC em urina de trabalhadores expostos ao fenol em fundições. O método mostrou-se linear de 5 a 200 µg/mL; coeficiente de regressão linear (r² de 0,999; limites de detecção e quantificação 2,0 e 5,0 µg/mL, respectivamente; precisão intra-ensaio entre 4,5 e 8,9% e inter-ensaio entre 5,7 e 14,2%; exatidão entre 6,2 e 11,9% e recuperação superior a 87%. O método demonstrou ser simples e rápido. Amostras provenientes de trabalhadores expostos ao fenol foram analisadas comprovando a aplicação da técnica na monitorização biológica.Phenol is used as an industrial chemical, disinfectant agent, in the preparation of phenolic resins and paint pigments. When in solid state, it shows a light pink color, ocre odor, and is hygroscopic. In acute occupational exposure, the compound can produce erythemic injuries and burn sensation and, chronically, affect the cellular maturation of bone marrow due the free quinones and 1,4-benzoquinone, deriving from hepatic metabolism of the hydroquinone by P450 isozyme (CYP2E1. The biological monitoring is

  19. Validação de método para determinação de 3,4-metilenodioximetanfetamina (MDMA em comprimidos de ecstasy por cromatografia em fase gasosa Validation of a gas-chromatographic method for the determination of 3,4-methylenedioxymethamphetamine(MDMA in ecstasy tablets

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    Silvio Fernandes Lapachinske

    2004-03-01

    Full Text Available O ecstasy é comercializado, de maneira ilegal, normalmente sob a forma de comprimidos, com cores, aspectos, dimensões e logotipos variados. Quimicamente, é a metilenodioximetanfetamina (MDMA, um composto sintético com propriedades estimulante central e alucinogênicas. Devido à grande expansão do abuso de ecstasy, também tem aumentado o número de casos de intoxicações, decorrentes diretamente da droga (MDMA e análogas e/ou de eventuais adulterantes. Algumas substâncias análogas à MDMA, já identificadas em comprimidos de ecstasy são: metilenodioxietilanfetamina (MDEA, metilenodioxianfetamina (MDA, metanfetamina e anfetamina. Como possíveis adulterantes, geralmente são encontradas cafeína e efedrinas. O objetivo deste trabalho foi a validação de um método analítico para quantificar a MDMA em comprimidos ou cápsulas de ecstasy, através da cromatografia em fase gasosa com detector de nitrogênio/fósforo (GC/NPD. Além disso, substâncias análogas à MDMA e adulterantes também foram identificados. O método, que consiste na dissolução direta da amostra em metanol, centrifugação e diluição do sobrenadante, demonstrou ser simples, rápido e eficiente. Os limites de detecção e quantificação para a MDMA foram respectivamente de 1,5 e 3,0 mg/100 mg de comprimido. Amostras de comprimidos e cápsulas apreendidos como sendo ecstasy provenientes de 25 lotes foram analisadas, apresentando considerável variabilidade na composição e na quantidade de MDMA.Ecstasy is illegally commercialized in the form of tablets with different aspects, colors, sizes, and logotypes. Chemically, ecstasy is 3,4-methylenedioxymethamphetamine (MDMA, a synthetic compound with stimulant and hallucinogenic proprieties. Due to the great expansion of ecstasy abuse, the number of cases of intoxications by MDMA, analogs and eventual adulterant compounds has also increased. Some MDMA analog substances, such as 3,4-methylenedioxyethylamphetamine (MDEA

  20. Avaliação de características dos ácidos húmicos de resíduos de origem urbana: II. métodos termodegradativos (pirólise acoplada à cromatografia gasosa / espectrometria de massa

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    L. P. Canellas

    2000-12-01

    Full Text Available Este trabalho objetivou investigar as principais unidades estruturais de ácidos húmicos obtidos do composto de resíduos sólidos urbano (AH-CRSU e lodo de estação de tratamento de esgoto (AH-LETE por meio da pirólise acoplada à cromatografia gasosa / espectrometria de massas. Os ácidos húmicos extraídos do lodo da estação de tratamento de esgotos apresentaram maior quantidade de mono e diaril ésteres de massa mais elevada. Os n-alcanos presentes nos AH-LETE revelaram-se de cadeia mais curta do que nos AH-CRSU. Foram incorporados na estrutura dos AH fragmentos de ftalatos, provavelmente em virtude da contaminação da matéria orgânica por plásticos. Os compostos aromáticos presentes nos AH-LETE originaram-se, principalmente, de derivados do naftaleno e derivados do benzeno com substituição por cadeias alifáticas maiores do que AH-CRSU. Os compostos nitrogenados presentes mostraram-se essencialmente heteroaromáticos e os oxigenados furanos substituídos originados da degradação de carboidratos. Os compostos oxiaromáticos predominantes foram fenóis substituídos.

  1. Evaluation of noni (Morinda citrifolia volatile profile by dynamic headspace and gas chromatography-mass spectrometry Avaliação do perfil de voláteis em noni (Morinda citrifolia por headspace dinâmico e cromatografia gasosa-espectrometria de massas

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    Adriana Sousa

    2010-09-01

    Full Text Available Noni is a fruit that has interested the scientific community due to its medicinal and functional activities. Different products that contain noni are already in the market, but their consumption could be impaired by their distinctive unpleasant aroma and flavor. The aim of this work was to evaluate the noni pulp volatile profile by dynamic headspace and gas chromatography-mass spectrometry. Thirty seven volatile compounds were detected, mainly alcohols (63.3%, esters (26.9%, cetones (7.4%, and acids (1.2%.O noni é um fruto que tem interessado à comunidade científica por sua atividade funcional e medicinal. Já se encontram no mercado diferentes produtos que contêm noni em sua composição, mas seu consumo tem sido prejudicado por seu aroma e sabor desagradáveis. O objetivo deste trabalho foi o de avaliar o perfil de voláteis da polpa de noni pela técnica de headspace dinâmico e cromatografia gasosa-espectrometria de massas. Foram detectados 37 compostos voláteis, sendo os principais: alcoóis (63,3%, ésteres (26,9%, cetonas (7,4% e ácidos (1,2%.

  2. Determinação dos níveis plasmáticos do ácido valpróico (ácido dipropilacético por cromatografia em fase gasosa

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    Lolita M. Tsanaclis

    1981-09-01

    Full Text Available Foi padronizado um método de determinação dos níveis plasmáticos do ácido valpróico por cromatografia a gás. Trata-se de método rápido e exato, que evita etapas como evaporação ou derivação. O padrão empregado foi o sal sódico do ácido valpróico em solução aquosa, cuja concentração exata é determinada através de titulação potenciométrica com ácido perclórico. O método foi avaliado, ao se submeter um plasma controle, às condições de análise.

  3. Cromatografia gasosa ultrarrápida: uma visão geral sobre parâmetros, instrumentação e aplicações Ultra fast gas chromatography: an overview of the main parameters, instrumentation and applications

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    Rodrigo Sequinel

    2010-01-01

    Full Text Available Since the introduction of GC there has been an ongoing interest in reducing time of analysis resulting in new terms and definitions such as ultra fast gas chromatography (UF-GC. One of the most used definitions describes UF-GC as a technique that combines the employment of short narrow bore column with very fast temperature programming rates producing chromatographic peaks in the range of 50 ms and allowing separations times in 1-2 min or less. This paper summarizes the analytical approaches, the main parameters involved and the instrumentation towards UF-GC.

  4. Identificação de compostos orgânicos e farmacêuticos em esgoto hospitalar utilizando cromatografia gasosa acoplada a espectrometria de massa Identification of organic and pharmaceutical compositions in hospital wastewater using a gas chromatograph coupled to mass spectrometry

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    Francisco Vieira Paiva

    2011-03-01

    Full Text Available Os resíduos líquidos provenientes dos estabelecimentos assistenciais de saúde são mais complexos do que os esgotos domésticos. Sua composição contém inúmeros compostos farmacêuticos, saneantes, elementos radiativos e de laboratórios. O conhecimento desses compostos pode auxiliar na escolha do tratamento adequado para esses esgotos e diminuir os impactos ambientais nos corpos receptores. A pesquisa foi realizada utilizando um sistema combinado (UASB e lodos ativados para tratar a água residuária de um hospital. Neste trabalho, foram realizadas análises físico-químicas para caracterização do esgoto e cromatografia gasosa acoplada à espectrometria de massa para identificação de compostos químicos farmacêuticos, podendo-se constatar a presença de inúmeros elementos residuais dos fármacos usados no hospital.Liquid waste residues from health care establishments are more complex than those from residential sewage. Their composition contains several pharmaceutical chemical composites, sanitizers, radioactive, and laboratorial elements. Knowing about these composites may aid in choosing the proper treatment for these sewages, and diminish the environmental impact in receptors. The study was carried out in a combined system (UASB and activated sludge to treat a hospital wastewater. In this experiment, material and chemical analyses were employed to trace sewage characteristics and gas chromatography associated with mass spectrometry to identify pharmacologic chemical composites, where innumerous residual elements were found in chromatographs.

  5. Comparação entre métodos de quantificação em cromatografia gasosa: um experimento para cursos de química Comparison of quantification methods in gas chromatography: an experiment for chemistry courses

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    Carolina Bastos Pereira Ligiero

    2009-01-01

    Full Text Available This article describes an experiment designed to teach quantitative determination in gas chromatography (GC in Organic and Analytical Chemistry practical classes. The experiment consisted of extracting and analyzing eugenol from clove seeds to perform a quantitative approach aimed at comparing results obtained by external and internal calibration procedures. Therefore, this experiment proved to be very effective tool to enhance students awareness on the need to understand different types of calibration in GC and on how to avoid common experimental errors, and to find the best ways to eliminate their interference during the quantitative analysis phase.

  6. 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)

  7. Análise dos compostos voláteis da aguardente de cana por concentração dinâmica do "headspace" e cromatografia gasosa-espectrometria de massas The analysis of volatile compounds from Brazilian sugar cane spirit by dynamic headspace concentration and gas chromatography-mass spectrometry

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    Ian Carneiro da Cunha Nóbrega

    2003-08-01

    Full Text Available Os compostos voláteis da aguardente de cana foram extraídos por meio da concentração dinâmica do "headspace" em armadilhas contendo Tenax-TA e analisados por cromatografia gasosa-espectrometria de massas. Cerca de 100 compostos voláteis, com número de carbonos que variavam de 5 a 18, foram detectados. Destes, 22 foram selecionados, sendo 18 ésteres, com base nas suas quantidades no extrato ou nas suas características sensoriais obtidas na literatura. Os compostos presentes em maiores quantidades foram o 3-metil-1-butanol (álcool isoamílico, 1,1-dietoxi-etano (acetaldeído dietil acetal e os ésteres acetato de 3-metilbutila, hexanoato de etila, octanoato de etila, decanoato de etila e dodecanoato de etila. Dentre os compostos identificados em menor quantidade, destacou-se, devido a sua natureza química, o composto sulfurado 4,5-de-hidro-2-metil-3(2H-tiofenona. Esta é a primeira vez que este e outros compostos voláteis são reportados em aguardente de cana. Conclui-se que a metodologia empregada neste trabalho permitiu a identificação de compostos voláteis da fração C5-C18, que potencialmente contribuem para o aroma da aguardente de cana.The volatile compounds of Brazilian sugar cane spirit, the fermented and distilled juice of sugar cane, were extracted by dynamic headspace concentration on Tenax-TA trap and analyzed by gas chromatography-mass spectrometry. Approximately 100 volatile compounds with carbon number ranging from 5 to 18 were detected. Among these, 18 esters and 4 compounds from other chemical classes were selected for this work on the basis of their quantity in the extract or their sensory qualities obtained from literature. The major compounds identified were 3-methyl-1-butanol (isoamyl alcohol, 1,1-diethoxy-ethane (acetaldehyde diethyl acetal and the esters 3-methylbutyl acetate, ethyl hexanoate, ethyl octanoate, ethyl decanoate and ethyl dodecanoate. In minor quantities, potentially important aroma compounds

  8. 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.

  9. Separação e determinação quantitativa dos alcanos lineares e dos cíclicos/ramificados em petróleos brasileiros por aduto de ureia e cromatografia gasosa: um estudo de caso revisitado

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    Elaine Marotta

    2014-01-01

    Full Text Available A complete analysis of oils and their fractions allows correlations to be defined between their composition and derivatives or related geological materials. This work focused on optimization and implementation of a method for separation and quantification of n-alkanes in Brazilian oil samples by urea adduction and GC-FID techniques. Ten samples with different ºAPI were analyzed in triplicate to quantify individual n-alkanes and cyclic/branched alkane fraction. For individual quantification of n-alkanes, internal standardization with deuterated n-tetracosane was used. The use of urea adduction for the separation and quantification of n-alkanes was highly effective, with recovery values of above 80%.

  10. Determination of fluconazole in serum and amniotic fluid of rats by gas-chromatography/mass spectometry (GC/MS Determinação de fluconazol em soro e líquido amniótico de ratas por cromatografia a gas/espectrometria de massas (CG/EM

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    Dione Marçal Lima

    2005-06-01

    Full Text Available Rats treated with oral dose of 100 mg/kg of fluconazole during pregnancy had their serum and amniotic fluid quantified for this drug using a GC/MS method. Fluconazole was extracted with ethyl acetate from samples and analysed by a GC-MS Shimadzu QP5050A system using a CBP-5 fused silica capillary column. Tioconazole was used as internal standard. Calibration curve was linear within the range 10.0 - 300.0 µg/mL. The limit of quantification was 0.1 µg/mL and no interference was observed in the blank serum and amniotic liquid. The mean concentrations of the drug in the serum and amniotic fluid were 206.01 ± 105.25 µg/mL and 125.34 ± 65.24 mug/mL, respectively. This procedure showed to be sensitive and efficient enough for the use in teratogenic studies of fluconazole and other azole drugs.Soro e líquido amniótico de ratas tratadas com fluconazol (dose oral de 100 mg/kg durante a prenhez foram quantificados para este fármaco usando cromatografia gasosa acoplada à espectroscopia de massas (CG/EM. O fluconazol foi extraído das amostras com acetato de etila e analisado empregando-se um cromatógrafo CG/EM Shimadzu QP5050A com coluna capilar de sílica fundida CBP-5. O tioconazol foi utilizado como padrão interno. A curva padrão foi linear no intervalo das concentrações de 10,0 a 300,0 µg/mL. O limite de quantificação foi de 0,1 µg/mL e não foi observada interferência no branco de soro e líquido amniótico. As concentrações médias do fármaco no soro e líquido amniótico foram 206,01 ± 105,25 µg/mL e 125,34 ± 65,24 µg/mL, respectivamente. Este procedimento mostrou-se sensível e eficiente para ser usado em estudos de teratogenicidade do fluconazol e outros azóis.

  11. A validated capillary gas chromatography method for guaco (Mikania glomerata S. quality control and rastreability: from plant biomass to phytomedicines Método validado por cromatografia gasosa capilar para o controle de qualidade e rastreabilidade de guaco (Mikania glomerata S.: da matéria-prima ao fitoterápico

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    Paula C. P. Bueno

    2009-03-01

    Full Text Available This work describes a full validation of a capillary gas chromatography analytical methodology using internal standardization for the quantification of coumarin (1,2-benzopyrone in guaco (Mikania glomerata Spreng - Asteraceae products: syrup, plant and its extract, including the stability study of the phytomedicine. For the analysis, it was used an HP-5 capillary column (30 m x 0.32 mm x 0.25 µm, hydrogen at a flow rate of 1.8 mL/min and the increasing temperature gradient was: 100 ºC to 250 ºC, 15 ºC/min. The temperature of injector (split 1:20 and detector were kept at 250 ºC and 270 ºC, respectively. The retention times of the standards for the above conditions were 2.86 minutes for 1, 2, 3, 4-tetramethylbenzene, 4.45 min for piperonal (internal standards, and 5.36 minutes for coumarin. After extraction procedure, the recovery of coumarin determined for plant raw material was 101.6 %, while for syrup it was 100.8 %. Detection and quantification limits were 0.5 µg/mL and 1.5 µg/mL, respectively. Precision was determined for all samples and the results were lower than 2.5 %. The total amount of coumarin in plant raw material, its extract and syrup were 0.38% w/w, 1.33 mg/mL and 0.143 mg/mL, respectively.Este trabalho descreve a validação completa de metodologia analítica empregando cromatografia gasosa capilar com padronização interna para quantificação da cumarina (1,2-benzopirona em produtos contendo guaco (Mikania glomerata Spreng - Asteraceae: xarope, planta e extrato padronizado, além do estudo de estabilidade do fitoterápico em questão. Utilizou-se uma coluna capilar HP-5 (30 m x 0,32 mm x 0,25 µm, hidrogênio a 1,8 mL/min e rampa de temperatura de 100 ºC a 250 ºC, a 15 ºC/min. A temperatura do injetor (split 1:20 foi de 250 ºC, enquanto a do detector foi de 270 ºC. Os tempos de retenção dos padrões foram: 2,86 minutos para o 1, 2, 3, 4-tetrametilbenzeno, 4,45 minutos para o piperonal (padrões internos e 5

  12. 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

  13. 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.

  14. 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.

  15. 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

    OpenAIRE

    Vanessa de Menezes Prata; Elissandro Soares Emídio; Haroldo Silveira Dórea

    2011-01-01

    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 dat...

  16. 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.

  17. Extração de ácido trans-trans mucônico urinário com polímeros de impressão molecular e análise por cromatografia gasosa: espectrometria de massas

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    Lidiane Silva Franqui

    2012-01-01

    Full Text Available This paper describes selective molecularly imprinted solid-phase extraction of ttMA from urine samples followed by derivatization and analysis by gas chromatography/mass spectrometry (GC/MS. The analytical calibration curve ranged from 0.3 to 7.0 mg L-1 (r = 0.999 and the limit of quantitation (LOQ was 0.3 mg L-1. The method was applied for the determination of ttMA in urine samples from smokers and concentrations detected ranged from < LOQ to 1.64 mg L-1. Thus, the proposed method proved adequate for the determination of urinary ttMA in the biomonitoring of occupational exposure to low levels of benzene.

  18. Hifenação das técnicas de extração sólido-líquido com partição a baixa temperatura(SLE/LTP) e microextração líquido-líquido dispersiva com solvente de baixa densidade (LDS/DLLME) para determinação de agrotóxicos em solos por GC/ECD

    OpenAIRE

    Noronha, Luiz Manoel Silva de

    2014-01-01

    Procedimentos de extração baseados nos princípios da química verde tem sido desenvolvidos desde 1990, com a miniaturização tendo um papel importante. A combinação da técnica extração sólido-líquido com partição em baixa temperatura (SLE/LTP) e a microextração líquido-líquido dispersiva com solvente de baixa densidade (LDS/DLLME), juntamente com a cromatografia gasosa com detector por captura de elétrons (GC/ECD) foi utilizada para a determinação de 2 agrotóxicos organofosforados e 4 piretróid...

  19. Two fast screening methods (GC-MS and TLC-ChEI assay for rapid evaluation of potential anticholinesterasic indole alkaloids in complex mixtures

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    Ivo J.C. Vieira

    2008-09-01

    associadas de modo a identificar facilmente novos inibidores colinesterásicos. A cromatografia em fase gasosa acoplada a espectrometria de massas (CG-EM das frações alcaloídicas apolares, obtidas da extração ácido-base do caule de T. laeta, revelou a presença de treze alcalóides monoindólicos, quatro deles confirmados por co-injeção com padrões previamente isolados. Os outros alcalóides foram tentativamente identificados pelo padrão de fragmentação de massas. Por cromatografia em fase gasosa com detecção por ionização de chama (CG-DIC e utilizando isatina como padrão interno, affinisina e voachalotina foram identificadas como substâncias majoritárias. As frações alcaloídicas obtidas e os quatorze alcalóides previamente isolados das raízes de T. laeta e T. hystrix foram analisados quanto à atividade inibitória das enzimas acetil (AChE e butirilcolinesterase (BuChE pelo método de Ellman em cromatografia em camada delgada (CCD-ChEI. Os resultados revelaram uma inibição seletiva dos alcalóides heyneanina e Nb-metilvoachalotina para BuChE e de 19-epi-isovoacristina para AChE, enquanto que olivacina, affinisina, ibogamina, affinina, conodurina e hystrixnina inibiram ambas as enzimas. Além de confirmar que alcalóides indólicos monoterpênicos são agentes terapêuticos promissores para o tratamento da DA, este é o primeiro relato da atividade anticolinesterásica de olivacina, um alcalóide piridocarbazólico.

  20. Characterization of the main automotive gasoline compounds by using gas chromatography; Caracterizacao dos principais componentes da gasolina automotiva atraves de cromatografia gasosa

    Energy Technology Data Exchange (ETDEWEB)

    Assis, Julio Cesar Rosa; Jaeger, Helena Valli; Almeida, Selmo Queiroz; Teixeira, Leonardo Sena Gomes; Pontes, Luiz Antonio Magalhaes; Vitor Sobrinho, Eledir; Guimaraes, Paulo Roberto Britto; Vianna, Regina Ferreira [Universidade Salvador - UNIFACS, Salvador, BA (Brazil). Dept. de Engenharia e Arquitetura]. E-mail: julio.assis@posgrad.unifacs.br

    2003-07-01

    Gasoline is composed of a number of hydrocarbons of varied structure and different functional groups, which have a marked influence on the final quality of the former. It is thus important to identify the main components of gasoline and how they influence some of its characteristics. This research work is concerned with the development of a technique, based on gas chromatography, for the separation and identification of more than 350 organic compounds likely to be present in gasoline. The study involved 50 gasoline samples collected at gas stations located in Salvador-Bahia (Brazil). The hydrocarbons identified were classified according to their main functional groups and compositions were obtained via a statistical treatment of the raw data. The results have shown that the gasoline used in Salvador has isopentane as the prevalent saturated compound, while m-xylene and methyl-butene are the most frequently found aromatic and olefin, respectively. (author)

  1. Avaliação de fragrância em detergente em pó por cromatografia gasosa e métodos quimiométricos

    OpenAIRE

    Robson Bonfim Godinho

    2009-01-01

    Resumo: Fragrância é uma mistura de moléculas orgânicas como ésteres, cetonas, aldeídos, hidrocarbonetos, alcoóis, entre outras, tendo como fontes substâncias de origem natural ou sintética, que quando combinadas em proporções harmônicas conferem uma característica odorífera ímpar em um perfume ou em um produto perfumado. Considerando essa característica, a primeira etapa desse trabalho foi o desenvolvimento de um método de análise dos compostos voláteis provenientes de uma fragrância por cro...

  2. ANÁLISE COMPARATIVA DO CONTEÚDO EM ESTEROIDES LIVRES DE DIFERENTES ÓLEOS, GORDURAS E BIODIESEIS POR CROMATOGRAFIA GASOSA

    Directory of Open Access Journals (Sweden)

    Kelly da S. Bezerra

    2015-05-01

    Full Text Available In this study, the percentage content of free steroid in oils, fats and biodiesel was analyzed. For this, the saponification reaction on a microscale was used, and this procedure for extraction of unsaponifiable fraction was studied in several experimental steps. After the process of saponification, the unsaponifiable fraction was analyzed by gas chromatography with flame ionization detector, where all steroids present in each oil, fat and biodiesel were identified and their contents determined and compared to their respective biodiesel. A reduction in unsaponifiable fraction of each oil and fat and its biodiesel was noted, as well as a reduction in the content of free steroids. The results showed that, compared to the sedimentation problem of steroids in biodiesel, some raw materials, such as chicken fat and babassu oil may be promising because they have low content and high reduction percentages of steroids when converted to biodiesel.

  3. Estado da arte da cromatografia gasosa de alta resolução e alta temperatura State of the art of high temperature high resolution gas chromatography

    Directory of Open Access Journals (Sweden)

    Alberto dos Santos Pereira

    2000-06-01

    Full Text Available The developments in stationary phase synthesis and capillary column technology, have opened new perspectives in analysis of high molecular mass compounds (³600 daltons and thermolabile organic compounds by High Temperature High Resolution Gas Chromatography (HT-HRGC. HT-HRGC is a new analytical borderline and its application to the analysis of high molecular mass compounds is still in its infancy. The apolar and medium polar gum phases can now be operated at temperatures up to 400-480ºC, being used for the analysis of n-alcanes up to C-100, lipids, oligosaccharides, industrial resins, polyglycerols, cyclodextrins, porphyrins, etc. This technique should play a leading role as a powerful tool, for many different analysis types, in multidisciplinary fields of Science.

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

    Directory of Open Access Journals (Sweden)

    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.

  5. Determinação de traços de Co e Co2 "em linha" por cromatografia em fase gasosa

    Directory of Open Access Journals (Sweden)

    Jesus Rosangela Novaes de

    1998-01-01

    Full Text Available The present work describes a rapid and sensitive method for the determination of carbon monoxide and carbon dioxide at low concentration levels, on line, in ethylene and hydrogen lines. These gases were separated in a column filled with Porapak Q, converted to methane and quantified by a flame ionization detector. Some modifications were made in the injection system and in the lines of the carrier gas. The detection limits of 2,6 ppbV and 4,85 ppbV for CO and CO2, respectively, were reached after modifications.

  6. Evaluacion de la cromatografia ionica para fomentar su uso en la investigacion y estudios de posgrado en ciencias del agua

    National Research Council Canada - National Science Library

    Trujillo, Eduardo; Fonseca, Guadalupe; Garcia, Miriam A; Martinez, Veronica

    2009-01-01

    .... Los resultados encontrados permiten afirmar que la cromatografia ionica es una tecnica analitica cualitativa y cuantitativa, rapida, economica, sensible y confiable y que puede ser realizada por estudiantes entrenados, no requiriendo de larga especializacion.

  7. ISOLAMENTO DA β-LACTOGLOBULINA DO SORO DO LEITE POR CROMATOGRAFIA IÔNICA

    OpenAIRE

    Susana Berleze de Pelegrini

    2013-01-01

    A alergia à proteína do leite de vaca atinge 2 a 5% dos lactentes e desencadeia sintomas que podem variar de leve a risco de vida. A β-lactoglobulina é a fração protéica mais alergênica do soro do leite. Vários processos foram desenvolvidos para a separação e purificação protéica, dentre eles a cromatografia de troca iônica. O objetivo deste trabalho foi realizar a separação da β-lactoglobulina do concentrado protéico do soro do leite através de cromatografia de troca...

  8. ISOLAMENTO DA β-LACTOGLOBULINA DO SORO DO LEITE POR CROMATOGRAFIA IÔNICA

    OpenAIRE

    Susana Berleze de Pelegrini

    2013-01-01

    A alergia à proteína do leite de vaca atinge 2 a 5% dos lactentes e desencadeia sintomas que podem variar de leve a risco de vida. A β-lactoglobulina é a fração protéica mais alergênica do soro do leite. Vários processos foram desenvolvidos para a separação e purificação protéica, dentre eles a cromatografia de troca iônica. O objetivo deste trabalho foi realizar a separação da β-lactoglobulina do concentrado protéico do soro do leite através de cromatografia de troca...

  9. Controle de autenticidade de óleos de copaíba comerciais por cromatografia gasosa de alta resolução Authenticity control of commercial copaiba oils by high resolution gas chromatography

    Directory of Open Access Journals (Sweden)

    Valdir F. Veiga Jr.

    1997-12-01

    Full Text Available Copaiba oil is a resin extracted from the trunk of trees of Copaifera species which grow in Brazil where it is widely used in popular medicine as an anti-inflammatory, antiseptic anti-bactericidal, diuretic, dermatological, expectorant, and anti-infective. The comparative study of the composition of commercial copaiba oils was carried out by high resolution gas chromatography (HRGC and high resolution gas chromatography-mass spectrometry (HRGC-MS analysis. The commercial oils were compared with authentic oils, collected from the southeast and northern regions of Brazil. Sixteen commercial oils were analysed and two of them revealed adulterations with fatty acids. Using the chromatographic profile of authentic copaiba species oils, it is possible to analyse commercial oils and determine the authenticity of these materials.

  10. Determinação de resíduos de pesticidas em plasma bovino por cromatografia gasosa-espectrometria de massas Pesticides residue determination in cattle plasma by gas chromatography-mass spectrometry

    Directory of Open Access Journals (Sweden)

    Daniele Fernanda Maffei

    2009-01-01

    Full Text Available An analytical method for the isolation based on matrix solid-phase dispersion technique and gas chromatographic determination of pesticides in cattle plasma is presented. It was fortified 0.25 g of plasma with pesticides and blended with 1 g each C18 and Na2SO4. The homogenized matter was transferred to a SPE cartridge, which contained 1 g of activated florisil with 5 mL acetonitrile. The analites were eluted under vaccum with 15 mL acetonitrile, the extract was analyzed by gas chromatography-mass spectrometry. The limit of quantification of the method was 0.04 mg L-1 for chlorphenvinfos and fipronil and 0.02 mg L-1 for cypermethrin..

  11. DETERMINAÇÃO DO PERFIL DE ÁCIDOS GRAXOS POR CROMATOGRAFIA GASOSA, COMPOSIÇÃO PROXIMAL E VALOR CALÓRICO DE CARNE DE AVESTRUZ (STRUTHIO CAMELLUS

    Directory of Open Access Journals (Sweden)

    Bruna Aparecida Souza MACHADO

    2013-04-01

    Full Text Available O avestruz é uma ave que apresenta notável potencial para a produção de carne, entretanto, na literatura existem poucos dados sobre a composição química deste produto, principalmente o que é produzido no Brasil. O objetivo deste estudo foi determinar a composição proximal, o perfil dos ácidos graxos e o valor calórico de corte comercial de carne (coxa de avestruz proveniente de supermercados e da estrutiocultura, desenvolvido no estado da Bahia – Brasil. Não foram encontradas diferenças significativas (p>0,05 entre os percentuais de umidade (73,52±0,54%, proteína (21,79±0,86%, lipídios totais (1,42±0,05% e de ácidos graxos, das amostras oriundas de supermercados e da estrutiocultura. Embora não tenham sido observadas diferenças estatisticamente significativas, os ácidos graxos majoritários presentes nas amostras experimentais foram o palmítico (20,24±0,45%, esteárico (11,55±0,44%, oleico (29,08±0,03% e linoleico (13,39±0,15%. Constatou-se que a coxa da carne de avestruz, cujo valor calórico variou de 95,55±0,20 a 103,87±0,03,quando comparada às carnes suínas e bovinas apresenta baixo valor calórico e valores de ácidos graxos poli-insaturados superiores, com teores de ω-3 similares aos de peixes de água doce, características desejáveis a saúde humana, sendo uma opção saudável de fonte alimentar animal.

  12. Aspectos moleculares da fração acida de querosene de aviação : sintese de padrões (fenolicos, acidos carboxilicos e neutros) para analise em cromatografia gasosa acoplada a espectrometria de massas

    OpenAIRE

    Joana D'Arc Felix de Sousa

    1990-01-01

    Resumo: O petróleo Cabiúnas, proveniente da Bacia de Campos, possui um índice de acidez considerável (IA = 1,0), classificando-o como petróleo de acidez média para alta. Sabemos que as frações do petróleo, Querosene de Aviação (QAV) e Gasolina, são obtidas numa faixa de ebulição (250-300°C) semelhante à faixa de destilação dos ácidos naftênicos (200-370°C). Este fato nos motivou a estudar a fração ácida do Querosene de Aviação em uma confirmação de resultados anteriores, deste laboratório. A ...

  13. Modificação de um micro-extrator de vidro para pré-enriquecimento de traços de pesticidas organoclorados de água para análise por cromatografia gasosa

    Directory of Open Access Journals (Sweden)

    Rocha Eduardo Carasek da

    1998-01-01

    Full Text Available Two models of a glass micro-extractor were constructed after modification of a model proposed in the literature. The two models were used for the simultaneous extraction and enrichment of organochlorinated pesticides from aqueous matrixes to an organic solution appropriate for the gas chromatographic analysis of the pesticide. It was established that the performance of one of the modified micro-extractors permits the pre-concentration of the pesticides to a level that allow their quantitation at the trace level with electron capture detection. It is thus concluded that the glass micro-extractor is a suitable tool for the sample preparation step in the gas chromatographic analysis of environmental pollutants of the class of pesticides.

  14. Comparação de diferentes abordagens para avaliação da incerteza na cromatografia gasosa do gás natural Comparison of different approaches to evaluate the uncertainty of gas chromatography for natural gas

    Directory of Open Access Journals (Sweden)

    Elcio Cruz de Oliveira

    2009-01-01

    Full Text Available The evaluation of uncertainty associated with an analytic result is an essential part of the measurement process. Recently, several approaches to evaluate the uncertainty in measurement have been developed. Here, the gas chromatography assay uncertainty for natural gas is compared by some of these approaches: the guide to the expression of uncertainty in measurement (GUM approach, top-down approach (reproducibility estimate from an inter-laboratory study, Barwick & Ellison (data from validation, study of variability and fuzzy approach. The comparison shows that GUM, Barwick & Ellison and fuzzy approaches lead to comparable uncertainty evaluations, which does not happen with the top-down approach and study of variability by the absence of data normality.

  15. Aumento da resposta analítica por meio da otimização do sistema de injeção sem divisão de fluxo em cromatografia gasosa empregando a lei dos gases ideais

    Directory of Open Access Journals (Sweden)

    Guilherme Post Sabin

    2011-01-01

    Full Text Available This paper reports the development of an easy, fast and effective procedure for the verification of the ideal gas law in splitless injection systems in order to improve the response. Results of a group of pesticides were used to demonstrate the suitability of the approach. The procedure helps establish experimental parameters through theoretical aspects. The improved instrumental response allowed extraction with lower sample volumes, the minimization of time and costs and the simplification of sample preparation.

  16. 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

    Directory of Open Access Journals (Sweden)

    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

  17. Aplicação de métodos quimiométricos na investigação do metaboloma de eucalipto por técnicas cromatográficas multidimensionais e hifenadas à espectrometria de massas

    OpenAIRE

    2014-01-01

    O presente trabalho é dedicado à aplicação de técnicas cromatográficas multidimensionais à problemas complexos de separação. No primeiro conjunto de estudos foram desenvolvidos métodos analíticos para investigação do metaboloma de plantas de interesse comercial. Para isso, foram utilizadas a cromatografia gasosa bidimensional abrangente (GC×GC-MS) e a cromatografia líquida de ultra eficiência (UHPLC-MS) acopladas à espectrometria de massas para aquisição do perfil metabólico de folhas de euca...

  18. Trocas gasosas e produtividade de três cultivares de meloeiro conduzidas com um e dois frutos por planta

    Directory of Open Access Journals (Sweden)

    Graciela Maiara Dalastra

    2014-12-01

    Full Text Available Objetivou-se, no presente trabalho, avaliar as trocas gasosas e sua influência na produtividade e qualidade de cultivares de melão conduzidas com um e dois frutos por planta. O experimento foi conduzido de setembro a dezembro de 2013. Utilizou-se o delineamento de blocos ao acaso, em esquema fatorial 3 x 2, com seis repetições. No primeiro fator foram alocadas as cultivares de melão pertencentes aos tipos amarelo, rendilhado e pele de sapo e no segundo fator, a condução das plantas com um e dois frutos por planta. Foram utilizadas três cultivares de melão para cada tipo. As avaliações foram realizadas aos 40 e aos 56 dias após o transplantio. As características avaliadas foram: taxa de assimilação líquida de CO2 (A, transpiração foliar (E, condutância estomática (g s e concentração interna de CO2 (Ci. A partir dessas medidas foi calculada a eficiência no uso da água (WUE. O teor de sólidos solúveis foi determinado por leitura direta, enquanto que a massa média dos frutos foi mensurada no momento da colheita, estimando-se a produtividade. Diante dos resultados, pode-se concluir que as diferenças nos índices de trocas gasosas para as cultivares de melão do tipo pele de sapo não influenciaram na produtividade e no teor de sólidos solúveis. Como melão do tipo amarelo e do tipo rendilhado recomendam-se as cultivares Goldex e Louis, respectivamente. Independente da cultivar, recomenda-se o cultivo de melão com dois frutos por planta, por assim as plantas apresentarem maior produtividade sem alterar de forma expressiva os índices de trocas gasosas delas.

  19. Caracterização de ácidos orgânicos por UPLC-PDA em plantas silvestres de uso alimentar

    OpenAIRE

    Pereira, Carla; Barros, Lillian; Carvalho, Ana Maria; Isabel C. F. R. Ferreira

    2012-01-01

    A análise de ácidos orgânicos tem-se tornado cada vez mais importante devido ao papel destes compostos na atividade fisiológica das plantas. Têm sido desenvolvidas várias técnicas de análise de ácidos orgânicos em plantas nomeadamente, cromatografia gasosa (GC), eletroforese capilar, cromatografia de troca iónica e cromatografia líquida de alta eficiência (HPLC). A determinação de ácidos orgânicos por GC requer passos de derivatização e, por isso, as técnicas de HPLC têm sido mais utilizadas....

  20. 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.

  1. Estimativa da composição gasosa em embalagem de atmosfera modificada contendo mangas (mangifera indica l. Cv. Keitt

    Directory of Open Access Journals (Sweden)

    Fábio Yamashita

    1997-08-01

    Full Text Available Foram determinadas as taxas de respiração e a perda de peso e composição gasosa no interior da embalagem, de mangas embaladas individualmente em filme de polietileno de baixa densidade com espessura de 24,5 μm, armazenadas a 7°C (80-90% UR; 12°C (75-85% UR; 17°C (70-80% UR; 22°C (65-75% UR e 25°C (65-75% UR. A partir dos resultados experimentais e equações de transferência de massa foram calculadas a permeabilidade da casca da manga ao vapor de água e a concentração de gás carbônico do espaço livre, após ter sido atingido um estado estacionário de transferência de massa. A concentração de gás carbônico calculada foi comparada com a obtida experimentalmente, tendo sido encontradas diferenças, dependendo da temperatura, entre -16% e 29%. A permeabilidade calculada da casca foi cerca de 600 vezes maior que a do filme plástico.

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

    OpenAIRE

    Bakan,Mefkur; Topuz,Ufuk; Esen, Asim; Basaranoglu,Gokcen; Ozturk, Erdogan

    2013-01-01

    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 em...

  3. Desenvolvimento de processo de recuperação de aprotinina a partir de efluente industrial centrado em cromatografia em quimotripsina imobilizada

    OpenAIRE

    Ana Carolina Barros de Genaro

    2000-01-01

    Resumo: A aprotinina é um inibidor de serino-proteases presente em órgãos bovinos, utilizado como composto farmacêutico em operações cirúrgicas e em cultura de células. Atualmente a aprotinina não é comercialmente produzida no Brasil. O objetivo deste trabalho foi desenvolver um processo de recuperação de aprotinina a partir de efluente industrial da produção de insulina bovina (SPI), centrado em cromatografia por quimotripsina imobilizada. Foram estudadas três estratégias: a) cromatografia e...

  4. Determinação espectrofotométrica e cromatográfica em fase gasosa de ácido tricloracético em urina

    Directory of Open Access Journals (Sweden)

    Pedrozo Maria de Fatima M.

    1996-01-01

    Full Text Available Solventes halogenados -- 1,1,1-tricloretano, tricloretileno, percloretileno -- apresentam o ácido tricloracético (TCA como produto de biotransformação comum, o qual pode ser utilizado como indicador biológico de dose interna na exposição a estes compostos. Foi realizado estudo de métodos espectrofotométrico e cromatográfico em fase gasosa para a determinação do TCA, bem como da aplicação destes métodos à sua determinação em urina de indivíduos expostos ao 1,1,1-tricloretano. Os resultados mostram a boa precisão à determinação do TCA em urina de indivíduos expostos ao 1,1,1-tricloretano e nenhuma diferença significativa foi observada entre os métodos, ainda que o cromatográfico em fase gasosa apresentasse menor limite de detecção.

  5. Determinação espectrofotométrica e cromatográfica em fase gasosa de ácido tricloracético em urina

    Directory of Open Access Journals (Sweden)

    Maria de Fatima M. Pedrozo

    1996-06-01

    Full Text Available Solventes halogenados -- 1,1,1-tricloretano, tricloretileno, percloretileno -- apresentam o ácido tricloracético (TCA como produto de biotransformação comum, o qual pode ser utilizado como indicador biológico de dose interna na exposição a estes compostos. Foi realizado estudo de métodos espectrofotométrico e cromatográfico em fase gasosa para a determinação do TCA, bem como da aplicação destes métodos à sua determinação em urina de indivíduos expostos ao 1,1,1-tricloretano. Os resultados mostram a boa precisão à determinação do TCA em urina de indivíduos expostos ao 1,1,1-tricloretano e nenhuma diferença significativa foi observada entre os métodos, ainda que o cromatográfico em fase gasosa apresentasse menor limite de detecção.

  6. COMPARAÇÃO DE IMUNODOSAGEM E CROMATOGRAFIA EM MINICOLUNA PARA TRIAGEM DE AFLATOXINAS EM AMENDOIM E MILHO

    Directory of Open Access Journals (Sweden)

    Célia Maria de SYLOS

    2009-07-01

    Full Text Available

    RESUMO: Foi realizada uma avaliação comparativa de imunodosagem (ELISA e cromatografia em minicoluna para a triagem de aflatoxinas em amendoim e milho. Foi verificado se havia contaminação da amostra e, nos casos positivos, se o nível era inferior ou superior a 20 µ/kg. Foram analisadas 10 amostras de amendoim (amendoim in natura, amendoim frito e paçoca e nove amostras de milho (milho para pipoca, farinha de milho e fubá. Os resultados obtidos pelos dois métodos foram concordantes. Cinqüenta por cento das amostras de amendoim estavam contaminadas com teores acima de20 µ/kg, enquanto nenhuma amostra de milho se apresentou positiva. A imunodosagem foi mais vantajosa em relação ao tempo de análise. Para a realização de cinco análises simultâneas, foram requeridos apenas 35 minutos; por minicoluna, foram necessários 105 minutos. O custo da análise foi de US$ 3/análise por imunodosagem. Os dois métodos demonstraram simplicidade, não exigindo muita prática por parte do analista. PALAVRAS-CHAVE: Aflatoxinas-triagem; cromatografia em minicoluna; imunodosagem.

  7. 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.

  8. Quantificação de sulfonamidas em leite por cromatografia líquida de alta eficiência via azoderivados

    National Research Council Canada - National Science Library

    Marcelo Volpatto Marques; Fabrício Fredo Naciuk; Ana Maria de Souza Mello; Nair Maria Seibel; João Gabriel Rosa dos Santos; Luiz Antonio Mazzini Fontoura

    2008-01-01

    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...

  9. Cuantificación de ketoconazol en champú por cromatografia líquida de alta eficiencia

    OpenAIRE

    Staub, Inara; Bergold, Ana Maria

    2004-01-01

    Fue desarrollado un procedimiento para cuantificar el ketoconazol en champú mediante cromatografia líquida de alta eficiencia. La fase móvil consiste en una mezcla de las siguientes soluciones: (A) monoisopropilamina-metanol (2:500 v/v) y (B) acetato de amônio-água (1:200 w/v) (7:3 v/v). El pH de la solución final fue ajustado a 5.5 con ácido acético. Fué utilizada una columna LiChrospher® 100 RP-8 (150 x 46 mm, 5 µm), flujo 1.0 mL/min, y detector UV (225 nm). La validación del méto...

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

    Directory of Open Access Journals (Sweden)

    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.

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

    Directory of Open Access Journals (Sweden)

    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.

  12. 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

  13. Derivatization of carbohydrates for GC and GC-MS analyses.

    Science.gov (United States)

    Ruiz-Matute, A I; Hernández-Hernández, O; Rodríguez-Sánchez, S; Sanz, M L; Martínez-Castro, I

    2011-05-15

    GC and GC-MS are excellent techniques for the analysis of carbohydrates; nevertheless the preparation of adequate derivatives is necessary. The different functional groups that can be found and the diversity of samples require specific methods. This review aims to collect the most important methodologies currently used, either published as new procedures or as new applications, for the analysis of carbohydrates. A high diversity of compounds with diverse functionalities has been selected: neutral carbohydrates (saccharides and polyalcohols), sugar acids, amino and iminosugars, polysaccharides, glycosides, glycoconjugates, anhydrosugars, difructose anhydrides and products resulting of Maillard reaction (osuloses, Amadori compounds). Chiral analysis has also been considered, describing the use of diastereomers and derivatives to be eluted on chiral stationary phases.

  14. Principais substâncias responsáveis pelo aroma de mangas comerciais brasileiras identificadas por cromatografia gasosa de alta resolução/olfatometria/espectrometria de massas Aroma impact substances on commercial brazilian mangoes by HRGC-O-AEDA-MS

    Directory of Open Access Journals (Sweden)

    Diógenes C. Lopes

    1999-02-01

    Full Text Available Six Brazilian commercial mangoes were analysed by HRGC-O-AEDA-MS, viz., Carlota, Haden, Espada, Coração de boi, Rubi and Tommy Atkins. All them showed ethyl butanoate as the main aroma character impact compound by AEDA evaluation. The ethyl esters of 2 and 3-methylbutanoic acids are also important, the main contribution in Carlota variety being 2(S enantiomer. In Rubi variety, both 2(R enantiomer and 3-methyl isomer contributes to the caprylic fruity note observed. In four varieties, viz., Haden, Espada, Rubi and Tommy Atkins, d-3-carene showed to be the second impact aroma compound presented. In Tommy Atkins variety, a-pinene also has a significant contribution, mainly due to its (1R,5R(+-enantiomer.

  15. Desenvolvimento e validação de metodologia de análise de misturas biodiesel: diesel utilizando cromatografia gasosa-espectrometria de massas Development and validation of a methodology FOR analysis of biodiesel: diesel blends using gas chromatography-mass spectrometry

    Directory of Open Access Journals (Sweden)

    Rita C. M. Faria

    2007-01-01

    Full Text Available The aim of this work was to develop and validate a method of analysis of biodiesel:diesel blends using HRGC-MS in SIM mode. The proposed method is applicable to biodiesel from linoleic oils, such as soybean oil. The following results were obtained: linearity over the methyl linoleate concentration range of 250-2500 mg L-1 (R² > 0.999; limits of detection and quantification of 2 and 5 mg L-1, respectively; recovery from 82 to 96% of biodiesel in diesel and repeatability < 2% (RSD. Comparison between two operators showed that it is not necessary the same operator to do the analysis.

  16. Desenvolvimento de métodos baseados na microextração líquido-líquido dispersiva e partição em baixa temperatura para determinação multirresíduo de agrotóxicos em água e solo por cromatografia gasosa

    OpenAIRE

    Alves, Renata Domingos

    2014-01-01

    A microbacia hidrográfica do rio Manhuaçu é uma sub-bacia do Rio Doce, cujo principal rio é o rio Manhuaçu. Essa bacia se localiza na zona leste de Minas Gerais, que se destaca pela grande produção de café. A região ainda caracteriza-se pelo relevo acidentado, favorecendo a erosão e também, com grandes possibilidades de que os agrotóxicos e fertilizantes aplicados nas plantações de café contaminem as águas superficiais. Diante deste cenário, o objetivo deste trabalho foi diagnosticar essa reg...

  17. Obtenção de biodiesel por transesterificação em dois estágios e sua caracterização por cromatografia gasosa: óleos e gorduras em laboratório de química orgânica

    Directory of Open Access Journals (Sweden)

    Diogo Müller de Oliveira

    2013-01-01

    Full Text Available Methanolic transesterification of oils and fats was carried out in a two steps procedure, under basic and acidic catalysis. Palm, soybean, canola, corn, rice, grapeseed, sunflower, peanut, pequi and olive oils, besides tallow and lard were used as feedstock. Specific gravity, relative viscosity, thin layer chromatography and gas chromatography were used to characterize the biodiesel. Biodiesel was obtained in high yield and purity. Results were used to discuss the following key-concepts: 1 - triglycerides, composition and properties; 2 - nucleophilic acyl substitution under basic and acid conditions, 3 - thin layer chromatography, 4 - gas chromatography and its quantitative methods.

  18. Análise de praguicidas organofosforados em água por extração em fase sólida (SPE utilizando discos C18 e cromatografia em fase gasosa: avaliação da contaminação do reservatório de Furnas (MG-Brasil

    Directory of Open Access Journals (Sweden)

    Santos Neto Alvaro José dos

    2005-01-01

    Full Text Available Solid phase extraction (SPE in C18 disks has been optimized and validated for extraction of 5 organophosphorus (OP pesticides in water. Extraction has been followed by separation and detection by gas chromatography/flame photometry. Excellent linearity was obtained for all compounds (r greater than 0.99, with CVs between 1.0-6.9%, recoveries between 73-95% and quantification limits between 2.5-5.0 µg L-1. Samples from Furnas dam were analyzed monthly during one year and 10% showed OP pesticide residues.

  19. Análise por cromatografia gasosa de BTEX nas emissões de motor de combustão interna alimentado com diesel e mistura diesel-biodiesel (B10 Analysis of BTEX in the emissions from an internal combustion engine burning diesel oil and diesel-biodiesel mixture (B10 by gas chromatography

    Directory of Open Access Journals (Sweden)

    Sérgio L. Ferreira

    2008-01-01

    Full Text Available This paper describes the procedures for analysing pollutant gases emitted by engines, such as volatile organic compounds (benzene, toluene, ethylbenzene, o-xylene, m-xylene and p-xylene by using high resolution gas chromatography (HRGC. For IC engine burning, in a broad sense, the use of the B10 mixture reduces drastically the emissions of aromatic compounds. Especially for benzene the reduction of concentrations occurs at the level of about 24.5%. Although a concentration value below 1 µg mL-1 has been obtained, this reduction is extremely significant since benzene is a carcinogenic compound.

  20. Quantitative analysis of Boehm's GC

    Institute of Scientific and Technical Information of China (English)

    GUAN Xue-tao; ZHANG Yuan-rui; GOU Xiao-gang; CHENG Xu

    2003-01-01

    The term garbage collection describes the automated process of finding previously allocated memorythatis no longer in use in order to make the memory available to satisfy subsequent allocation requests. Wehave reviewed existing papers and implementations of GC, and especially analyzed Boehm' s C codes, which isa real-time mark-sweep GC running under Linux and ANSI C standard. In this paper, we will quantitatively an-alyze the performance of different configurations of Boehm' s collector subjected to different workloads. Reportedmeasurements demonstrate that a refined garbage collector is a viable alternative to traditional explicit memorymanagement techniques, even for low-level languages. It is more a trade-off for certain system than an all-or-nothing proposition.

  1. Quantificação de sulfonamidas em leite por cromatografia líquida de alta eficiência via azoderivados

    OpenAIRE

    Marques, M.V.; NACIUK, F. F.; MELLO, A. M. de S.; SEIBEL, N. M.; SANTOS, J. G. R. dos; FONTOURA, L. A. M.

    2008-01-01

    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 quant...

  2. Chemical composition of essential oil from the bark of Croton cajucara Bentham=Composição química do óleo essencial das cascas de Croton cajucara Bentham

    Directory of Open Access Journals (Sweden)

    Domingos Sávio Nunes

    2012-07-01

    Full Text Available The essential oil from the bark of Croton cajucara Bentham, popularly known as sacaca or cajuçara, was obtained by hydrodistillation, yielding 1.28% of the former bark mass, and analyzed by gas chromatography (GC and gas chromatography coupled to mass spectrometry (GC-MS. In total, 50 compounds were identified, with oxygenated sesquiterpenes composing the majority of components. The main compounds identified were: cyperene (12.36%, α-guaiene, (11.50% and epi-β-Santalene (8.70%.O óleo essencial das cascas de Croton cajucara Bentham, conhecida popularmente por sacaca ou cajuçara, foi obtido por hidrodestilação com rendimento de 1,28% em relação à massa de material vegetal e analisado por cromatografia gasosa (CG e cromatografia gasosa acoplada à espectrometria de massas (CG-EM. No total foram identificados 50 compostos, com os sesquiterpenos oxigenados como a maioria dos componentes. Os constituintes majoritários identificados foram o cipereno 12,36%, α-guaieno 11,50% e o epi-β-santeleno 8,70%.

  3. 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...

  4. Gas exchange of the umbu tree under semi-arid conditions Trocas gasosas do umbuzeiro sob condições semi-áridas

    Directory of Open Access Journals (Sweden)

    José Moacir Pinheiro Lima Filho

    2004-08-01

    Full Text Available A study was carried out at Embrapa Semi-Árido, Petrolina-PE, Brazil, aiming to understand the gas exchange process of the umbu tree (Spondias tuberosa Arr. Cam. in the dry and rainy seasons. Stomatal conductance, transpiration, photosynthesis and internal CO2 concentration were obtained with a portable infrared gas analyzer (IRGA. During the dry season the umbu tree showed a much lower stomatal conductance early in the morning, as soon as the vapor pressure deficit increased, apparently affecting CO2 assimilation more than transpiration. The highest values were detected around 6:00 am but decreased to the lowest points between 10:00 am and 2:00 pm. During the rainy season, however, stomatal conductance, transpiration and photosynthesis were significantly higher, reaching the highest values between 8:00 and 10:00 am and the lowest around 2:00 pm. It was also observed at 4:00 pm, mainly during the rainy season, an increase on these variables indicating that the umbu tree exhibits a two-picked daily course of gas exchange.Realizou-se um trabalho na Embrapa Semi-Árido, em Petrolina-PE, com o objetivo de estudar as trocas gasosas do umbuzeiro (Spondias tuberosa Arr. Cam., durante as estações seca e chuvosa. Os resultados obtidos basearam-se em observações da condutância estomática, transpiração, fotossíntese e concentração interna de CO2, mensuradas com auxílio de um analisador portátil de gás infravermelho. Durante a estação seca, o umbuzeiro apresentou baixa condutividade estomática logo no início do dia, decrescendo à medida que aumentou o déficit de pressão de vapor, aparentemente afetando mais a assimilação de CO2 que a transpiração. Os valores mais altos foram observados em torno de 6 h, decrescendo até atingir os valores mais baixos entre 10 h e 14 h. Entretanto, durante a estação chuvosa, a condutividade estomática, transpiração e fotossíntese foram significativamente maiores, atingindo os valores mais altos

  5. MOMA GC-MS coupling

    Science.gov (United States)

    Buch, A.; Pinnick, V. T.; Grand, N.; Szopa, C.; Danell, R.; Lustrement, B.; Freissinet, C.; van Amerom, F. H.; Raulin, F.; Glavin, D. P.; Stalport, F.; Coll, P. J.; Arevalo, R. D.; Brinckerhoff, W. B.; Goesmann, F.; Mahaffy, P. R.

    2013-12-01

    The joint ESA-Roscosmos Exo-Mars-2018 rover mission seeks the signs of past or present life on Mars. 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, with particular focus on the characterization of organic content. Central to MOMA instrumentation is a gas chromatograph-mass spectrometer (GC-MS) which provides the unique ability to characterize a broad range of compounds allowing chemical analyses of volatile and non-volatile species. The Gas chromatograph and the oven have been built at LATMOS/LISA (France) and at MPS (Germany) respectively whereas the mass spectrometer has been built at the NASA Goddard Space Flight Center (USA). Both instruments have been tested separately first and have been coupled in order to test the efficiency of the future MOMA GC-MS instrument. The main objective of the second step has been to test the quantitative response of both instruments while they are coupled and to characterize the combined instrument detection limit for several compounds. A final experiment has been done in order to test the feasibility of the separation and detection of a mixture contained in a soil sample introduced in the MOMA oven.

  6. Efeitos da pleurotomia na mecânica pulmonar e trocas gasosas após cirurgia de revascularização do miocárdio sem circulação extracorpórea

    OpenAIRE

    Tavolaro,Kelly Cristiani

    2008-01-01

    OBJETIVO: Avaliar os efeitos da pleurotomia na mecânica pulmonar e trocas gasosas após cirurgia de revascularização do miocárdio (RM), utilizando enxerto de artéria torácica interna esquerda (ATIE), sem circulação extracorpórea (CEC). MÉTODO: Trinta e dois pacientes foram alocados prospectivamente em dois grupos: grupo PA (n=16 pacientes com abertura da cavidade pleural esquerda); grupo PI (n=16 pacientes com cavidade pleural intacta). Todos os pacientes foram submetidos às medidas de comp...

  7. Quantificação de sulfonamidas em leite por cromatografia líquida de alta eficiência via azoderivados Sulfonamides quantification in milk by high performace liquid chromatography via azoderivatives

    National Research Council Canada - National Science Library

    Marcelo Volpatto Marques; Fabrício Fredo Naciuk; Ana Maria de Souza Mello; Nair Maria Seibel; João Gabriel Rosa dos Santos; Luiz Antonio Mazzini Fontoura

    2008-01-01

    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...

  8. Split Left GC-Lpp Semigroups

    Institute of Scientific and Technical Information of China (English)

    Zhen Zhen LI; Xiao Jiang GUO; Zhi Qing FU

    2012-01-01

    A left GC-lpp semigroup S is called split if the natural homomorphism γb of S onto S/γ induced by γ is split.It is proved that a left GC-lpp semigroup is split if and only if it has a left adequate transversal.In particular,a construction theorem for split left GC-lpp semigroups is established.

  9. 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 prepa......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...... for measuring Gc-globulin in horses. Studies in rodents and humans have shown that Gc-globulin is a multifunctional acute phase plasma protein, which removes actin from the blood by binding it and facilitating its clearance from the circulation by the liver. As such, Gc-globulin prevents hyper coagulation...

  10. Gas exchange of potted Tabebuia aurea plants under hydric stress=Trocas gasosas em plantas envasadas de Tabebuia aurea sob estresse hídrico.

    Directory of Open Access Journals (Sweden)

    Sônia Cristina Juliano de Gualtieri

    2011-10-01

    Full Text Available To evaluate the effects of hydric stress on CO2 and H2O exchange, five-month-old Tabebuia aurea seedlings cultivated in planting bags were subjected to hydric stress by suppressing irrigation for 21 days. After 14 days without irrigation, the rates of transpiration, stomatal conductance and net photosynthesis in leaves were zero, while the hydric potential of leaves reached -2.4 MPa. After this point, daily irrigation was resumed, and the values of the measured variables recovered to initial levels after 96 hours (transpiration rate from 3.2 to 3.5 mmol m-2 s-1; stomatal conductance rate from 0.32 to 0.35 mol m-2 s-1 and photosynthesis rate from 8.0 to 9.8 µmol m-2 s-1. Likewise, hydric potential values were similar to those at the beginning of the experiment (-0.6 MPa. These results demonstrate that T. aurea has mechanisms to tolerate a period of hydric deficit, which may be considered ecologically relevant.Visando avaliar os efeitos do estresse hídrico sobre as trocas gasosas de CO2 e H2O, mudas de paratudo com cinco meses de idade cultivadas em sacos de plantio foram submetidas a estresse hídrico simulado pela supressão da irrigação durante 21 dias. Após 14 dias de supressão de irrigação, os valores de transpiração, condutância estomática e fotossíntese líquida das folhas foram nulos, enquanto o potencial hídrico das folhas atingiu -2,4 MPa. A partir deste ponto foi reiniciada a irrigação diária, sendo que após 96 horas as taxas voltaram a oscilar na faixa dos valores iniciais (transpiração - 3,2 a 3,5 mmol m-2 s-1; condutância estomática - 0,32 a 0,35 mol m-2 s-1; e, fotossíntese - 8,0 a 9,8 µmol m-2 s-1, além do potencial hídrico voltar a apresentar valores similares ao início do experimento (-0,6 MPa, demonstrando que a espécie possui mecanismos para tolerar déficit hídrico durante um período que pode ser considerado ecologicamente relevante.

  11. Trocas gasosas e ciclo fotossintético da figueira 'Roxo de Valinhos' Gas exchanges and cycle fhotosynthetic in fig tree 'Roxo de Valinhos'

    Directory of Open Access Journals (Sweden)

    Andréa Carvalho da Silva

    2010-06-01

    Full Text Available No presente trabalho, determinaram-se as trocas gasosas de folhas de figueira 'Roxo de valinhos' e o ciclo fotossintético por meio da relação isotópica 12C/13C. Essas medidas foram realizadas sempre na região mediana das folhas, completamente expandidas e totalmente expostas à radiação solar, no período das 09h00min às 10h30min. As folhas fotossinteticamente ativas da figueira apresentaram área foliar em torno de 160cm², com uma assimilação de 14,38µmol m-2 s-1 de CO2, cujos valores isotópicos médios no ramo 1 e no 2 são -28,98±0,69‰ e -29,28±0,85‰, respectivamente. Com base nos valores da fotossíntese máxima e na discriminação isotópica do 13C, evidenciou-se que a figueira pode ser considerada uma planta do ciclo fotossintético C3.In the present research, it was determined the gas exchange of the 'Roxo de Valinhos' fig tree and the cycle photosynthetic through the isotopic relation 12C/13C. These measures were always carried in the average region of the leaves, completely expanded, entirely displayed to the solar radiation, in the period from 09h00min to 10h30min. The sheets photosynthetic active leaf area had around 160cm², with 14.38 -2 s-1 assimilation CO2, and mean isotopic values in the branch 1 and 2 of -28.98±0.69‰ and -29.28±0,85‰, respectively. Based in the values of the maximum photosynthesis and in the discrimination isotopic of the 13C, the fig tree can be considered a plant which belongs to photosynthetic C3 cycle.

  12. 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

    exchange chromatography. The separated isoforms and several commercial preparations of individual isoforms were characterized by mass spectrometry. This revealed that the major isoforms were non-glycosylated. Compared to the Gc-1f isoform the other dominating isoforms represented an Asp/Glu substitution......Gc globulin, also called vitamin D-binding protein, is a plasma protein involved in the extracellular actin-scavenger system, vitamin D transport and possibly also other biological activities. Low levels of Gc globulin have been found to correlate with multiple organ failure and non......-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...

  13. 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...... for measuring Gc-globulin in horses. Studies in rodents and humans have shown that Gc-globulin is a multifunctional acute phase plasma protein, which removes actin from the blood by binding it and facilitating its clearance from the circulation by the liver. As such, Gc-globulin prevents hyper coagulation......-globulin infusions. Reference List    1.   Vasconcellos CA and Lind SE. Coordinated inhibition of actin-induced platelet aggregation by plasma gelsolin and vitamin D-binding protein. Blood 1993;82:3648-3657....

  14. Caracterização físico-química e análises por espectrofotometria e cromatografia de Peperomia pellucida L. (H. B. K.)

    OpenAIRE

    R. M. F. Silva; Ribeiro,J.F.A.; M.C.C. Freitas; ARRUDA, M. S. P.; NASCIMENTO, M.N.; W.L.R. Barbosa; P.J. Rolim Neto

    2013-01-01

    O objetivo deste trabalho foi realizar a caracterização físico-química do pó e da tintura, e análise por espectrofotometria e cromatografia do extrato seco de Peperomia pellucida L. (H. B. K.). As metodologias seguiram a Farmacopéia Brasileira IV ed., com exceção da prospecção química, da espectrofotometria, da obtenção do perfil cromatográfico do extrato seco, e determinação do resíduo seco. A prospecção química revelou a presença de saponinas espumídicas; açúcares redutores; proteínas e ami...

  15. 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.

  16. The GC-heterogeneity of teleost fishes

    Directory of Open Access Journals (Sweden)

    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

  17. Trocas gasosas em folhas de sol e sombreadas de cajueiro anão em diferentes regimes hídricos Gas exchange in leaves of sun and shade of cashew in different water regimes

    OpenAIRE

    Michella de Albuquerque Lima; Marlos Alves Bezerra; Enéas Gomes Filho; Ciro de Miranda Pinto; Joaquim Enéas Filho

    2010-01-01

    Foram analisadas as variações sazonais nas taxas de trocas gasosas em lâminas foliares, sombreadas e a pleno sol, de cajueiro anão precoce (Anacardium occidentale L.), quando submetidas aos regimes de irrigação e de sequeiro. Os clones CCP 76 e BRS 189 foram mensalmente avaliados quanto ao seu desempenho fisiológico em relação à condutância estomática (g s), às taxas transpiratórias (E) e fotossintéticas (A), à temperatura foliar e à relação entre as concentrações interna e externa de CO2 (Ci...

  18. Modulation techniques and applications in comprehensive two-dimensional gas chromatography (GC x GC)

    Energy Technology Data Exchange (ETDEWEB)

    Pursch, Matthias [Dow Deutschland GmbH and Co. OHG, Analytical Sciences, 77836 Rheinmuenster (Germany); Sun, Kefu; Winniford, Bill; Weber, Andy [Dow Chemical Company, Analytical Sciences, Freeport, TX 77541 (United States); Cortes, Hernan; McCabe, Terry [Dow Chemical Company, Analytical Sciences, Midland MI 48667 (United States); Luong, Jim [Dow Canada, Analytical Sciences, Fort Saskatchewan (Canada)

    2002-07-01

    More than a decade after Phillips' first published work this article reviews recent developments in comprehensive two-dimensional gas chromatography (GC x GC). Special attention is devoted to the further development and diversity of modulation devices. These include heated sweepers, cryofocused modulators, and a variety of diaphragm valve-switching strategies. It is demonstrated that all modulation approaches can be very well suited to GC x GC, depending on the particular application. Diaphragm-valve modulation is very powerful for volatile organic compounds. Slotted heater and cryofocused modulation are preferred for samples that contain non-volatile components. Applications ranging from petroleum to environmental and biological samples are illustrated. Extension of the technique to GC x GC-mass spectrometry (MS) is also discussed and trends for future research activity are pointed out. (orig.)

  19. Determinação espectrofotométrica e cromatográfica em fase gasosa de ácido tricloracético em urina Spectrophotometric and gas chromatographic determination of trichloroacetic acid in urine

    Directory of Open Access Journals (Sweden)

    Maria de Fatima M. Pedrozo

    1996-06-01

    Full Text Available Solventes halogenados -- 1,1,1-tricloretano, tricloretileno, percloretileno -- apresentam o ácido tricloracético (TCA como produto de biotransformação comum, o qual pode ser utilizado como indicador biológico de dose interna na exposição a estes compostos. Foi realizado estudo de métodos espectrofotométrico e cromatográfico em fase gasosa para a determinação do TCA, bem como da aplicação destes métodos à sua determinação em urina de indivíduos expostos ao 1,1,1-tricloretano. Os resultados mostram a boa precisão à determinação do TCA em urina de indivíduos expostos ao 1,1,1-tricloretano e nenhuma diferença significativa foi observada entre os métodos, ainda que o cromatográfico em fase gasosa apresentasse menor limite de detecção.Some chlorinated hydrocarbon solvents -- 1,1,1-trichloroethane, tricloroethylene and perchloroethylene -- have a common biotransformation product, trichloroacetic acid, which can be used as their biological exposure index. The spectrophotometric and gas chromatographic methods for the determination of trichloroacetic acid were studied and used as well as in its determination in the urine of workers exposed to 1,1,1-trichloroethane . Both methods showed good precision and no statistically significant difference was found although the gas cromatographic method presented a lower detection limit.

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

    Directory of Open Access Journals (Sweden)

    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.

  1. 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...

  2. Ocorrência de aflatoxinas em arroz consumido por militares do Exército Brasileiro por cromatografia em camada delgada e cromatografia líquida de alta eficiência Incidence of aflatoxins in rice to be consumed by militaries in the brazilian army by thin layer chromatography and high performance liquid chromatography methods

    Directory of Open Access Journals (Sweden)

    Jader Oliveira da Silva

    2008-08-01

    Full Text Available Fungos do gênero Aspergillus como A. flavus e A. parasiticus são capazes de produzir metabólitos secundários tóxicos denominados aflatoxinas. Estas espécies podem se desenvolver rapidamente em cereais sob condições favoráveis. A partir do conhecimento dos riscos à saúde decorrentes da presença de aflatoxinas em alimentos, foi realizado um levantamento para avaliar a presença de aflatoxinas em arroz beneficiado polido tipo I, destinado ao consumo dos militares do Exército Brasileiro. As amostras foram coletadas no armazém do 5º Batalhão de Suprimento do Exército Brasileiro, Curitiba-PR no período de novembro de 2003 a fevereiro de 2004 e avaliada a ocorrência de aflatoxinas B1, B2, G1 e G2, utilizando-se as técnicas de Cromatografia em Camada Delgada (CCD e Cromatografia Líquida de Alta Eficiência (CLAE. Objetivou-se, neste trabalho, contribuir com o controle de qualidade dos alimentos consumidos pelos militares da 5º Região Militar do Exército Brasileiro, no que se refere ao controle dos níveis de aflatoxinas e comparar as técnicas de CCD e CLAE. Do total de 30 amostras analisadas por cromatografia em camada delgada, não foi verificada em nenhuma a presença de aflatoxinas. De 26 amostras analisadas por cromatografia líquida de alta eficiência, seis (23,07% apresentaram positividade para aflatoxina B1 (AFB1, com níveis entre 0,54 e 2,04µg/kg e uma (3,84% apresentou presença de aflatoxina B2 (AFB2 com 1,84µg/kg.Aspergillus are fungal species like a A flavus and A parasiticus and they are able to develop secondary metabolites called mycotoxins. They grow quickly under ideal conditions. From the moment one discovered its danger for health resulted from the presence of aflatoxins in foods, an achievement was carried out to evaluate the presence of a mycotoxins lifiting in benefited polished rice type 1, used by Brazilian army. The samples were collected at " 5º Batalhão de Suprimento" (army departament from

  3. 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 determi

  4. Semi-automated non-target processing in GC × GC-MS metabolomics analysis: Applicability for biomedical studies

    NARCIS (Netherlands)

    Koek, M.M.; Kloet, F.M. van der; Kleemann, R.; Kooistra, T.; Verheij, E.R.; Hankemeier, T.

    2011-01-01

    Due to the complexity of typical metabolomics samples and the many steps required to obtain quantitative data in GC × GC-MS consisting of deconvolution, peak picking, peak merging, and integration, the unbiased non-target quantification of GC × GC-MS data still poses a major challenge in metabolomic

  5. Determinação simultânea de quatro anticonvulsiviantes por cromatografia liquida de alta pressão (HPLC

    Directory of Open Access Journals (Sweden)

    A. Andriolo

    1984-09-01

    Full Text Available São revistas as indicações de monitorização terapêutica dos quatro anticonvulsivantes de maior aplicação» na prática médica diária em nosso meio e é descrito um método simples, sensível e preciso de quantificação destas drogas em soro ou plasma, por cromatografia líquida de alta pressão. O método permite a determinação simultânea de fenobarbital, fenitoína, carbamazepina e primidona, que são perfeitamente separados dos componentes normais do plasma e de outros medicamentos eventualmente presentes na amostra. A eluição foi monitorizada em 214 nm e a concentração de cada uma das drogas foi calculada pela relação entre as alturas dos picos destas com a dos respectivos padrões. Os resultados foram comparados com os obtidos por enzima-imunoensaio, apresentando os seguintes coeficientes de correlação: fenobarbital r= 0,990, fenitoína r = 0,993, carbamazepina r = 0,994 e primidona r = 0,992. Algumas outras drogas foram analisadas no sentido de avaliar eventuais interferências.

  6. Caracterização físico-química e análises por espectrofotometria e cromatografia de Peperomia pellucida L. (H. B. K.

    Directory of Open Access Journals (Sweden)

    R.M.F. Silva

    2013-01-01

    Full Text Available O objetivo deste trabalho foi realizar a caracterização físico-química do pó e da tintura, e análise por espectrofotometria e cromatografia do extrato seco de Peperomia pellucida L. (H. B. K.. As metodologias seguiram a Farmacopéia Brasileira IV ed., com exceção da prospecção química, da espectrofotometria, da obtenção do perfil cromatográfico do extrato seco, e determinação do resíduo seco. A prospecção química revelou a presença de saponinas espumídicas; açúcares redutores; proteínas e aminoácidos; fenóis; taninos; flavonóides; esteróides e triterpenóides. Na análise por CCD, o melhor perfil da fração flavonoídica foi obtido com MeOH/CHOOH (90:10. Foi confirmada, através de CLAE, a presença de 3',4',7-tri-O-metoxiflavona no extrato seco deste material vegetal. Os resultados obtidos contribuem para a determinação de especificações de uma futura monografia em Farmacopéias da Peperomia pellucida L. (H.B.K..

  7. 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

    Directory of Open Access Journals (Sweden)

    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

  8. 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

  9. 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

    Directory of Open Access Journals (Sweden)

    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

  10. Outdoor and indoor benzene evaluation by GC-FID and GC-MS/MS

    OpenAIRE

    José A. Sousa; Domingues, Valentina F.; Rosas, Mónica S.; Ribeiro, Susana; Alvim-Ferraz, Maria da Conceição M.

    2011-01-01

    The evaluation of benzene in different environments such as indoor (with and without tobacco smoke), a city area, countryside, gas stations and near exhaust pipes from cars running on different types of fuels was performed. The samples were analyzed using gas chromatography (GC) with flame ionization detection (FID) and tandem mass spectrometric detection (MS/MS) (to confirm the identification of benzene in the air samples). Operating conditions for the GC-MS analysis were optimized ...

  11. Identification and determination of (+)-sesamin in Semen Cuscutae by capillary GC and GC-MS

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    (+)-Sesamin was found in Semen Cuscutae for the first time. A rapid and simple approach for the analysis of (+)-sesamin in different sources of Semen Cuscutae is proposed, which used GC-FID for the determination of (+)-sesamin and GC-MS for its identification. The result suggested that this approach could be used to identify Semen Cuscutae from various sources based on the different content of (+)-sesamin in them.

  12. Copolímeros de estireno-divinilbenzeno para aplicação em cromatografia de exclusão por tamanho Styrene-Divinylbenzene copolymers for application in size exclusion chromatography

    Directory of Open Access Journals (Sweden)

    Márcia Angelica F.S. Neves

    1997-09-01

    Full Text Available Copolímeros de estireno-divinilbenzeno para a aplicação em cromatografia de exclusão por tamanho foram sintetizados através de polimerização em suspensão aquosa modificada pela presença de diluentes. Na síntese dos copolímeros foram variados os seguintes parâmetros reacionais: tipo de diluente, grau de diluição e teor de divinilbenzeno. Os copolímeros obtidos como partículas esféricas com tamanho médio em torno de 10 µm foram caracterizados quanto à porosidade no estado seco e às propriedades de inchamento. Os copolímeros foram utilizados como material de empacotamento de colunas para cromatografia de exclusão por tamanho (SEC. O aumento do grau de diluição na síntese do copolímero aumentou o limite de exclusão da cromatografia, porém a redução do poder solvatante do diluente teve um efeito mais pronunciado sobre esse parâmetro.Styrene-divinylbenzene copolymers were synthesized by modified suspension polymerization in presence of diluents. In the copolymers synthesis, the following reaction parameters were varied: diluent type, dilution degree and divinylbenzene content. The copolymers obtained as spherical particles with average diameter around 10 µm. were characterized by their porosity in dry state and by their swelling properties. The copolymers were applied as packing material of size exclusion chromatography columns. The increase of dilution degree in the copolymer synthesis increased the chromatography exclusion limit, but the decrease of diluent-copolymer affinity provoked a more accentuated effect on that parameter.

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

    Directory of Open Access Journals (Sweden)

    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

  14. Analysis of intra-genomic GC content homogeneity within prokaryotes

    DEFF Research Database (Denmark)

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

    2010-01-01

    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......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...... 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...

  15. Quantificação de sulfonamidas em leite por cromatografia líquida de alta eficiência via azoderivados Sulfonamides quantification in milk by high performace liquid chromatography via azoderivatives

    OpenAIRE

    Marcelo Volpatto Marques; Fabrício Fredo Naciuk; Ana Maria de Souza Mello; Nair Maria Seibel; João Gabriel Rosa dos Santos; Luiz Antonio Mazzini Fontoura

    2008-01-01

    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 quant...

  16. Modern methods of sample preparation for GC analysis

    OpenAIRE

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

    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 of ‘modern’ sample-preparation techniques has been introduced, which have partly superseded their ‘classical’ counterparts. These novel techniques include off-line and on-line (sometimes semi- or f...

  17. Determination of phthalates in polymer materials - comparison of GC/MS and GC/ECD methods

    Directory of Open Access Journals (Sweden)

    Katarzyna Jaworek

    2013-01-01

    Full Text Available The paper presents two methods for determination of phthalates in polymer materials. The methods compared were gas chromatography combined with the mass spectrometry (GC/MS and gas chromatography with electron capture detector (GC/ECD. The GC/ECD technique was chosen for this comparison, because the ECD detector was one of few capable of detecting phthalates. In both cases the same procedure of sample preparation with ultrasonic extraction was applied. Overall recoveries were 76-100 % with relative of standard deviation (R.S.D. values in the range 0.6-19 %. The values of limit of detection (LOD for GC/MS method ranged from 3.46 µg mL- 1 to 10.10 µg mL- 1, depending on the determined phthalate, while in case of the GC/ECD method they were in the range from 2.97 µg mL- 1 to 4.29 µg mL- 1. The methods were applied for determination of: dimethyl phthalate, diethyl phthalate, di-n-butyl phthalate, benzyl butyl phthalate, bis(2-ethylhexyl phthalate, diisononyl phthalate, diisoocyl phthalate in polymer material. The seventeen kinds of samples were analyzed. Most of the materials selected for the analyses were made from polyethylene (PE, polyvinyl chloride (PVC and polystyrene (PS.

  18. Gc globulin as a diagnostic and prognostic marker in horses

    DEFF Research Database (Denmark)

    Pihl, Tina Holberg

    Group specific (Gc) globulin also known as vitamin D-binding protein is part of the extracellular actin-scavenging system that removes actin from the circulation. Actin is an intracellular structural protein, which is released to blood in patients with tissue injury and cell death. Circulating...... 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...

  19. Choosing between GC FTIR and GC MS spectra for an efficient intelligent identification of illicit amphetamines

    Science.gov (United States)

    Gosav, S.; Dinica, R.; Praisler, M.

    2008-09-01

    In this paper we are presenting a comparative analysis between several expert systems built for the identification of illicit amphetamines based on their GC-FTIR and GC-MS spectra. The systems were built using Artificial Neural Networks (ANNs), and are dedicated to the recognition of amphetamines. Structure-activity relationships are incorporated into the knowledge base, allowing the systems to identify the amphetamines according to their toxicological activity (stimulant or hallucinogenic). The results show that GC-FTIR data are much more relevant for the efficiency of the expert systems, probably due to the fact that these spectra constitute a "fingerprint" of the molecular structures. We are also presenting a spectroscopic analysis in order to evaluate the relevance of each type of input variable (absorption and abundance) on which the recognition of an unknown sample is based.

  20. Analysis of intra-genomic GC content homogeneity within prokaryotes

    Directory of Open Access Journals (Sweden)

    Bohlin Jon

    2010-08-01

    Full Text Available Abstract Background 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 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 of the total genome. A low GCVAR indicates intra-genomic GC homogeneity and high GCVAR heterogeneity. Results The regression analyses indicated that GCVAR was significantly associated with domain (i.e. archaea or bacteria, phylum, and oxygen requirement. GCVAR was significantly higher among anaerobes than 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 was also found but appears to be non-linear and varies greatly among phyla. Conclusions Our findings show that GCVAR is linked with oxygen requirement, while mean genomic GC content is not. We therefore suggest that GCVAR should be used as a complement to mean GC content.

  1. Chemical composition of the essential oils from two subspecies of Protium heptaphyllum Composição química do óleo essencial de duas subespécies do Protium heptaphyllum

    Directory of Open Access Journals (Sweden)

    Delcio Dias Marques

    2010-03-01

    Full Text Available Qualitative and quantitative analyses of the volatile constituents from resin of Protium heptaphyllum (Aubl. Marchand subsp. ulei (Swat Daly (PHU, and Protium heptaphyllum (Aubl. Marchand subsp. heptaphyllum (PHH, Burseraceae were performed using GC-MS and GC-FID. The resins were collected around the city of Cruzeiro do Sul, state of Acre, Brazil. Essential oils from the two subspecies were extracted by hydrodistillation with a yield of 8.6% (PHU and 11.3% (PHH; the main components were terpinolene (42.31% and p-cymene (39.93% for subspecies ulei (PHU and heptaphyllum (PHH, respectively.As análises qualitativa e quantitativa dos óleos essenciais obtidos das resinas das espécies Protium heptaphyllum (Aubl. Marchand subespécie ulei (Swat Daly (PHU e Protium heptaphyllum (Aubl. Marchand subespécie heptaphyllum (PHH, Burseraceae, foram realizadas utilizando cromatografia em fase gasosa acoplado a um espectrômetro de massa (CG-EM e cromatografia a gás com detector de chama (CG-DIC. As resinas foram coletadas no Município de Cruzeiro do Sul, Acre, Brasil. O óleo essencial das oleoresinas foi extraído por hidrodestilação fornecendo rendimento 8,6% para PHU e 11,3% para PHH. Os monoterpenos terpinoleno (42.31% e p-cimeno (39.93% foram os constituintes principais para PHU e PHH, respectivamente.

  2. Analysis of Turkish lignite tar by coupled LC/GC, GC/MS, and capillary SFC

    Energy Technology Data Exchange (ETDEWEB)

    Davies, I.L.; Raynor, M.W.; Urwin, D.J.; Bartle, K.D.; Tolay, M.; Ekinci, E.; Schwartz, H.E.

    1988-11-01

    This work describes the analysis of a pyrolysis product of a lignite sample obtained from the Turkish Goynuk reserve. The aliphatic, aromatic and polar compounds present in the tar are separated and identified by various chromatographic techniques: capillary gas chromatography/mass spectrometry (GC/MS), on-line high performance microbore liquid chromatography/capillary gas chromatography (LC/GC) and capillary supercritical fluid chromatography (SFC). The suitability of each technique for this particular application is discussed, and semi-quantitative results are presented for the major components detected. 35 refs., 6 figs., 3 tabs.

  3. Accumulation of GC donor splice signals in mammals

    Directory of Open Access Journals (Sweden)

    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.

  4. Electrochemical impedance studies of methanol oxidation on GC/Ni and GC/NiCu electrode

    Energy Technology Data Exchange (ETDEWEB)

    Danaee, I.; Jafarian, M.; Forouzandeh, F.; Mahjani, M.G. [Department of Chemistry, K.N. Toosi University of Technology, PO Box 15875-4416, Tehran (Iran); Gobal, F. [Department of Chemistry, Sharif University of Technology, PO Box 11365-9516, Tehran (Iran)

    2009-01-15

    The electro-oxidation of methanol on nickel and nickel-copper alloy modified glassy carbon electrodes (GC/Ni and GC/NiCu) in a 1 M NaOH solution at different concentrations of methanol was studied by the method of ac-impedance spectroscopy. Two semicircles in the first quadrant of a Nyquist diagram were observed for electro-oxidation of methanol on GC/Ni corresponding to charge transfer resistance and adsorption of intermediates. Electro-oxidation of methanol on GC/NiCu shows negative resistance in impedance plots as signified by semi-circles terminating in the second quadrant. The impedance behavior shows different patterns at different applied anodic potential. The influence of the electrode potential on impedance pattern is studied and a mathematical model was put forward to quantitatively account for the impedance behavior of methanol oxidation. At potentials higher than 0.49 V vs. Ag/AgCl, a pseudoinductive behavior is observed but at higher than 0.58 V, impedance patterns terminate in the second quadrant. The conditions required for this behavior are delineated with the use of the impedance model. (author)

  5. Water status and gas exchange of umbu plants (Spondias tuberosa Arr. Cam. propagated by seeds and stem cuttings Estado hídrico e trocas gasosas de umbuzeiros (Spondias tuberosa Arr. Cam. propagados por sementes e estaquia

    Directory of Open Access Journals (Sweden)

    José Moacir Pinheiro Lima Filho

    2007-08-01

    Full Text Available The experiment was carried out at the Embrapa Semi-Árido, Petrolina-PE, Brazil, in order to study the physiological responses of umbu plants propagated by seeds and by stem cuttings under water stress conditions, based on leaf water potential and gas exchange measurements. Data were collected in one-year plants established in pots containing 30 kg of a sandy soil and submitted to twenty-day progressive soil water deficit. The evaluations were based on leaf water potential and gas exchange data collection using psychrometric chambers and a portable infra-red gas analyzer, respectively. Plants propagated by seeds maintained a significantly higher water potential, stomatal conductance, transpiration and photosynthesis under decreasing soil water availability. However, plants propagated by stem cuttings were unable to maintain a favorable internal water balance, reflecting negatively on stomatal conductance and leaf gas exchange. This fact is probably because umbu plants propagated by stem cuttings are not prone to formation of root tubers which are reservoirs for water and solutes. Thus, the establishing of umbu plants propagated by stem cuttings must be avoided in areas subjected to soil water deficit.O experimento foi realizado na Embrapa Semi-Árido, Petrolina-PE, Brasil, objetivando estudar as respostas fisiológicas de umbuzeiros propagados por sementes e por estaquia, sob condições de deficiência hídrica. Os dados foram coletados em plantas com aproximadamente um ano de idade, estabelecidas em vasos contendo 30 kg de solo de textura arenosa e submetidas a déficit progressivo de água, durante 20 dias. As avaliações foram realizadas, tomando-se como base o potencial hídrico foliar e as trocas gasosas, monitorados com auxílio de câmaras psicrométricas e um analisador portátil de gás por infravermelho, respectivamente. As plantas propagandas por sementes mantiveram valores de potencial hídrico, condutância estomática, transpira

  6. 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

    Directory of Open Access Journals (Sweden)

    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

  7. DWPF GC FILTER ASSEMBLY SAMPLING AND ANALYSIS

    Energy Technology Data Exchange (ETDEWEB)

    Bannochie, C.; Imrich, K.

    2009-11-11

    On March 18, 2009 a Defense Waste Processing Facility (DWPF) GC Line Filter Assembly was received at the Savannah River National Laboratory (SRNL). This filter assembly was removed from operation following the completion of Sludge Batch 4 processing in the DWPF. Work on this sample was requested in a Technical Assistance Request. This document reports the pictures, observations, samples collected, and analytical results for the assembly. The assembly arrived at SRNL separated into its three component filters: high efficiency particulate air (HEPA)-1, HEPA-2, and a high efficiency mist evaporator (HEME). Each stage of the assembly's media was sampled and examined visually and by scanning electron microscopy (SEM). Solids built up in the filter housing following the first stage HEME, were dissolved in dilute nitric acid and analyzed by ICP-AES and the undissolved white solids were analyzed by x-ray diffraction (XRD). The vast majority of the material in each of the three stages of the DWPF GC Line Filter Assembly appears to be contaminated with a Hg compound that is {approx}59 wt% Hg on a total solids basis. The Hg species was identified by XRD analysis to contain a mixture of Hg{sub 4}(OH)(NO{sub 3}){sub 3} and Hg{sub 10}(OH){sub 4}(NO{sub 3}){sub 6}. Only in the core sample of the second stage HEPA, did this material appear to be completely covering portions of the filter media, possibly explaining the pressure drops observed by DWPF. The fact that the material migrates through the HEME filter and both HEPA filters, and that it was seen collecting on the outlet side of the HEME filter, would seem to indicate that these filters are not efficient at removing this material. Further SRAT off-gas system modeling should help determine the extent of Hg breakthrough past the Mercury Water Wash Tank (MWWT). The SRAT off-gas system has not been modeled since startup of the facility. Improvements to the efficiency of Hg stripping prior to the ammonia scrubber would seem

  8. Predicting Partitioning and Diffusion Properties of Nonpolar Chemicals in Biotic Media and Passive Sampler Phases by GC × GC.

    Science.gov (United States)

    Nabi, Deedar; Arey, J Samuel

    2017-02-14

    The chemical parameters needed to explain and predict bioavailability, biodynamics, and baseline toxicity are not readily available for most nonpolar chemicals detected in the environment. Here, we demonstrate that comprehensive two-dimensional gas chromatography (GC × GC) retention times can be used to predict 26 relevant properties for nonpolar chemicals, specifically: partition coefficients for diverse biotic media and passive sampler phases; aquatic baseline toxicity; and relevant diffusion coefficients. The considered biotic and passive sampler phases include membrane and storage lipids, serum and muscle proteins, carbohydrates, algae, mussels, polydimethylsiloxane, polyethylene, polyoxymethylene, polyacrylate, polyurethane, and semipermeable membrane devices. GC × GC-based chemical property predictions are validated with a compilation of 1038 experimental property data collected from the literature. As an example application, we overlay a map of baseline toxicity to fathead minnows onto the separated analyte signal of a polychlorinated alkanes (chlorinated paraffins) technical mixture that contains 7820 congeners. In a second application, GC × GC-estimated properties are used to parametrize multiphase partitioning models for mammalian tissues and organs. In a third example, we estimate chemical depuration kinetics for mussels. Finally, we illustrate an approach to screen the GC × GC chromatogram for nonpolar chemicals of potentially high concern, defined based on their GC × GC-estimated biopartitioning properties, diffusion properties, and baseline toxicity.

  9. 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

  10. Quantitation using GC-TOF-MS: example of bromazepam.

    Science.gov (United States)

    Aebi, B; Sturny-Jungo, R; Bernhard, W; Blanke, R; Hirsch, R

    2002-08-14

    Time-of-flight mass spectrometry (TOF-MS) offers new perspectives for forensic toxicology. Qualitative and quantitative analyses of a mixture of three selected benzodiazepines (diazepam, nordazepam and bromazepam) were used to compare gas chromatography (GC-TOF-MS, quadrupole GC-MS, GC-ECD) and liquid chromatography (HPLC-DAD) data. Method validation parameters like LOD, LOQ, S/N-ratios reflect the capabilities of GC-TOF-MS. Five-point calibrations for bromazepam in human peripheral blood (50, 100, 160, 200, 300 ng/ml) using medazepam as internal standard (1000 ng/ml) were performed. The calibrations using GC-TOF-MS (using the fragments of m/z 236 and 288), GC-ECD (dual system) and HPLC-DAD (at 235 nm) all showed correlation coefficients close or superior to 0.99. Quadrupole GC-MS data was not used in the comparison of extracted samples due to the low sensitivity in the full scan mode. Two analyses of real cases concerning bromazepam are presented. In the first case, the presence or absence of bromazepam could not be established with both HPLC-DAD and GC-ECD due to background signals. The extracted ion chromatograms and spectrum traces after the analysis with the GC-TOF-MS could clearly excluded the presence of bromazepam. The second case illustrates the quantitation of bromazepam, where both HPLC-DAD and GC-ECD were unable to give satisfactory results, again due to interfering background signals. The analyses performed on the GC-TOF-MS-system demonstrated high sensitivity and also high selectivity due to the high quality of mass spectra obtained. The advantages of GC-TOF-MS make it a promising analytical technique for forensic toxicology.

  11. SSR Cluster and Fertility Loci Analysis of GC13

    Institute of Scientific and Technical Information of China (English)

    NONG Bao-xuan; XIA Xiu-zhong; LIANG Yao-mao; LU Gang; ZHANG Zong-qiong; LI Dan-ting

    2011-01-01

    [Objective] The research aimed to clarify the genetic mechanism of special wide compatibility of GC13.[Method] The clustering analyses of GC13,five indica,five japonica and five wide compatibility varieties were carried out by using 70 SSR primers.[Result] GC13 was clustered into japonica group and had far genetic relationship with indica and wide compatibility variety.Two fertility loci were detected in GC13,in which one closely linked to RM225 on chromosome 6.According to the position on the chromosome,it speculated that this locus was allelic to S5.GC13 carried the allelic gene S5-n at this locus.The other locus closely linked to RM408 on chromosome 8 and was provisionally designated as Sg(t).At this locus,GC13 carried Sg(t)-i allelic gene,which was consistent with IR36.The effect of S5 locus was stronger than that of Sg(t).[Conclusion] The research laid the good foundation for using the wide compatibility line GC13 to breed the hybrid between subspecies.%[Objective] The research aimed to clarify the genetic mechanism of special wide compatibility of GC13.[Method] The clustering analyses of GC13,five indica,five japonica and five wide compatibility varieties were carried out by using 70 SSR primers.[Result

  12. Avaliação das técnicas de determinação de Nitrogênio por cromatografia iônica (IC e por teor de nitrogênio total (TN por quimiluminescência

    Directory of Open Access Journals (Sweden)

    Lucélia Hoehne

    2015-12-01

    Full Text Available A determinação de nitrogênio pode ser feita por diferentes técnicas, tais como Kjedahl, Nitrogênio Total (NT por quimioluminescência, cromatografia iônica (IC, entre outras. A determinação do nitrogênio total proposta por Kjeldahl em 1883, ainda é muito usada por ser uma técnica confiável, porém, tem a desvantagem de gerar resíduos e ter o tempo de análise elevado. Desse modo, outras técnicas recentes podem ser usadas para determinar o nitrogênio, reduzindo os resíduos e tempo de análise. A luminescência é o fenômeno caracterizado pela emissão de luz de uma molécula que estava no seu estado excitado. A quimioluminescência é amplamente utilizada para determinar a concentração dos óxidos de nitrogênio nos gases de combustão. Já a cromatografia iônica é uma variante da cromatografia líquida que utiliza resinas de troca iônica para separar íons atômicos ou moleculares com base na sua interação com a resina. Dessa forma, este trabalho tem o objetivo de comparar as técnicas de IC e de quimioluminescência para a determinação de nitrogênio em amostras aquosas. Para isso, foram feitos padrões de nitrogênio e as amostras foram avaliadas nas duas técnicas. Verificou-se o tempo de análise, bem como o preparo da amostra. Também foi verificada a linearidade da curva em cada técnica. Como resultado, foi visto que ambas apresentaram dados satisfatórios e resultados semelhantes.

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

    Directory of Open Access Journals (Sweden)

    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.

  14. Sulfonamidas em leite por cromatografia líquida de alta eficiência com derivação pré-coluna e detecção por fluorescência

    OpenAIRE

    ALABURDA, J.; RUVIER, V.; SHUNDO, L.; de Almeida, A. P.; TIGLEA, P.; M. Sabino

    2007-01-01

    O objetivo deste trabalho foi avaliar e validar um método para deteminação de resíduos de sulfatiazol (STZ), sulfametazina (SMZ) e sulfadimetoxina (SDM) em leite UHT integral. A extração foi realizada com diclorometano e coluna de extração em fase sólida de sílica. Os resíduos, após derivação com fluorescamina, foram quantificados por cromatografia líquida de alta eficiência com detector de fluorescência. O limite de detecção das três sulfas em amostra de leite integral foi 0,3 µg L-1 e o lim...

  15. Isolamento químico e validação analítica por cromatografia líquida de alta eficiência de quercitrina em Solidago chilensis Meyen (Asteraceae

    Directory of Open Access Journals (Sweden)

    C.A.D. VECHIA

    2016-01-01

    Full Text Available RESUMO A espécie Solidago chilensis Meyen, Asteraceae é conhecida como erva-lanceta ou arnica-brasileira, sendo utilizada popularmente como antimicrobiana e para o tratamento de inflamações tópicas. No entanto, estudos fitoquímicos e farmacológicos para as partes aéreas são escassos. Neste trabalho, realizou-se a determinação de flavonoides por espectrofotometria de UV/Vis, prospecção fitoquímica da fração acetato de etila visando o isolamento do constituinte químico majoritário e validação analítica por cromatografia líquida de alta eficiência (CLAE. O teor de flavonoides totais foi de 5,42%, representados como hiperosídeo. O fracionamento químico utilizando métodos cromatográficos (cromatografia líquida em coluna gel de sílica; CHCl3:EtOH; 8:2 v/v e espectroscópicos (1H RMN,13C RMN e ESI-MS revelou o isolamento de quercetina-3-O-α-L-ramnosídeo(quercitrina. A sensibilidade e a linearidade (r = 0,999 da validação analítica, utilizando a quercitrina isolada do extrato hidroalcoólico da planta, revelaram um rendimento de 5,29% do analito em relação à droga vegetal. Precisão, recuperação e robustez, além dos valores estabelecidos para os limites de detecção (LOD e de quantificação (LOQ, poderão ser utilizados como parâmetros de qualidade para extratos à base de S. chilensis.

  16. Trocas gasosas em videira sob regime de estresse hídrico. II. fotorrespiração e comportamento varietal Gas exchanges in grapevines under water stress regime. II. photorespiration and varietal behavior

    Directory of Open Access Journals (Sweden)

    Murillo de Albuquerque Regina

    1999-01-01

    Full Text Available Analisou-se a fotorrespiração em folhas de videira (Vitis vinifera L. submetidas a um regime de estresse hídrico, com o objetivo de caracterizar o comportamento de diferentes cultivares. Foram utilizadas plantas de dois anos, enxertadas sobre o porta-enxerto Fercal, plantadas em vasos plásticos e cultivadas em ambiente controlado. A fotorrespiração foi calculada a partir de medidas das trocas gasosas foliares. Os valores absolutos da fotorrespiração variaram pouco entre cultivares e nível de irrigação; já a eficiência da carboxilação e o ponto de compensação ao CO2 foram bastante afetados pelo estresse hídrico, o que revela diferentes níveis de sensibilidade varietal. Foi verificada a ocorrência de inibição não-estomática da fotossíntese, afetando diferencialmente as cultivares analisadas. Destacou-se, ainda, a maior adaptação da Chardonnay às condições de estresse hídrico, em oposição à grande sensibilidade da Sémillon e da Ugni blanc.The photorespiration in grapevines (Vitis vinifera L. leaves subjected to a water stress regime was analysed with the purpose of characterizing the behavior of different cultivars. Two-year old plants were used, grafted on Fercal, planted in plastic pots and cultivated in controlled environment. The photorespiration was calculated from leaf gas exchange measurements taken by means of a portable infrared CO2 analyser (LCA3-ADC, working in an open circuit. The absolute photorespiration values varied little among cultivars and level of irrigation, whereas the carboxylation efficiency and the CO2 compensation point were highly affected by the water stress, thereby evidencing different varietal sensitivity levels. The occurrence of a nonstomatal inhibition of the photosynthesis was verified affecting in a specific way the cultivars analysed. The Chardonnay adapted itself better to the water stress conditions as opposed to the high sensitivity on the part of Sémillon and Ugni blanc.

  17. 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 additi

  18. Outdoor and indoor benzene evaluation by GC-FID and GC-MS/MS.

    Science.gov (United States)

    Sousa, José A; Domingues, Valentina F; Rosas, Mónica S; Ribeiro, Susana O; Alvim-Ferraz, Conceiçao M; Delerue-Matos, Cristina F

    2011-01-01

    The evaluation of benzene in different environments such as indoor (with and without tobacco smoke), a city area, countryside, gas stations and near exhaust pipes from cars running on different types of fuels was performed. The samples were analyzed using gas chromatography (GC) with flame ionization detection (FID) and tandem mass spectrometric detection (MS/MS) (to confirm the identification of benzene in the air samples). Operating conditions for the GC-MS analysis were optimized as well as the sampling and sample preparation. The results obtained in this work indicate that i) the type of fuel directly influences the benzene concentration in the air. Gasoline with additives provided the highest amount of benzene followed by unleaded gasoline and diesel; ii) the benzene concentration in the gas station was always higher than the advisable limit established by law (5 μg m⁻³) and during the unloading of gasoline the achieved concentration was 8371 μg m⁻³; iii) the data from the countryside (Taliscas) and the urban city (Matosinhos) were below 5 μg m⁻³ except 5 days after a fire on a petroleum refinery plant located near the city; iv) it was proven that in coffee shops where smoking is allowed the benzene concentration is higher (6 μg m⁻³) than in coffee shops where this is forbidden (4 μg m⁻³). This method may also be helpful for environmental analytical chemists who use GC-MS/MS for the confirmation or/and quantification of benzene.

  19. Characterization and classification of complex PAH samples using GC-qMS and GC-TOFMS.

    Science.gov (United States)

    Bergknut, Magnus; Frech, Kristina; Andersson, Patrik L; Haglund, Peter; Tysklind, Mats

    2006-12-01

    The aim of this study was to compare the polycyclic aromatic hydrocarbon (PAH) contents in a number of complex samples, including soil samples from industrial sites, anti-skid sand, urban dust and ash samples from municipal solid waste incinerators. The samples were characterized by routine analysis of PAHs (gas chromatography-quadrupole mass spectrometry) and gas chromatography-time of flight mass spectrometry (GC-TOFMS). Classification of the samples by principal component analysis (PCA) according to their composition of PAHs revealed that samples associated with traffic and the municipal incinerator formed homogeneous clusters, while the PAH-contaminated soils clustered in separate groups. Using spectral data to resolve co-eluting chromatographic peaks, 962 peaks could be identified in the GC-TOFMS analysis of a pooled sample and 123-527 peaks in the individual samples. Many of the studied extracts included a unique set of chemicals, indicating that they had a much more diverse contamination profile than their PAH contents suggested. Compared to routine analysis, GC-TOFMS provided more detailed information about each sample and in this study a large number of alkylated PAHs were found to be associated with the corresponding unsubstituted PAHs. The possibility to filter peaks according to different criteria (e.g. to include only peaks that were detected in the analysis of another sample) was explored and used to identify unique as well as common compounds within samples. This procedure could prove to be valuable for obtaining relevant chemical data for use in conjunction with results from various biological test systems.

  20. MDMA毒品简介及GC/MS分析%Determination of MDMA by GC/MS

    Institute of Scientific and Technical Information of China (English)

    张春水; 郑珲; 徐鹏

    2004-01-01

    对一例MDMA毒品案件进行技术检测,采用气质联用技术(GC/MS)准确分析了MDMA片剂中物质成分,检出了MDMA、胡椒素甲醛及咖啡因等成分,并建立了该类毒品检验的快速分析方法,为打击毒品犯罪提供了技术保障.

  1. Crescimento e índices de troca gasosa em plantas de pepino irrigadas com água enriquecida com CO2 Growth analysis and gaseous exchange in cucumber plants irrigated with carbon dioxide enriched water

    Directory of Open Access Journals (Sweden)

    Kathia A.L. Canizares

    2004-12-01

    Full Text Available Avaliou-se o efeito do enriquecimento da água de irrigação com CO2 sobre índices fisiológicos de desenvolvimento e troca gasosa de folhas de plantas de pepino do tipo japonês, cultivados em ambiente protegido. Os experimentos realizados em duas épocas do ano foram instalados em delineamento experimental de blocos ao acaso com 4 tratamentos e 5 repetições. Os tratamentos foram constituídos pelos híbridos Hokuho e Tsuyataro, irrigados com água comum ou enriquecida com CO2, em uma concentração de 1‰ no primeiro e 0,25‰ no segundo experimento. A produção de massa de material seco e área foliar adotaram tendência exponencial, não sendo possível observar o início da diminuição da taxa de produção de massa do material seco aos 63 dias após transplante (DAT. A taxa de crescimento da comunidade e taxa de crescimento relativa do híbrido Hokuho irrigado com água comum foi diferente do irrigado com água enriquecida com CO2, no entanto, no híbrido Tsuyataro foram semelhantes. A taxa de assimilação líquida atingiu a máxima pendente na fase de crescimento vegetativo e floração, e foi reduzida drasticamente após os 20 DAT no híbrido Hokuho, e após os 35 DAT no híbrido Tsuyataro. A razão de área foliar diminuiu ligeiramente nos dois híbridos com o desenvolvimento do cultivo. No início observaram-se diferenças entre irrigação com água comum e enriquecida com CO2, porém após 20 DAT não se apreciaram mais diferenças. Quanto a troca gasosa, a taxa assimilatória líquida de CO2 e de transpiração, conductância estomática e eficiência no uso da água foram semelhantes entre plantas irrigadas com água comum e enriquecida com CO2 durante o primeiro semestre. Já no segundo semestre, maiores valores foram registrados pelas plantas irrigadas com água enriquecida.Experiments under protected cultivation, in two sowing dates, were set up to evaluate the effect of irrigation water enriched or not with CO2, on

  2. Transporte de oócitos bovinos em meio de maturação sem controle de atmosfera gasosa Transport of bovine oocytes in maturation medium without a controlled gaseous atmosphere

    Directory of Open Access Journals (Sweden)

    Fábio Gallas Leivas

    2004-02-01

    Full Text Available Oócitos (n=1177 bovinos obtidos da aspiração de folículos com diâmetro entre 2 e 8mm, de ovários de matadouro foram divididos aleatoriamente em quatro tratamentos com 11 repetições. Os oócitos foram maturados por 24h em TCM-199 Sais de Earle, acrescido de 25mM de bicarbonato de sódio, 25mM de HEPES, rFHS-h, Soro de Vaca em Estro (SVE e piruvato, em estufa a 39ºC, com 5% de CO2 em ar e umidade saturada (Grupo Controle, n=296 ou, submetidos ao transporte simulado por 6 (T6, n=286, 12 (T12, n=294 ou 18h (T18, n=301 em meio de maturação TCM+HEPES, em banho-maria a 39ºC, com os mesmos componentes utilizados para o Grupo Controle, porém com apenas 1mM de bicarbonato. Decorrido cada período de transporte, os mesmos foram transferidos para placas com meio de maturação, completando o período de 24h em estufa, nas mesmas condições do Grupo Controle. O período de fecundação foi de 18h em condições semelhantes de temperatura e atmosfera gasosa, em FERT-TALP acrescido de heparina, sendo a dose inseminante de 1x106 espermatozóides/mL, selecionados por migração ascendente. Os prováveis zigotos foram cultivados em meio SOF + 5% SVE por 8 dias, em estufa a 39ºC, em bolsas gaseificadas com 5% CO2, 5% O2 e 90% N2. Na avaliação da clivagem, não houve diferença entre os tratamentos. As taxas de desenvolvimento embrionário no dia 7 foram semelhantes para os grupos Controle (20,9%, T6 (19,2% e T12 (21,4%, com uma redução (P0,05 na taxa de eclosão. O número médio de células dos blastocistos eclodidos não diferiu (P>0,05 entre os grupos Controle (136, T6 (125,5 e T12 (126,8. Esses resultados indicam a possibilidade do transporte de oócitos bovinos em meio de maturação TCM+HEPES, sem controle da atmosfera gasosa, a 39ºC, pelo período de até 12h. Esta técnica oferece uma alternativa prática e eficiente para o transporte dos oócitos bovinos destinados à produção in vitro de embriões bovinos (PIV.Oocytes (n=1177

  3. Evidence of selection upon genomic GC-content in bacteria.

    Directory of Open Access Journals (Sweden)

    Falk Hildebrand

    2010-09-01

    Full Text Available The genomic GC-content of bacteria varies dramatically, from less than 20% to more than 70%. This variation is generally ascribed to differences in the pattern of mutation between bacteria. Here we test this hypothesis by examining patterns of synonymous polymorphism using datasets from 149 bacterial species. We find a large excess of synonymous GC→AT mutations over AT→GC mutations segregating in all but the most AT-rich bacteria, across a broad range of phylogenetically diverse species. We show that the excess of GC→AT mutations is inconsistent with mutation bias, since it would imply that most GC-rich bacteria are declining in GC-content; such a pattern would be unsustainable. We also show that the patterns are probably not due to translational selection or biased gene conversion, because optimal codons tend to be AT-rich, and the excess of GC→AT SNPs is observed in datasets with no evidence of recombination. We therefore conclude that there is selection to increase synonymous GC-content in many species. Since synonymous GC-content is highly correlated to genomic GC-content, we further conclude that there is selection on genomic base composition in many bacteria.

  4. Hyphenated GC-FTIR and GC-MS techniques applied in the analysis of bioactive compounds

    Science.gov (United States)

    Gosav, Steluta; Paduraru, Nicoleta; Praisler, Mirela

    2014-08-01

    The drugs of abuse, which affect human nature and cause numerous crimes, have become a serious problem throughout the world. There are hundreds of amphetamine analogues on the black market. They consist of various alterations of the basic amphetamine molecular structure, which are yet not yet included in the lists of forbidden compounds although they retain or slightly modify the hallucinogenic effects of their parent compound. It is their important variety that makes their identification quite a challenge. A number of analytical procedures for the identification of amphetamines and their analogues have recently been reported. We are presenting the profile of the main hallucinogenic amphetamines obtained with the hyphenated techniques that are recommended for the identification of illicit amphetamines, i. e. gas chromatography combined with mass spectrometry (GC-MS) and gas chromatography coupled with Fourier transform infrared spectrometry (GC-FTIR). The infrared spectra of the analyzed hallucinogenic amphetamines present some absorption bands (1490 cm-1, 1440 cm-1, 1245 cm-1, 1050 cm-1 and 940 cm-1) that are very stable as position and shape, while their intensity depends of the side-chain substitution. The specific ionic fragment of the studied hallucinogenic compounds is the 3,4-methylenedioxybenzyl cation (m/e = 135) which has a small relative abundance (lesser than 20%). The complementarity of the above mentioned techniques for the identification of hallucinogenic compounds is discussed.

  5. Evaluation of GC-APCI/MS and GC-FID as a complementary platform.

    Science.gov (United States)

    Pacchiarotta, Tiziana; Nevedomskaya, Ekaterina; Carrasco-Pancorbo, Alegria; Deelder, André M; Mayboroda, Oleg A

    2010-12-01

    With a development of the metabolomics field, complementary cross-platform approaches started to attract attention, as none of the contemporary analytical methods had the capacity to cover the entire space of the human metabolome. In the current manuscript, we have evaluated an online coupling of gas chromatography (GC)-mass spectrometry (MS) and flame ionization detector (FID) as ways of cross-detector analysis. The possible value of this combination was recognized from the very first days of GC-MS history but was never explored in detail. We have compared the basic analytical parameters of both detectors, such as limit of detection (LOD) and limit of quantification, with intra- and interday reproducibility. We show that for the majority of the tested compounds, MS detector demonstrates lower LOD. At the same time, FID appeared to be more robust, showing lower relative standard deviations (RSDs) for intra- and interday reproducibility. We conclude that the gain of this dual detector acquisition appears to be most evident for complex biological samples, where wide dynamic range and predictable response of FID are useful for an initial quantitative overview of sample composition and estimation of molar proportions of different metabolites. MS provides reliable, structural information and superior, at least in the case of atmospheric pressure chemical ionization, sensitivity. Taken together, both detectors represent a flexible tool for explorative studies and if supported by a powerful data-processing algorithm, would appear to be useful in any metabolic profiling study.

  6. [GC x GC measurements of atmospheric aromatic compounds near a busy high-speed road in Beijing].

    Science.gov (United States)

    Mao, Ting; Xu, Xiao-bin; Wang, Ying

    2009-10-15

    Comprehensive two-dimensional gas chromatography (GC x GC) is a powerful instrumental tool often used to analyze complex mixtures. An optimized GC x GC method had been applied to the quantitative analysis of aromatic compounds in air samples collected near a busy high-speed road in Beijing during the 2007 National Holidays. In the resulting GC x GC chromatograms, aromatic species were resolved from other compound classes and were grouped in a manner that facilitated identification and integration, showing more information of aromatic compounds compared to traditional one-dimensional GC. Totally more than 30 aromatic species were identified and quantified. The average concentrations of monocyclic aromatic compounds ranged from 0.75 x 10(-9) to 24.64 x 10(-9) C, with toluene having the highest concentration, followed by m, p-xylene and ethylbenzene. The average concentrations of the measured polycyclic aromatic compounds ranged from 0.03 x 10(-9) to 2.28 x 10(-9) C, with naphthalene having the highest concentration, followed by 2-methyl-naphthalene and 4-methyl-1, 1'-biphenyl. The four-ring and higher polycyclic aromatic compounds were not detectable in the gaseous samples. The levels of aromatic compounds were significantly influenced by meteorological parameters. Benzene and toluene were poorly correlated with higher aromatic compounds though the latter compounds were highly correlated among each other, suggesting that both were significantly influenced by sources other than vehicle exhaust and gasoline evaporation.

  7. Micro GC's for Contaminant Monitoring in Spacecraft Air Project

    Data.gov (United States)

    National Aeronautics and Space Administration — Based on the successful separation of 20 compounds using a 1 m coated microcolumn in Phase I, we propose to design a new micro-gas chromatograph (microGC) system to...

  8. Fast GC for Space Applications Based on PIES Technology Project

    Data.gov (United States)

    National Aeronautics and Space Administration — Development of a novel analytical instrument which combines the advantages of fast GC and a detector capable of identifying species is proposed. Experiments in the...

  9. Fast GC for Space Applications Based on PIES Technology Project

    Data.gov (United States)

    National Aeronautics and Space Administration — This SBIR Phase II project is aimed at the development of an analytical instrument which combines the advantages of fast gas chromatography (GC) and a detector that...

  10. Application of GC-FID and GC-MS for assessing PAHs in suspended dust.

    Science.gov (United States)

    Weglarz, A; Skrok, R

    2000-07-01

    The social concern about polycyclic aromatic hydrocarbons (PAHs) is due to the awareness that several of them are carcinogens and are present in polluted air. Several epidemiological investigations have tried to assess the influence of air pollution on the incidence in the population (1). Some authors have suggest that 1-10% of the incidence of lung cancer is caused by air pollution (2, 3). Several sources, e.g. traffic, oil heating, wood stoves, industry may contribute PAHs to the air pollution. Therefore continuous air pollution control applying selective and precise analytical procedures is needed. The submitted work presents results of examination of sixteen polycyclic aromatic hydrocarbons [naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, chrysene, benzo(a)anthracene, benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(a)pyrene, indeno(1,2,3-cd)pyrene, dibenzo(a, h)anthracene, benzo(ghi)perylene] settled on particles of 10 microns fractions of ashes, emitted from industrial and communication sources. Samples of suspended dust were collected at twelve measuring points, from May to June 1998, in 24-hour cycles, in accordance with US EPA methodology. PAHs were extracted from suspended dust in a Soxhlet apparatus and then exposed to extraction in a liquid-solid system (solid extraction-SPE) to eliminate redundant pollution, which may interfere with compounds by determined analysis. Samples were then analyzed using by capillary gas chromatographs "Varian" model 3400 with FID and MS detectors. Results of analysis make it possible to determine the influence of industry and traffic on atmospheric pollution, to compare results of two analytical methods (GC-FID and GC-MS).

  11. The analysis of linear and monomethylalkanes in exhaled breath samples by GC×GC-FID and GC-MS/MS.

    Science.gov (United States)

    Hengerics Szabó, Alexandra; Podolec, Peter; Ferenczy, Viktória; Kubinec, Róbert; Blaško, Jaroslav; Soják, Ladislav; Górová, Renáta; Addová, Gabriela; Ostrovský, Ivan; Višňovský, Jozef; Bierhanzl, Václav; Čabala, Radomír; Amann, Anton

    2015-01-26

    A new arrangement of the INCAT (inside needle capillary adsorption trap) device with Carbopack X and Carboxen 1000 as sorbent materials was applied for sampling, preconcentration and injection of C6C19n-alkanes and their monomethyl analogs in exhaled breath samples. For the analysis both GC-MS/MS and GC×GC-FID techniques were used. Identification of the analytes was based on standards, measured retention indices and selective SRM transitions of the individual isomers. The GC-MS/MS detection limits were in the range from 2.1 pg for n-tetradecane to 86 pg for 5-methyloctadecane. The GC×GC-FID detection limits ranged from 19 pg for n-dodecane to 110 pg for 3-methyloctane.

  12. Detection of virgin coconut oil adulteration with animal fats using quantitative cholesterol by GC × GC-TOF/MS analysis.

    Science.gov (United States)

    Xu, Baocheng; Li, Peiwu; Ma, Fei; Wang, Xiuping; Matthäus, Bertrand; Chen, Ran; Yang, Qingqing; Zhang, Wen; Zhang, Qi

    2015-07-01

    A new method based on the cholesterol level was developed to detect the presence of animal fats in virgin coconut oil (VCO). In this study, the sterols in VCO and animal fats was separated using conventional one-dimensional gas chromatography (1D GC) and comprehensive two-dimensional gas chromatography (GC×GC). Compared with 1D GC, the GC×GC system could obtain a complete baseline separation of the sterol trimethylsilyl ethers derived from cholesterol and cholestanol, so that the cholesterol content in pure VCO and false VCO adulterated with animal fats could be accurately determined. Cholesterol, a main sterol found in animal fats, represented less than 5mg/kg of VCO. The study demonstrated that the determination of the cholesterol level in VCO could be used for reliable detection of the presence of lard, chicken fat, mutton tallow, beef tallow, or their mixture in VCO at a level as little as 0.25%.

  13. Relações hídricas e trocas gasosas em vinhedo sob cobertura plástica Water relations and leaf gas exchange in vineyard with plastic overhead cover

    Directory of Open Access Journals (Sweden)

    Geraldo Chavarria

    2008-12-01

    Full Text Available No presente estudo, determinaram-se as influências da cobertura plástica impermeável (CP sobre a demanda evaporativa atmosférica e o potencial da água no solo, bem como as conseqüências destas sobre as trocas gasosas foliares (fotossíntese, condutância estomática e transpiração e o potencial da água na folha da videira. As avaliações foram realizadas nos ciclos 2005/06 e 2006/07, em um vinhedo da cv. Moscato Giallo, conduzido em "Y", com cobertura plástica impermeável tipo ráfia (160 mm, em 12 fileiras com 35 m, deixando-se cinco fileiras sem cobertura (controle. Em ambas as áreas, avaliou-se o microclima quanto à temperatura do ar, umidade relativa do ar, radiação fotossinteticamente ativa e velocidade do vento, próximos ao dossel vegetativo. A CP aumentou a disponibilidade hídrica no solo nas entrelinhas e restringiu-a nas linhas, sobretudo em profundidades mais superficiais (0-10 cm. A CP também diminuiu a demanda evaporativa atmosférica, principalmente pela redução da velocidade do vento (-90%, aumentando o potencial da água na folha e a condutância estomática. De modo geral, a CP pode favorecer a condição hídrica e elevar a capacidade de assimilação de carbono em videiras.This study evaluated the plastic overhead cover (POC effect on evaporative demand of atmosphere and soil water content, as well as their consequences on gas exchange (photosynthesis, stomatal conductance and transpiration and leaf water potential in grapevine. The experiment was carried out during the 2005/06 and 2006/07 seasons, in a vineyard of 'Moscato Giallo', trained in "Y" and covered with an impermeable plastic cloth (2.65 m x 160 mm, in 12 rows with 35 m, with five rows left uncovered (control. In both areas, the microclimate was evaluated, in terms of air temperature, air relative humidity, radiation photosynthetically active and wind speed above the canopy. The POC increased the soil water content between rows and restricted it

  14. Growth and gas exchange in the cowpea under saline irrigation and rates of potassium = Crescimento e trocas gasosas de plantas de feijão-caupi sob irrigação salina e doses de potássio

    Directory of Open Access Journals (Sweden)

    Stella da Silva Prazeres

    2015-06-01

    quais foram submetidas a níveis crescentes de salinidade, utilizando-se água de irrigação com condutividade elétrica (CEa de 0,8; 2,2; 3,6 e 5,0 dS m-1 e doses crescentes de potássio (K na forma de KCl (0,5; 1,0; 2,0 e 4,0 g por vaso KCl. Aos 47 e aos 55 dias após o plantio (DAP foram realizadas leituras das trocas gasosas foliares e de crescimento das plantas (comprimento da haste principal, diâmetro do caule e matéria seca total, respectivamente. O aumento da salinidade da água de irrigação reduziu o comprimento da haste principal, diâmetro do caule e matéria seca total, em ambas as cultivares. As maiores doses de potássio em conjunto com a salinidade proporcionaram efeito depressivo no crescimento da haste principal e na condutância estomática, em comparação ao efeito isolado da salinidade, sendo um indicativo da intensificação dos efeitos osmóticos. A existência de interações entre salinidade e potássio é um indicativo de que a dose ótima desse nutriente depende da salinidade na zona radicular das plantas, sendo uma informação importante para o manejo de cultivos em ambientes salinos.

  15. Leaf traits and gas exchange in saplings of native tree species in the Central Amazon Características foliares e trocas gasosas em arvoretas de espécies nativas da Amazônia Central

    Directory of Open Access Journals (Sweden)

    Keila Rego Mendes

    2010-12-01

    Full Text Available Global climate models predict changes on the length of the dry season in the Amazon which may affect tree physiology. The aims of this work were to determine the effect of the rainfall regime and fraction of sky visible (FSV at the forest understory on leaf traits and gas exchange of ten rainforest tree species in the Central Amazon, Brazil. We also examined the relationship between specific leaf area (SLA, leaf thickness (LT, and leaf nitrogen content on photosynthetic parameters. Data were collected in January (rainy season and August (dry season of 2008. A diurnal pattern was observed for light saturated photosynthesis (Amax and stomatal conductance (g s, and irrespective of species, Amax was lower in the dry season. However, no effect of the rainfall regime was observed on g s nor on the photosynthetic capacity (Apot, measured at saturating [CO2]. Apot and leaf thickness increased with FSV, the converse was true for the FSV-SLA relationship. Also, a positive relationship was observed between Apot per unit leaf area and leaf nitrogen content, and between Apot per unit mass and SLA. Although the rainfall regime only slightly affects soil moisture, photosynthetic traits seem to be responsive to rainfall-related environmental factors, which eventually lead to an effect on Amax. Finally, we report that little variation in FSV seems to affect leaf physiology (Apot and leaf anatomy (leaf thickness.Os modelos climáticos globais prevêem mudanças na extensão da época seca na Amazônia, o que pode afetar a fisiologia das árvores. Os objetivos deste trabalho foram determinar o efeito da sazonalidade da precipitação e fração de céu visível (FSV no sub-bosque da floresta nas características foliares e trocas gasosas de 10 espécies florestais da Amazônia Central. Também examinou-se a relação entre área foliar específica (SLA, espessura da folha (LT e nitrogênio foliar em parâmetros fotossintéticos. Os resultados foram coletados nos

  16. Determination of elaidic and vaccenic acids in foods using GC×GC-FID and GC×GC-TOFMS.

    Science.gov (United States)

    Ha, Jaeho; Seo, Dongwon; Shin, Dongbin

    2011-07-15

    Trans fatty acids (TFAs) are present in meat and dairy products as m ruminant animals and in vegetable fats due to partial hydrogenation. This study aimed to discriminate between natural (N-TFA) and hydrogenated trans fatty (H-TFA) acids by GC×GC-flame ionization detection (GC×GC-FID) and comprehensive GC×GC-time-of-flight mass spectrometry (GC×GC-TOFMS). The separation of two kinds of trans fats, vaccenic acid (18:1 trans-11) and elaidic acid (18:1 trans-9), was performed using GC×GC-FID and GC×GC-TOFMS. A 100 m×0.25 mm I.D.×0.2 μm (film thickness) SP-2560 (bis-cyanopropyl polysiloxane) fused capillary column (first separation dimension, 1D) was coupled to a 1.5 m×0.18 mm I.D.×0.18 μm (film thickness) RTX-5 (5% diphenyl/95% dimethyl polysiloxane) fused capillary column (second separation dimension, 2D). The RSD of the intra-day repeatability by both GC×GC-FID and GC×GC-TOFMS for elaidic and vaccenic acids was ≤9.56% and ≤9.97%, and the RSD of the inter-day repeatability was ≤8.49 and ≤9.06%, respectively. It was found that the V/E value (vaccenic acid to elaidic acid ratio) could be used to distinguish H-TFA from N-TFA and to evaluate the quality of the fatty foods.

  17. 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.

  18. Aroma active components in aqueous kiwi fruit essence and kiwi fruit puree by GC-MS and multidimensional GC/GC-O.

    Science.gov (United States)

    Jordán, María J; Margaría, Carlos A; Shaw, Philip E; Goodner, Kevin L

    2002-09-11

    Gas chromatography-mass spectrometry (GC-MS) and multidimensional gas chromatography olfactometry (GC/GC-O) were utilized to study the aroma profile and the aroma active components of commercial kiwi essence and the initial fresh fruit puree. Totals of 29 and 33 components were identified and quantified in the essence and the puree, respectively. Ten components were quantified for the first time as constituents of the kiwi fruit including 3-penten-2-ol, 3-hydroxy-2-butanone, 3-methyl-2-butenal, 2-hexanol, nonanal, 3-methyl-1-butanol, 2-methyl-1-butanol, 3-methyl-2-butanone, 3-methyl 3-buten-2-one, and octane. Analysis of these samples by multidimensional gas chromatography-olfactometry (GC-O) allowed for the identification of >80% of the aroma active components present at level traces in this fruit. A total of 35 components appear to contribute to the aroma of kiwi fresh puree and its aqueous essence. Components described for the first time as constituents of the aroma profile in this fruit were 2-ethylfuran, 3-methyl-1-butanol, 2-cyclohexen-1-one, (E,E)-2,6-nonadienal, diethyl succinate, and hexyl hexanoate.

  19. 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...

  20. 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

    Directory of Open Access Journals (Sweden)

    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.

  1. CROMATOGRAFIA DE AFINIDADE COM CORANTE RED A versus TROCA IÔNICA-PERMEABILIDADE EM GEL: COMPARAÇÃO DA PRATICIDADE NA PURIFICAÇÃO DE ENTEROTOXINA ESTAFILOCÓCICA A

    Directory of Open Access Journals (Sweden)

    M. KAMOGAE

    1998-05-01

    Full Text Available O presente trabalho compara processos de purificação de enterotoxina estafilocócica A, utilizando cromatografia de afinidade com corante Red A em relação a troca iônica (SP - Sephadex C-25 - permeabilidade em gel (Sephadex G-75. Aplicou-se nas colunas o sobrenadante da cultura de Staphylococcus aureus 722 em caldo contendo 3% de triptona e suplementado com 1% de extrato de levedura, previamente concentradas com Amberlite CG-50. O processo capturou rapidamente a EEA, porém a proporção de 15 mg de resina para 150 mg de toxina causou saturação, recuperando apenas 10 a 30% de toxina do sobrenadante. A cromatografia de afinidade com Red A permitiu a recuperação de 60,87% de toxina aplicada em 76 horas, em relação a 114 horas requeridas para purificação utilizando coluna de troca iônica e permeabilidade em gel, com rendimento de 6,5%. O perfil eletroforético das amostras purificadas indicaram que, a toxina obtida da coluna Red A apresentou teor de pureza superior, na ordem de 90%, em relação a 60% atingida pelo método clássico.Culture supernatant of Staphylococcus aureus 722 in 3% triptone plus 1% yeast extract was used for EEA purification, proceeding comparison between dye ligand Red A affinity chromatography and classic chromatography. The capture of SEA with Amberlite CG-50 allowed rapid enterotoxin concentration from the culture supernatant. However, the ratio of 15 mg of the resin to a total of 150 mg of the toxin satured the resin, giving only 10 to 30% of SEA recuperation from the supernatant. The elution of concentrated material throught the Red A column resulted in a recovery of 60,87% of the toxin, and required 76 hours, indicating advantage on classic chromatography. Ion exchange column plus gel filtration recovered only 6,5 % of the SEA, and required 114 hours to conclude the procedure. The eletrophoresis of purified SEA indicated high grade of toxin obtained from Red A column, with 90 % of purity, compared to 60

  2. Determinação de daidzeína, genisteína e gliciteína em cápsulas de isoflavonas por cromatografia em camada delgada (CCD e cromatografia líquida de alta eficiência (CLAE Determination of daidzein, genistein and glycitein in isoflavone capsules by thin layer chromatography (TLC and high performance liquid chromatography (HPLC

    Directory of Open Access Journals (Sweden)

    Isabela da Costa César

    2007-12-01

    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.The use of herbal products and supplements based on isoflavone dry extracts has increased considerably in the last decade, mainly due to beneficial effects to relief of the menopausal symptoms credited to those compounds. Genistein, daidzein and glycitein are the most abundant isoflavone aglycones found in soy extract, where they also occur as glycosides. Concerning their uses, there is neither standardization regarding the minimum content of each aglycone in the extracts or capsules, nor an official method to the quality control of these products. The present work presents a TLC method for qualitative analysis of the three aglycones and their glycosides in extracts and capsules of isoflavones, before and after acid hydrolysis. The quantitative analysis of the

  3. Degenerate polynomial patches of degree 11 for almostGC2 interpolation over triangles

    NARCIS (Netherlands)

    Hogervorst, Bas J.; Damme, van Ruud

    1993-01-01

    We consider the problem of interpolating scattered data in ℝ3 by analmost geometrically smoothGC2 surface, where almostGC2 meansGC2 except in a finite number of points (the vertices), where the surface isGC1. A local method is proposed, based on employing so-called degenerate triangular Bernstein-Bé

  4. 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.

  5. 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%.

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

    Directory of Open Access Journals (Sweden)

    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.

  7. 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.

  8. Determination of Paraffin in Bean Thread Noodles by Employing GC/MS and GC/FID Technology%GC-MS、GC-FID测定粉丝中的石蜡含量

    Institute of Scientific and Technical Information of China (English)

    舒平; 杨卫花; 甘献明

    2010-01-01

    利用GC-MS,GC-FID技术,对粉丝样品中的石蜡检测进行了方法建立及实际样品测试.分析结果表明,该方法对粉丝中百蜡检测的相对标准偏差为2.3%~4.7%,样品的回收率为96%~103%.方法简便、准确、可靠、前处理简单.

  9. GC/MS法测定MDMA毒品成分

    Institute of Scientific and Technical Information of China (English)

    张春水; 刘克林; 何毅; 郑珲; 王朝虹

    2003-01-01

    MDMA是由甲基苯丙胺类毒品衍生而来的一种新型毒品,也属于联合国管制和禁用药品.本文通过对一例MDMA片剂的GC/MS分析,确定了该片剂中的主要毒品成分及辅助成分,建立了一个快速分析检验该类片剂毒品的GC/MS方法.

  10. Assessment of the −174G/C (rs1800795 and −572G/C (rs1800796 Interleukin 6 Gene Polymorphisms in Egyptian Patients with Rheumatoid Arthritis

    Directory of Open Access Journals (Sweden)

    Khalda Amr

    2016-10-01

    CONCLUSION: A significant association of IL-6 −174G/C gene polymorphism and RA in Egyptian population was found with significantly higher frequencies of GC and CC genotypes and C allele in RA patients compared to controls. No association was found between IL-6 −572G/C gene polymorphism and RA.

  11. Comparison of Aroma-Active Volatiles in Oolong Tea Infusions Using GC-Olfactometry, GC-FPD, and GC-MS.

    Science.gov (United States)

    Zhu, JianCai; Chen, Feng; Wang, LingYing; Niu, YunWei; Yu, Dan; Shu, Chang; Chen, HeXing; Wang, HongLin; Xiao, ZuoBing

    2015-09-02

    The aroma profile of oolong tea infusions (Dongdingwulong, DDWL; Tieguanyin, TGY; Dahongpao, DHP) were investigated in this study. Gas chromatography-olfactometry (GC-O) with the method of aroma intensity (AI) was employed to investigate the aroma-active compounds in tea infusions. The results presented forty-three, forty-five, and forty-eight aroma-active compounds in the TGY, DHP, and DDWL infusions, including six, seven, and five sulfur compounds, respectively. In addition, the concentration of volatile compounds in the tea infusions was further quantitated by solid phase microextraction-gas chromatography (SPME)-GC-MS and SPME-GC-flame photometric detection (FPD). Totally, seventy-six and thirteen volatile and sulfur compounds were detected in three types of tea infusions, respectively. Quantitative results showed that forty-seven aroma compounds were at concentrations higher than their corresponding odor thresholds. On the basis of the odor activity values (OAVs), 2-methylpropanal (OAV: 230-455), 3-methylbutanal (1-353), 2-methylbutanal (34-68), nerolidol (108-184), (E)-2-heptenal (148-294), hexanal (134-230), octanal (28-131), β-damascenone (29-59), indole (96-138), 6-methyl-5-hepten-2-one (34-67), (R)-(-)-linalool (63-87), and dimethyl sulfide (7-1320) presented relatively higher OAVs than those of other compounds, indicating the importance of these compounds in the overall aroma of tea infusions.

  12. GC/GC-MS analysis, isolation and identification of bioactive essential oil components from the Bhutanese medicinal plant, Pleurospermum amabile.

    Science.gov (United States)

    Wangchuk, Phurpa; Keller, Paul A; Pyne, Stephen G; Taweechotipatr, Malai; Kamchonwongpaisan, Sumalee

    2013-09-01

    We have hydrodistilled the essential oil (EO) from the aerial parts of the Bhutanese medicinal plant, Pleurospermum amabile using a Clevenger apparatus and evaluated this EO by GC/GC-MS and NMR analysis followed by testing for bioactivity. The GC-MS analysis identified 52 compounds with (E)-isomyristicin as a major component (32.2%). Repeated purification yielded four compounds; (E)-isomyristicin (1), (E)-isoapiol (2), methyl eugenol (3) and (E)-isoelemicin (4). Compound 2 and the mother EO showed the best antiplasmodial activity against the Plasmodium falciparum strains, TM4/8.2 (chloroquine and antifolate sensitive) and K1CB1 (multidrug resistant). They exhibited mild antibacterial activity against Bacillus subtilis. None of the test samples showed cytotoxicity.

  13. Aroma compound analysis of Eruca sativa (Brassicaceae) SPME headspace leaf samples using GC, GC-MS, and olfactometry.

    Science.gov (United States)

    Jirovetz, Leopold; Smith, David; Buchbauer, Gerhard

    2002-07-31

    The aroma compounds of rocket salad (Eruca sativa) SPME headspace samples of fresh leaves were analyzed using GC, GC-MS, and olfactometry. More than 50 constituents of the Eruca headspace could be identified to be essential volatiles, responsible for the characteristic intense green; herbal; nutty and almond-like; Brassicaceae-like (direction of cabbage, broccoli, and mustard); and horseradish-like aroma of these salad leaves. As aroma impact compounds, especially isothiocyanates, and derivatives of butane, hexane, octane, and nonane were identified. 4-Methylthiobutyl isothiocyanate (14.2%), cis-3-hexen-1-ol (11.0%), cis-3-hexenyl butanoate (10.8%), 5-methylthiopentyl isothiocyanate (9.3%), cis-3-hexenyl 2-methylbutanoate (5.4%), and 5-methylthiopentanenitrile (5.0%) were found in concentrations higher than 5.0% (calculated as % peak area of GC analysis using a nonpolar column).

  14. Antibiogram and GC analysis of Euphorbia hirta leaf extract

    OpenAIRE

    2007-01-01

    The antibiogram activity of ethanolic and aqueous extract of E.hirta was studied. Ethanol extract of the plant showed the maximal antibacterial activity and G.C Analysis showed the presence of citronellal. The extract showed inhibited the growth of E.coli, S.aureus, P.aeruginosa, Proteus etc.,

  15. On the interpretation of the CHC factor Gc

    NARCIS (Netherlands)

    K.-J. Kan; R.A. Kievit; C. Dolan; H. van der Maas

    2011-01-01

    On the one hand, the factors Gf and Gc in the Cattell-Horn-Carroll (CHC) model of intelligence are hypothesized to represent individual differences in unique psychological or biological capacities. On the other hand, they are interpreted as representing the theoretical variables fluid and crystalliz

  16. 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.

  17. Odor-active compounds in cooked rice cultivars from Camargue (France) analyzed by GC-O and GC-MS.

    Science.gov (United States)

    Maraval, Isabelle; Mestres, Christian; Pernin, Karine; Ribeyre, Fabienne; Boulanger, Renaud; Guichard, Elisabeth; Gunata, Ziya

    2008-07-09

    Volatile compounds of cooked rice from scented (Aychade, Fidji) and nonscented (Ruille) cultivars grown in the Camargue area in France were compared to that of a marketed Asian scented one (Thai) by gas chromatography-olfactometry (GC-O) and gas chromatography-mass spectrometry (GC-MS). GC-O analyses of the organic extracts resulted in the perception of 40 odorous compounds. Only two compounds, oct-1-en-3-one and 2-acetyl-1-pyrroline, were almost always perceived. Hierarchical cluster analysis showed that most of the difference between rice odors was linked to quantitative differences with only 11 compounds being specific to some of the rice. Sixty compounds were identified and quantified by GC-MS, including a few new odor-active components. Principal component analysis enabled us to differentiate scented cultivars from a nonscented one, and scented rice cultivars from Camargue from a Thai sample. Calculated odor-active values evidenced that the Thai sample odor differed from that of scented Camargue cultivars because of the degradation of lipids and of cinnamic acid compounds.

  18. Método analítico para a determinação de meloxicam em plasma humano por cromatografia líquida de alta eficiência (CLAE Determination of meloxicam in human plasma by HPLC

    Directory of Open Access Journals (Sweden)

    Valentina Porta

    2005-06-01

    Full Text Available Desenvolveu-se e validou-se método analítico simples, rápido e específico para quantificação de meloxicam (inibidor da COX-2 em plasma humano através da cromatografia líquida de alta eficiência, para aplicação em estudos de bioequivalência. Piroxicam foi utilizado como padrão interno. Empregou-se cromatografia em fase reversa com coluna modelo Synergi RP-MAX (150 x 4,6 mm, à temperatura de 30 ºC e fase móvel constituída por mistura de acetonitrila e tampão fosfato 0,025 mol/L pH 4,5 (40:60, v/v, a um fluxo de 1,0 mL/min. Os analitos foram detectados por UV a 364 nm. As amostras de plasma foram acidificadas com ácido clorídrico 1 mol/L, extraídas utilizando-se éter terc-butil metílico e, após filtração e secagem, o resíduo foi reconstituído em 250 mL de fase móvel para injeção em CLAE. Os tempos de retenção para meloxicam (padrão e piroxicam (padrão interno foram 3,35 e 4,19 minutos, respectivamente. Este método apresentou linearidade na faixa de concentração entre 50-4000 ng/mL (R² = 0,9995, com limite de quantificação inferior de 50 ng/mL e exatidão de 114%. O método analítico desenvolvido neste trabalho demonstrou especificidade, linearidade, precisão e exatidão adequadas, permitindo sua aplicação em ensaios de bioequivalência.A simple, rapid and specific high-performance liquid cromatographic (HPLC method was developed and validated to estimate meloxicam (COX-2 inhibitor levels in human plasma. Piroxicam was used as internal standard. Reversed phase chromatography was conducted using a Synergi RP-MAX (150 x 4.6 mm column at 30 ºC and a mobile phase of acetonitrile and 0.025 mol/L pH 4,5 phosphate buffer (40:60, v/v, at a flow rate of 1mL/min. Analytes were detected at 364 nm. Plasma samples were acidified with 1 mol/L hydrochloric acid and extracted with tert-butyl methyl ether, evaporated to dryness, reconstituted in 250 mL of mobile phase and injected in the column. The retention time of

  19. A new type of GC-MS with advanced capabilities

    Science.gov (United States)

    Fialkov, Alexander B.; Steiner, Urs; Jones, Larry; Amirav, Aviv

    2006-03-01

    We have combined the benefits of supersonic molecular beam interface and its related fly-through electron ionization (EI) ion source with the advanced features of the Varian 1200L gas chromatography-mass spectrometry (GC-MS) and mass spectrometry-mass spectrometry (MS-MS), resulting in a new and powerful GC-MS platform with record setting performance. Electron ionization of vibrationally cold molecules in the supersonic molecular beams (SMB) (cold EI) provided mass spectra with enhanced molecular ion, yet with good library search results and superior identification probabilities. We found that high GC column flow rates lower the elution temperature for any given compounds. This allows much larger molecules to elute at the maximum temperature of standard columns. We analyzed a mixture of heavy linear chain hydrocarbons all the way to C84H170 with a molecular weight of 1179.3 amu, using a 4 m 0.25 mm i.d. column and 32 ml/min He flow rate. Furthermore, we obtained a dominant molecular ion to all these compounds. The lower elution temperatures also greatly enhance the ability to analyze very thermally labile compounds such as carbamate pesticides. The experimental 1200 system is capable of triple quadrupole based MS-MS. We found that MS-MS on the molecular ion is much more effective than on fragment ions, and thus, the enhancement of the molecular ion directly improves the MS-MS sensitivity. Fast GC-MS analysis was also explored, based on very high column flow rate for fast splitless injections without affecting the sensitivity, and on the high system selectivity due to the combination of enhanced molecular ion and MS-MS. We demonstrate a few seconds long GC-MS-MS analysis of diazinon, spiked at 10 ng/g in a mixed fruit and vegetable extract. The feature of enhanced molecular ion provides significant enhancement in the detection sensitivity via SIM and RSIM on the molecular ion. While octafluoronaphthalene (OFN) detection limit of below 1 fg in SIM mode is shown, the

  20. Comparison Between Three Chromatographic (GC-ECD, GC-PFPD and GC-ITD-MS) Methods and a UV-Vis Spectrophotometric Method for the Determination of Dithiocarbamates in Lettuce

    OpenAIRE

    Pizzutti,Ionara R.; Kok,André de; Silva,Rosselei C. da; Rohers,Graciele N.

    2017-01-01

    The purpose of this study was to compare the performance of gas chromatographic with electron capture detector, pulsed flame photometric detector and mass spectrometry (GC-ECD, GC-PFPD and GC-MS) and UV-Vis spectrophotometric methods, based on acidic hydrolysis with tin(II) chloride of dithiocarbamate and analysis of the evolved CS2. For the validation studies were assessed linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy and precision. Recovery experiments were pe...

  1. Determinação do 5-hidroximetilfurfural em méis utilizando cromatografia eletrocinética capilar micelar Determination of 5-hydroxymethyl-2-furaldehyde in honey by micellar eletrokinetic capillary electrophoresis

    Directory of Open Access Journals (Sweden)

    Sandra Jussara Nunes da Silva

    2008-12-01

    Full Text Available Neste trabalho foi investigado o índice de HMF (5-hidroximetilfurfural em méis comercializados em Porto Alegre - RS, utilizando Cromatografia Capilar Eletrocinética Micelar. O HMF, produto da condensação da frutose, é um indicador da qualidade e conservação do mel. Foram analisadas 11 marcas de méis comercializados na cidade de Porto Alegre. O composto estudado esteve presente em todas as amostras, em um intervalo de concentração de 0,191 a 6,206 mg.kg-1. Para quantificar o HMF presente nos méis, utilizou-se a técnica de adição de padrão. A taxa de recuperação foi de 98% e o limite de detecção foi de 0,025 mg.kg-1. O limite permitido de HMF em méis, segundo a legislação brasileira, é de 60 mg.kg-1.In this work, the occurrence of HMF (5-hydroxymethylfurfural in honey marketed in Porto Alegre - RS was investigated using Micellar Electrokinetic Capillary Chromatography. The HMF, which is the product of the fructose condensation, is an indicator of honey quality and conservation. Eleven types of honey commercialized in Porto Alegre were analyzed, and all of them contained HMF in a range from 0.191 to 6.206 mg.kg-1. In order to quantify the HMF present in the samples, the technique of standard addition was employed. The recovery was 98% and the detection limit was 0.025 mg.kg-1. The allowed limit of HMF in honey, according to the Brazilian Legislation, is 60 mg.kg-1.

  2. 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.

  3. 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..

    Directory of Open Access Journals (Sweden)

    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

  4. Effects of GC bias in next-generation-sequencing data on de novo genome assembly.

    Science.gov (United States)

    Chen, Yen-Chun; Liu, Tsunglin; Yu, Chun-Hui; Chiang, Tzen-Yuh; Hwang, Chi-Chuan

    2013-01-01

    Next-generation-sequencing (NGS) has revolutionized the field of genome assembly because of its much higher data throughput and much lower cost compared with traditional Sanger sequencing. However, NGS poses new computational challenges to de novo genome assembly. Among the challenges, GC bias in NGS data is known to aggravate genome assembly. However, it is not clear to what extent GC bias affects genome assembly in general. In this work, we conduct a systematic analysis on the effects of GC bias on genome assembly. Our analyses reveal that GC bias only lowers assembly completeness when the degree of GC bias is above a threshold. At a strong GC bias, the assembly fragmentation due to GC bias can be explained by the low coverage of reads in the GC-poor or GC-rich regions of a genome. This effect is observed for all the assemblers under study. Increasing the total amount of NGS data thus rescues the assembly fragmentation because of GC bias. However, the amount of data needed for a full rescue depends on the distribution of GC contents. Both low and high coverage depths due to GC bias lower the accuracy of assembly. These pieces of information provide guidance toward a better de novo genome assembly in the presence of GC bias.

  5. New group of oligosaccharides excreted in honeydew from scale insects Stigmacoccus sp. And coccus hesperidium L. Novo grupo de oligossacarídeos excretado no "honeydew" das cochonilhas Stigmacoccus sp. e coccus hesperidum L.

    Directory of Open Access Journals (Sweden)

    Amauri Bogo

    2003-08-01

    Full Text Available Analysis of the honeydew from scale insects Stigmacoccus sp. and Coccus hesperidium (L. were carried out by paper chromatography, FAB-MS and GC-MS. The results showed three components (tri-, tetra- and penta-saccharides which were composed by 1,4 glucose(s linked to the glucose of sucrose. The findings therefore imply significant and novel metabolic transformations of sugars by the insect and/or microbial symbionts. From these results, structures and common names as "Stigmatriose, Stigmatetraose and Stigmapentose" were proposed for these oligosaccharides because they were found initially in Stigmacoccus sp. honeydew.Análise da secreção doce ou açucarada produzida pelas cochonilhas Stigmacoccus sp. e Coccus hesperidium (L. foi realizada pelas técnicas de cromatografia de papel, bombardeamento de átomo rápido-espectrometria de massas (FAB-MS e cromatografia gasosa-espectrometria de massas (GC-MS. Os resultados mostraram a presença de três oligossacarídeos (tri-, tetra- e pentassacarídeos os quais são compostos por uma ou mais moléculas de 1,4-glucopiranose ligadas à posição 1-glucopiranose do dissacarídeo sacarose. A constatação da presença destes oligossacarídeos na secreção doce ou açucarada das espécies citadas sugere um significante e novo metabolismo de transformação de açucares pelo inseto e/ou por simbiontes microbianos. A partir destes resultados, e por não existirem referências sobre o assunto, sugerem-se as fórmulas estruturais e os nomes comuns de "Estigmatriose, Estigmatetraose e Estigmapentaose" pelo fato de terem sido inicialmente encotrados no honeydew de Stigmacoccus sp.

  6. GC/MS DETERMINATION OF BIOACTIVE COMPONENTS OF PLEUROTUS OSTREATUS

    Directory of Open Access Journals (Sweden)

    V.Priya

    2012-03-01

    Full Text Available In this study, the bioactive components of Pleurotus ostreatus have been evaluated using GC/MS. The chemical compositions of the hydroalcholic extract of Pleurotus ostreatus were investigated using Perkin-Elmer Chromatography–Mass Spectrometry, while the mass spectra of the compounds found in the extract was matched with the National Institute of Standards and Technology (NIST library. GC/MS analysis of hydroalcholic extract of Pleurotus ostreatus revealed the existence of Cholestane-3,7,1,25-tetrol tetraacetate,(3a,5a,7a,12 a-55.20, 9,12-Octadecadienoic acid,methyl ester(E,E-18.55,14,17- Octadecadienoic acid,methyl ester(E,E-5.59,Pentadecanoic acid, ethyl ester-3.84.. The results of this study offer a platform for using Pleurotus ostreatus as herbal alternative for the current synthetic antimicrobial agents.

  7. GC/MS Analysis of the Aromatic Composition of Gasoline

    Science.gov (United States)

    Kostecka, Keith S.; Rabah, Ashraf; Palmer, Charles F., Jr.

    1995-09-01

    The gas chromatography/mass spectrometry (GC/MS) analysis of three brands of regular unleaded gasoline was conducted as part of the independent project of an undergraduate journalism major. In his work, samples of each gasoline were diluted down to part per million (ppm) levels with dichloromethane and then one microliter injections were made onto a Hewlett-Packard GC (5890 Series II unit). Mass spectra were also obtained on each sample through use of a 5971A mass selective detector (MSD). Subsequent characterization was consequently effected through utilization of the standard mass spectra available in a 49,000 compound National Bureau of Standards reference library. Comparison of the obtained and standard spectra revealed that the same aromatic hydrocarbons (including, in part: benzene, the xylenes, naphthalene, and methylated naphthalenes) were present in all three samples. Percentage values for these and other aromatic hydrocarbons were then generated and tabulated.

  8. Analysis of Volatile Compounds in Foie Gras by SDE,GC-MS and GC-O%SDE联合GC-MS与GC-O分析鹅肥肝挥发性风味物质

    Institute of Scientific and Technical Information of China (English)

    谢章斌; 范亚苇; 邓泽元; 刘蓉; 李静; 胡蒋宁; 杜金平

    2011-01-01

    The volatile compounds in foie gras was extracted by simultaneous distillation extraction(SDE) and analyzed by gas chromatography-mass spectrometry(GC-MS) and gas chromatography-olfactometry(GC-O).Totally 41 volatile flavor compounds were identified including 8 hydrocarbons,4 alcohols,2 phenols 7 aldehydes,5 ketones,1 acids,7 ester,7 other compounds and 3 unknown compounds.Among these compounds,hexanal,2-ethylcyclohexanol,nonanal,2-pentadecanone,6,10,14-trimethyl-tetradecanal,di-n-octyl phthalate made a greater contribution to the flavor of foie gras.%采用同时蒸馏萃取法(simultaneous distillation extraction,SDE)提取鹅肥肝的挥发性风味物质,结合气质联用技术(gas chromatography-mass spectrometry,GC-MS)和气相色谱-嗅闻技术(gas chromatography-olfactometry,GC-O)对其挥发性风味物质和主体风味物质进行分析。鉴定出41种风味成分,其中烃类8种、醇类4种、酚类2种、醛类7种、酮类5种、酸类1种、酯类7种、其他7种,3种未鉴定出。同时6种物质对鹅肥肝的风味有较大贡献,分别是己醛、2-乙基环己醇、壬醛、6,10,14-三甲基-2-十五烷酮、十四烷醛和邻苯二甲酸二正辛酯。

  9. Model GC1312S Multifunction Integrated Optical Circuit Devices

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    Model GC1312S multifunction integrated optical circuit device (MIOC) used in inertial-grade interferometric fiber optics gyroscopes (IFOGs) is fabricated by annealing and proton exchange process (APE). The unique feature of the device is the incorporation of the beat detection circuit besides all the features the conventional single Y-branch multifunction integrated optical circuit devices have. The device structure, operation principle and typical characteristics, etc., are briefly presented in this paper.

  10. Comparison of GC-FPD and GC-FID in determining ethanethiol in air of workplace%GC-FPD与GC-FID用于测定工作场所空气中乙硫醇的方法比较

    Institute of Scientific and Technical Information of China (English)

    李颜岩; 史立新

    2013-01-01

    目的 比较工作场所空气中乙硫醇采用FPD(火焰光度检测器)与FID(氢焰离子化检测器)气相色谱测定的方法.方法 空气中以分子或蒸汽态存在的乙硫醇用浸渍玻璃纤维滤纸采集,经洗脱与提取后进样,弱极性色谱柱分离,分别采用FPD、FID进行检测,比较方法学技术指标.结果 FID测定乙硫醇在0.2μg/ml ~ 8.4 μg/ml范围内线性关系良好,r=0.9999,检出限为0.2μg/nnl,与FPD的测定结果基本相当.结论 采用GC-FID测定空气中的乙硫醇的技术参数与用GC-FPD基本等效;GC-FID较为常见,使用与推广更具有实际意义.

  11. Phytochemical studies on Allamanda cathartica L. using GC-MS

    Institute of Scientific and Technical Information of China (English)

    Prabhadevi V; Sahaya Sathish S; Johnson M; Venkatramani B; Janakiraman N

    2012-01-01

    Objective: To explore the phytochemical constituents present in Allamanda cathartica (A. cathartica) L. using GC-MS. Methods: 20 g of the powdered leaf and stem sample of A. cathartica was equilibrated with 200 d/m of A. cathartica ethanol for 24 h, separately. The volume of the supernatant was later reduced by heating to 2 d/m. The concentrated ethanolic extracts were further subjected to GC-MS analysis. Results: The GC-MS analyses determined the presence of 28 different phytochemical compounds in the ethanolic leaf extract of A. cathartica. The major phytoconstituents were 9,12,15-octadecatrienoic acid (Z,Z,Z)- (16.39%), n-hexadecanoic acid (14.08%), 3-O-methyl-d-glucose (11.03%) and 9,12,15-octadecatrienoic acid ethyl ester (Z,Z,Z)-(10.58%). The ethanolic stem extract of A. cathartica showed the presence of 26 different bioactive compounds. The major ones are 3-O-methyl-d-glucose (29.86%), 2-furancarboxaldehyde 5-(hydroxymethyl)- (14.87%), n-hexadecanoic acid (9.13%) and 9,12,15-octadecatrienoic acid (Z,Z,Z)- (7.34%). Conclusions: This study helps to predict the formula and structure of biomolecules which can be used as drugs and further investigation may lead to the development of drug formulation.

  12. Detection of the Spermicide Nonoxynol-9 Via GC-MS

    Science.gov (United States)

    Musah, Rabi A.; Vuong, Angela L.; Henck, Colin; Shepard, Jason R. E.

    2012-05-01

    The spermicide nonoxynol-9 is actually a complex mixture of dozens of closely related amphiphilic compounds, and the chemical properties of this assortment significantly hamper its characterization by GC-MS. The inability to perform routine GC-MS testing on nonoxynol-9 has limited its evidentiary value in forensic casework, which relies heavily on this technique for analysis. A disturbing trend in sexual assault is the use of condoms by assailants, to avoid leaving behind DNA evidence that can connect a perpetrator to a victim. This observation necessitates the development of alternative methods for the analysis of trace evidence that can show causal links between a victim and a suspect. Detection of lubricants associated with sexual assault is one such way to establish this connection. The development of GC-MS methods that permit facile detection of both nonoxynol-9 alone and nonoxynol-9 extracted from other complex matrices that have potential as trace evidence in sexual assault is reported. A detection limit of 2.14 μg of nonoxynol-9 is demonstrated, and a detailed mass spectral profile that elaborates on what is known of its structure is provided.

  13. Potential deleterious role of anti-Neu5Gc antibodies in xenotransplantation.

    Science.gov (United States)

    Salama, Apolline; Evanno, Gwénaëlle; Harb, Jean; Soulillou, Jean-Paul

    2015-01-01

    Human beings do not synthesize the glycolyl form of the sialic acid (Neu5Gc) and only express the acetylated form of the sugar, whereas a diet-based intake of Neu5Gc provokes a natural immunization and production of anti-Neu5Gc antibodies in human serum. However, Neu5Gc is expressed on mammal glycoproteins and glycolipids in most organs and cells. We review here the relevance of Neu5Gc and anti-Neu5Gc antibodies in the context of xenotransplantation and the use of animal-derived molecules and products, as well as the possible consequences of a long-term exposure to anti-Neu5Gc antibodies in recipients of xenografts. In addition, the importance of an accurate estimation of the anti-Neu5Gc response following xenotransplantation and the future contribution of knockout animals mimicking the human situation are also assessed.

  14. Group-specific component (GC) polymorphism in Cádiz (southern Spain).

    Science.gov (United States)

    Vizcaya, M A; Romero, J L; Gamero, J J; Arufe, M I

    1992-01-01

    The genetic polymorphism of group-specific component (GC) was analysed in a sample of 443 healthy unrelated subjects of both sexes resident in the province of Cádiz (Southern Spain). Isoelectric focusing was carried out in polyacrylamide gels followed by staining with coomassie blue R 250. The estimated gene frequencies were as follows: GC*1S = 0.6185; GC*1F = 0.1162; GC*2 = 0.2652.

  15. Comparative Analysis of Volatile Composition in Chinese Truffles via GC × GC/HR-TOF/MS and Electronic Nose

    Directory of Open Access Journals (Sweden)

    Ning Zhang

    2016-04-01

    Full Text Available To compare the volatile compounds of Chinese black truffle and white truffle from Yunnan province, this study presents the application of a direct solvent extraction/solvent-assisted flavor evaporation (DSE-SAFE coupled with a comprehensive two-dimensional gas chromatography (GC × GC high resolution time-of-flight mass spectrometry (HR-TOF/MS and an electronic nose. Both of the analytical methods could distinguish the aroma profile of the two samples. In terms of the overall profile of truffle samples in this research, more kinds of acids were detected via the method of DSE-SAFE. Besides, compounds identified in black truffle (BT, but not in white truffle (WT, or vice versa, and those detected in both samples at different levels were considered to play an important role in differentiating the two samples. According to the analysis of electronic nose, the two samples could be separated, as well.

  16. Identification of the Bacterial Cellular Lipid Fraction by Using Fast GC × GC-MS and Innovative MS Libraries

    Science.gov (United States)

    Mondello, Luigi; Tranchida, Peter Quinto; Purcaro, Giorgia; Fanali, Chiara; Dugo, Paola; La Camera, Erminia; Bisignano, Carlo

    The bacteria fatty acid (FA) profile has been extensively studied for taxonomic classification purposes, since bacteria, in general, contain particular and rare fatty acids, compared to animal and plant tissues. In the last few years, the concern about pathogenic microorganisms used as bioterrorist agents has increased; therefore, rapid methods for the characterization of bacteria are necessary. In the present research, a half-an-hour procedure, to analyze bacteria, was developed: a 2-min one-step sample preparation step, was followed by a relatively fast comprehensive 2D GC-MS separation (25 min). Furthermore, dedicated mass spectrometry libraries were constructed for bacteria and FA identification. Finally, data-processing was carried out with the support of novel comprehensive 2D GC software.

  17. Analysis of essential oils from Scutellaria orientalis ssp. alpina and S. utriculata by GC and GC-MS.

    Science.gov (United States)

    Formisano, Carmen; Rigano, Daniela; Senatore, Felice; Piozzi, Franco; Arnold, Nelly Apostolides

    2011-09-01

    The chemical composition of the essential oils obtained from aerial parts of Scutellaria orientalis L. ssp. alpina (Boiss.) O. Schwarz and S. utriculata Labill. growing wild in Lebanon, were analyzed by GC and GC-MS. In S. orientalis ssp. alpina, strongly characterized by sesquiterpenes (41.2%) and particularly sesquiterpene hydrocarbons (31.7%), hexahydrofarnesylacetone (11.7%) was recognized as the main constituent, together with hexadecanoic acid (7.6%), caryophyllene (7.4%), caryophyllene oxide (6.8%), 4-vinylguaiacol (5.4%) and germacrene D (5.4%). S. utriculata oil was instead constituted above all by monoterpenes (42.2%), particularly oxygen containing monoterpenes (39.9%), and in this oil the main compounds were linalool (20.1%), 4-vinyl guaiacol (15.5%), alpha-terpineol (8.9%), (E)-nerolidol (8.9%) and geraniol (8.2%).

  18. Comparative determination of methyl mercury in whole blood samples using GC-ICP-MS and GC-MS techniques.

    Science.gov (United States)

    Hippler, J; Hoppe, H W; Mosel, F; Rettenmeier, A W; Hirner, A V

    2009-08-15

    Two methods for the determination of methyl mercury (MeHg) in whole blood samples based on different mass spectrometric detection techniques are compared. The methods were employed in two studies in which the internal exposure of a group of mercury-exposed workers to total mercury and MeHg was investigated. Blood samples of these workers were analysed for MeHg independently from each other in two laboratories using similar extraction procedures but different detection techniques, viz. coupled GC-EI-MS/ICP-MS and GC-MS using D(3)-MeHg as internal standard. MeHg was detected in all blood samples in concentrations ranging from 0.3 to 9.0 microg/L. Though different detection techniques were employed, the results obtained by the two laboratories were in relatively good agreement.

  19. [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.

  20. Estudo comparativo dos óleos voláteis de algumas espécies de Piperaceae Comparative study of the essential oils of some species of Piperaceae

    Directory of Open Access Journals (Sweden)

    J.M.O. Mesquita

    2005-03-01

    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.Essential oils from various vegetal species of the Piperaceae family were analysed by Capillary Gas Chromatography (GC and Gas Chromatography/Mass Spectrometry (GC/MS. The investigated species were: Piper aduncum, P. amalago, P. arboreum, P. cernuum, P. hispidum, P. regnelii, P. submarginalum, P. vicosanum and Pothomorphe umbellata. Over 80% of the essential oils compounds were identified by the qualitative and quantitative analysis. The analysed species showed the predominance of sesquiterpenoids, except for P. hispidum, P. submarginalum and P. vicosanum in which the predominant compounds were monoterpenoids. For the 9 studied species, the major compounds found

  1. [Vectorial angle method for studying on GC fingerprint of naphtha in Alpinia officinarum Hance].

    Science.gov (United States)

    Feng, Yi-Fan; Zhou, Xuan; Guo, Xiao-Ling

    2006-01-01

    To establish GC quality analysis and GC fingerprint spectrum of naphtha in Alpinia officinarum Hance. The naphtha in Alpinia officinarum Hance was extracted and analyzed by GC to establish the fingerprint spectrum. The results were analyzed by similarity grade calculate method to compare the fingerprint difference of Alpinia officinarum Hance. The GC fingerprint spectrum of Alpinia officinarum Hance were established. It consisted of 11 peaks. The GC spectrum results were analyzed by similarity grade calculate method which can divide Alpinia officinarum Hance into various habitats. The fingerprint spectrum can be used to distinguish Alpinia officinarum Hance and to evaluate its quality.

  2. 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.

  3. Quantitative relationship between synonymous codon usage bias and GC composition across unicellular genomes

    Directory of Open Access Journals (Sweden)

    Kleinhofs Andris

    2004-06-01

    Full Text Available Abstract Background Codon usage bias has been widely reported to correlate with GC composition. However, the quantitative relationship between codon usage bias and GC composition across species has not been reported. Results Based on an informatics method (SCUO we developed previously using Shannon informational theory and maximum entropy theory, we investigated the quantitative relationship between codon usage bias and GC composition. The regression based on 70 bacterial and 16 archaeal genomes showed that in bacteria, SCUO = -2.06 * GC3 + 2.05*(GC32 + 0.65, r = 0.91, and that in archaea, SCUO = -1.79 * GC3 + 1.85*(GC32 + 0.56, r = 0.89. We developed an analytical model to quantify synonymous codon usage bias by GC compositions based on SCUO. The parameters within this model were inferred by inspecting the relationship between codon usage bias and GC composition across 70 bacterial and 16 archaeal genomes. We further simplified this relationship using only GC3. This simple model was supported by computational simulation. Conclusions The synonymous codon usage bias could be simply expressed as 1+ (p/2log2(p/2 + ((1-p/2log2((l-p/2, where p = GC3. The software we developed for measuring SCUO (codonO is available at http://digbio.missouri.edu/~wanx/cu/codonO.

  4. GC-AMS program at NIES-TERRA

    Energy Technology Data Exchange (ETDEWEB)

    Shibata, Yasuyuki; Yoneda, Minoru; Tanaka, Atsushi; Uehiro, Takashi; Ito, Hiroyasu; Morita, Masatoshi [National Inst. for Environmental Studies, Environmental Chemistry Division, Tsukuba, Ibaraki (Japan); Hirota, Masashi [Environmental Research Center, Tsukuba, Ibaraki (Japan); Uchida, Masao [Japan Marine Science and Technology Center, Yokosuka, Kanagawa (Japan); Yoshinaga, Jun [Tokyo Univ., Tokyo (Japan)

    2002-04-01

    A cosmogenic radioisotope, carbon-14 ({sup 14}C), is a unique tracer for the discrimination of materials/compounds originated from fossil fuels (dead carbon containing no {sup 14}C) from those produced by biomass burning or biological activity (modern carbon with {sup 14}C/{sup 12}C=1.2 x 10{sup -12}). The outline and the present status of the research program, GC-AMS, on the elucidation of both fossil fuel contribution to the environmental pollution and the natural carbon cycling will be presented. (author)

  5. Ochratoxin A detection by spectrofluorimetry compared with high performance liquid c hromatography in coffee/ Espectrofluorimetria comparada à cromatografia líquida de alta eficiência na detecção de ocratoxina A em café

    Directory of Open Access Journals (Sweden)

    Elisa Yoko Hirooka

    2008-08-01

    Full Text Available The Brazilian coffee production plays important role both in the national and oversea trade. The quality and sanity of coffee depend on fungal contamination, with emphasis on ochratoxin A (OTA producing species, which is a nephrotoxin with hazardous effect in public health. The exigency on continuous monitoring and control of OTA in agricultural commodity requires a simple, rapid and accessible analytical methodology. The objective of this research was to set up the spectrofluorimetric method for OTA detection intended for monitoring in coffee, which was developed in data-correlation with high efficiency liquid chromatography (HPLC. The performance of spectrofluorimetric analysis was evaluated using artificially contaminated coffee (10, 20 and 50 ng/g, and the data compared with HPLC. Although of the fault of former technique, with recovery of 40.14 % and correlation coefficient of 0.79 when compared to HPLC, i.e. low reliability and inadequate efficiency, the data showed perspective to follow the improvement inserting new tool, and further standardization and certification.A cafeicultura brasileira apresenta grande importância ao mercado interno e comércio exterior. A qualidade e sanidade do café dependem da contaminação fúngica, com ênfase as espécies produtoras de ocratoxina A (OTA, uma nefrotoxina de efeito deletério à saúde pública. A necessidade de contínuo monitoramento e controle de OTA em produtos agrícolas requer metodologia analítica simples, rápida e acessível. O trabalho teve como objetivo padronizar um método espectrofluorimétrico para detecção de OTA visando monitoramento em grãos de café, correlacionando-o com a cromatografia líquida de alta eficiência (CLAE. A aplicabilidade da espectrofluorimetria foi avaliada em café artificialmente contaminado com OTA (10, 20 e 50 ng/g, comparando os resultados obtidos com a CLAE. Embora a fluorimetria tenha apresentado resultados insatisfatórios, com recupera

  6. Uso da cromatografia de exclusão por tamanho na caracterização de substâncias húmicas de Latossolo Vermelho-Escuro sob efeito da calagem

    Directory of Open Access Journals (Sweden)

    C. A. Silva

    2000-09-01

    Full Text Available Este estudo avaliou o peso molecular estimado (PM e as proporções de frações ácidos húmicos (FAH e frações ácidos fúlvicos (FAF presentes em substâncias húmicas (SH, extraídas com NaOH 0,1 M e resina trocadora de íons, originárias de Latossolo Vermelho-Escuro sob floresta e cultivado com laranja, em áreas com e sem calagem, por meio da cromatografia de exclusão por tamanho de alta eficiência (CETAE. Na calibração do PM com o tempo de retenção de diferentes compostos na coluna cromatográfica, utilizaram-se moléculas de sulfonato de poliestireno de sódio (SPS e acetona. A análise das substâncias húmicas revelou que as FAFs e FAHs dos materiais de solo apresentaram tempo de eluição e, portanto, pesos moleculares muito similares àqueles determinados para os ácidos padrões. Os cromatogramas obtidos mostraram que o uso e o manejo do solo não introduziram mudanças no PM e na relação FAF:FAH das substâncias húmicas. Por outro lado, o método de extração influenciou, de forma marcante, as proporções de FAH e FAF, com mais FAH nos materiais extraídos com a resina trocadora de íons e maiores proporções de FAF nas substâncias húmicas extraídas com NaOH. As proporções de FAF e FAH obtidas por meio do método proposto pela SISH estiveram muito próximas àquelas determinadas com a CETAE, no material húmico extraído com a resina Chelex, demonstrando o potencial desta técnica na determinação do PM e das proporções de FAH e FAF em substâncias húmicas originárias de solos.

  7. Validation of an automated screening method for persistent organic contaminants in fats and oils by GC × GC-ToFMS

    NARCIS (Netherlands)

    Lopez Sanchez, Patricia; Tienstra, Marc; Lommen, Arjen; Mol, Hans G.J.

    2016-01-01

    An screening method, comprised of straightforward sample treatment based on silica clean-up, GC × GC-ToFMS detection and automated data processing with the non-proprietary free downloadable software MetAlignID, has been successfully validated with respect to false negatives for the sum PCB 28, 52

  8. 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...

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

    Directory of Open Access Journals (Sweden)

    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.

  10. Study on the Indicators of Spilled Oil with GC-FID%溢油指示物(或指标)的GC-FID研究

    Institute of Scientific and Technical Information of China (English)

    徐恒振; 周传光; 马永安; 尚龙生; 李洪; 姚子伟; 张国光; 孙育红; 吴之庆

    2001-01-01

    Spilled oil in marine environment were analyzed with GC-FID.The indicators of spilled oil were given out.The results showed that GC-FID is a fast method for study of the indicators of spilled oil.%应用气相色谱氢焰离子化检测器(GC-FID)分析环境溢油,给出了GC-FID鉴别溢油的指示物(或指标)。结果表明,在溢油指示物(或指标)的研究中,气相色谱法(GC-FID)是一种快速有效的方法。

  11. 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. 

  12. Supercritical fluid chromatography-A Hybrid of GC and LC

    Directory of Open Access Journals (Sweden)

    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.

  13. GC-MS study of Nigella sativa (seeds fatty oil

    Directory of Open Access Journals (Sweden)

    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.

  14. GC x GC-ECD: a promising method for the determination of dioxins and dioxin-like PCBs in food and feed

    Energy Technology Data Exchange (ETDEWEB)

    Haglund, Peter; Danielsson, Conny; Wiberg, Karin [Umeaa University, Department of Chemistry, Umeaa (Sweden); Korytar, Peter [Wageningen IMARES - Institute for Marine Resources and Ecosystem Studies, P.O. Box 68, IJmuiden (Netherlands); Diaz, Jordi [Ramon Llull University, Analytical and Environmental Chemistry, Institute Quimic de Sarria, Barcelona (Spain); Leonards, Pim; Boer, Jacob de [Free University, Institute for Environmental Studies (IVM), Amsterdam (Netherlands); Brinkman, Udo A.T. [Free University, Department of Analytical Chemistry and Applied Spectroscopy (ACAS), Amsterdam (Netherlands)

    2008-04-15

    There is a need for cost-efficient alternatives to gas chromatography (GC)-high-resolution mass spectrometry (HRMS) for the analysis of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) and dioxin-like polychlorinated biphenyls (PCBs) in food and feed. Comprehensive two-dimensional GC-micro electron capture detection (GC x GC-{mu}ECD) was tested and all relevant (according to the World Health Organisation, WHO) PCDD/Fs and PCBs could be separated when using a DB-XLB/LC-50 column combination. Validation tests by two laboratories showed that detectability, repeatability, reproducibility and accuracy of GC x GC-{mu}ECD are all statistically consistent with GC-HRMS results. A limit of detection of 0.5 pg WHO PCDD/F tetrachlorodibenzo-p-dioxin equivalency concentration per gram of fish oil was established. The reproducibility was less than 10%, which is below the recommended EU value for reference methods (less than 15%). Injections of vegetable oil extracts spiked with PCBs, polychlorinated naphthalenes and diphenyl ethers at concentrations of 200 ng/g showed no significant impact on the dioxin results, confirming in that way the robustness of the method. The use of GC x GC-{mu}ECD as a routine method for food and feed analysis is therefore recommended. However, the data evaluation of low dioxin concentrations is still laborious owing to the need for manual integration. This makes the overall analysis costs higher than those of GC-HRMS. Further developments of software are needed (and expected) to reduce the data evaluation time. Combination of the current method with pressurised liquid extraction with in-cell cleanup will result in further reduction of analysis costs. (orig.)

  15. Compensatory signals associated with the activation of human GC 5' splice sites.

    Science.gov (United States)

    Kralovicova, Jana; Hwang, Gyulin; Asplund, A Charlotta; Churbanov, Alexander; Smith, C I Edvard; Vorechovsky, Igor

    2011-09-01

    GC 5' splice sites (5'ss) are present in ∼1% of human introns, but factors promoting their efficient selection are poorly understood. Here, we describe a case of X-linked agammaglobulinemia resulting from a GC 5'ss activated by a mutation in BTK intron 3. This GC 5'ss was intrinsically weak, yet it was selected in >90% primary transcripts in the presence of a strong and intact natural GT counterpart. We show that efficient selection of this GC 5'ss required a high density of GAA/CAA-containing splicing enhancers in the exonized segment and was promoted by SR proteins 9G8, Tra2β and SC35. The GC 5'ss was efficiently inhibited by splice-switching oligonucleotides targeting either the GC 5'ss itself or the enhancer. Comprehensive analysis of natural GC-AG introns and previously reported pathogenic GC 5'ss showed that their efficient activation was facilitated by higher densities of splicing enhancers and lower densities of silencers than their GT 5'ss equivalents. Removal of the GC-AG introns was promoted to a minor extent by the splice-site strength of adjacent exons and inhibited by flanking Alu repeats, with the first downstream Alus located on average at a longer distance from the GC 5'ss than other transposable elements. These results provide new insights into the splicing code that governs selection of noncanonical splice sites.

  16. Integration of GC/EI-MS and GC/NCI-MS for simultaneous quantitative determination of opiates, amphetamines, MDMA, ketamine, and metabolites in human hair.

    Science.gov (United States)

    Wu, Ya-Hsueh; Lin, Keh-Liang; Chen, Su-Chin; Chang, Yan-Zin

    2008-07-15

    In this paper, the possibility of using a multiple ionization mode approach of GC/MS was developed for the simultaneous hair testing of common drugs of abuse in Asia, including amphetamines (amphetamine, AP; methamphetamine, MA; methylenedioxy amphetamine, MDA; methylenedioxy methamphetamine, MDMA; methylenedioxy ethylamphetamine, MDEA), ketamine (ketamine, K; norketamine, NK), and opiates (morphine, MOR; codeine, COD; 6-acetylmorphine, 6-AM). This strategy integrated the characteristics of gas chromatography-mass spectrometry (GC-MS) using electron impact ionization (EI) and negative chemical ionization (NCI). Hair samples (25 mg) were washed, cut, and incubated overnight at 25 degrees C in methanol-trifluoroacetic acid (methanol-TFA). The samples were extracted by solid phase extraction (SPE) procedure, derivatized using heptafluorobutyric acid anhydride (HFBA) at 70 degrees C for 30 min, and the derivatives analyzed by GC-MS with EI and NCI. The limit of detection (LOD) with GC/EI-MS analysis obtained were 0.03 ng/mg for AP, MA, MDA, MDMA, and MDEA; 0.05 ng/mg for K, NK, MOR, and COD; and 0.08 ng/mg for 6-AM. The LOD of GC/NCI-MS analysis was much lower than GC/EI-MS analysis. The LOD obtained were 30 pg/mg for AP and MDA in GC/EI-MS and 2 pg/mg in GC/NCI-MS. Therefore, the sensitivity of AP and MDA in GC/NCI-MS was improved from 15-fold compared with EI. The sensitivity of AP, MA, MDA, MDMA, MDEA, MOR, and COD was improved from 15- to 60-fold compared with EI. In addition, the sensitivity of 6-AM increased 8-fold through selection of m/z 197 for the quantitative ion. Moreover, K and NK could dramatically improve their sensitivity at 200- and 2000-fold. The integration of GC/EI-MS and GC/NCI-MS can obtain the high sensitivity and complementary results of drugs of abuse in hair. Six hair samples from known drug abusers were examined by this new strategy. These results show that integrating the characteristics of GC/EI-MS and GC/NCI-MS were not only enhancement of

  17. Determination of aromatic compounds in eluates of pyrolysis solid residues using HS-GC-MS and DLLME-GC-MS.

    Science.gov (United States)

    Bernardo, Maria S; Gonçalves, M; Lapa, N; Barbosa, R; Mendes, B; Pinto, F; Gulyurtlu, Ibrahim

    2009-11-15

    A method for the determination of 15 aromatic hydrocarbons in eluates from solid residues produced during the co-pyrolysis of plastics and pine biomass was developed. In a first step, several sampling techniques (headspace solid phase microextraction (HS-SPME), static headspace sampling (HS), and dispersive liquid-liquid microextraction (DLLME) were compared in order to evaluate their sensitivity towards these analytes. HS-SPME and HS sampling had the better performance, but DLLME was itself as a technique able to extract volatiles with a significant enrichment factor. HS sampling coupled with GC-MS was chosen for method validation for the analytes tested. Calibration curves were constructed for each analyte with correlation coefficients higher than 0.999. The limits of detection were in the range of 0.66-37.85 ng/L. The precision of the HS method was evaluated and good repeatability was achieved with relative standard deviations of 4.8-13.2%. The recoveries of the analytes were evaluated by analysing fortified real eluate samples and were in the range of 60.6-113.9%. The validated method was applied in real eluate samples. Benzene, toluene, ethylbenzene and xylenes (BTEX) were the compounds in higher concentrations. The DLLME technique coupled with GC-MS was used to investigate the presence of less volatile contaminants in eluate samples. This analysis revealed the presence of significant amounts of alkyl phenols and other aromatic compounds with appreciable water solubility.

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

    Directory of Open Access Journals (Sweden)

    Victoria Andrea Arana

    2016-01-01

    Full Text Available 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.

  19. Attempted suicide by ingestion of chlorpyrifos: identification in serum and gastric content by GC-FID/GC-MS.

    Science.gov (United States)

    Martínez, María A; Ballesteros, Salomé; Sánchez de la Torre, Carolina; Sanchiz, Antonio; Almarza, Elena; García-Aguilera, Alejandro

    2004-10-01

    A mild case of self-poisoning with a chlorpyrifos formulation following oral ingestion is reported. A 15-year-old female went to the emergency room after the ingestion of a product from a bottle marked with a label "Poison". On admission, she was obtunded, with normal vital signs and a strong smell of solvent. Therapeutic measures included the application of decontamination procedures, oxygen, and gastric protectors. She had a good outcome with mild CNS depression and bradycardia. Two hours after ingestion, biological samples were collected in the emergency room and sent for analysis to our laboratory with instructions to investigate the presence of solvents. The serum and gastric content contained 5.3 and 9.4 microg/mL of unmetabolized chlorpyrifos, 4.6 and 6.9 microg/mL of toluene, and 2.5 and 7.9 microg/mL of butyl acetate, respectively. Small traces of other solvents and tetradifon were also detected. Toxicological analyses were negative for ethanol, other volatile solvents, and common drugs of abuse. The simultaneous determination of chlorpyrifos, toluene, and butyl acetate was performed using the combination of gas chromatography (GC)-flame ionization detection for screening analysis and GC-mass spectrometry for confirmation of the obtained results. The method provides an excellent and rapid tool for use in cases of pesticide poisonings, allowing the simultaneous detection of the pesticide and distillates in the performance of systematic toxicological analysis in forensic and clinical laboratories.

  20. Chronological study of diazinon in putrefied viscera of rats using GC/MS, GC/EC and TLC.

    Science.gov (United States)

    Elsirafy, A A; Ghanem, A A; Eid, A E; Eldakroory, S A

    2000-03-27

    A qualitative and qualitative weekly study of diazinon in experimental rats after a lethal dose is described. GC/MS and TLC were used for qualitative, and GC/EC for quantitative analysis. The replicate content of diazinon in stomach and intestine (S/I) revealed a high rate of decrease during the first month. The liver (L) content fluctuates through a general trend of decrease. Immediate post-mortem content of 34.5 mg in summer and 94 in winter was found in S/L samples, while it was 0.79 and 0.63 respectively for L-samples. The respective remaining amount after 2 months was 1. 16, 4.40 (S/I), 0.61 and 0.66 mg (L). A round figure of 4% remains in S/L samples. The chronological plots indicate the possibility of detection at longer periods. Interpretation of data is outlined regarding relative contents of organs and the factors affecting persistence of diazinon in putrefied viscera.

  1. Intoxicação em cães e gatos: diagnóstico toxicológico empregando cromatografia em camada delgada e cromatografia líquida de alta pressão com detecção ultravioleta em amostras estomacais Intoxication in dogs and cats: toxicological diagnosis using thin layer chromatography and high pressure liquid chromatography with ultraviolet detection in stomach samples

    Directory of Open Access Journals (Sweden)

    Rachel Picada Bulcão

    2010-05-01

    Full Text Available Agrotóxicos e raticidas são responsáveis por inúmeras intoxicações humanas e animais. Dados preliminares sugerem que o uso ilegal desses compostos com a finalidade de intoxicação fatal em pequenos animais é uma prática comum na região central do Estado do Rio Grande do Sul. O Laboratório de Toxicologia (LATOX recebe amostras de casos em que a principal suspeita é a intoxicação por agrotóxicos ou raticidas (lícitos e ilícitos. O presente estudo teve como objetivo apresentar um levantamento das intoxicações de pequenos animais, analisadas pelo LATOX no período de 2004 a 2008, sendo identificados os xenobióticos por meio de métodos analíticos otimizados pelo laboratório, incluindo screening por cromatografia em camada delgada (CCD e possível confirmação por cromatografia líquida de alta eficiência (CLAE-UV. No período, foram analisadas 68 amostras oriundas de intoxicações em cães e gatos. As amostras biológicas analisadas foram o estômago e o conteúdo estomacal, das quais a CCD permitiu a identificação de carbamatos, warfarina e estricnina. Esta mostrou ser uma técnica qualitativa eficiente e adequada para esse propósito, além de ser relativamente rápida, de baixo custo e de sofrer pouca interferência de componentes da matriz. Também foi realizado um screening toxicológico por CLAE-UV para os carbamatos n-metilados: aldicarb, carbaril, carbofuran e propoxur. O resultado das análises indicou que o principal agente tóxico encontrado foi o aldicarb (chumbinho, responsável por 39,7% das intoxicações (27 casos, seguido por estricnina (seis casos, warfarina (três casos e monofluoracetato de sódio (um caso. Sendo assim, o "chumbinho" foi o principal agente envolvido em intoxicações de cães e gatos na região central do Estado no período avaliado, e os métodos analíticos CCD e CLAE-UV podem ser utilizados de forma eficiente na rotina laboratorial para identificação e confirmação dos xenobi

  2. 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

    Directory of Open Access Journals (Sweden)

    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

  3. 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.

  4. The −174G/C and −572G/C Interleukin 6 Promoter Gene Polymorphisms in Mexican Patients with Rheumatoid Arthritis: A Case-Control Study

    Science.gov (United States)

    Zavaleta-Muñiz, S. A.; Martín-Márquez, B. T.; Gonzalez-Lopez, L.; Gonzalez-Montoya, N. G.; Díaz-Toscano, M. L.; Ponce-Guarneros, J. M.; Ruiz-Padilla, A. J.; Mercado, M. Vázquez-Del; Maldonado-González, M.; Fafutis-Morris, M.; Flores-Martínez, S. E.; Martínez-García, E. A.; Gamez-Nava, J. I.

    2013-01-01

    Objective. There is a lack of information about the genotype frequencies of IL-6 −174G/C and −572G/C polymorphisms in Mexicans with rheumatoid arthritis (RA). Therefore, the aim of this study was to evaluate the association of the IL-6 −174G/C and −572G/C polymorphisms in Mexican mestizo with RA. Methods. We included 137 patients with RA and 102 healthy controls. Patients were assessed for clinical characteristics. IL-6 −174G/C and −572G/C polymorphisms were genotyped using PCR-RFLP analysis. Allele and genotype frequencies and the Hardy-Weinberg equilibrium were computed. Odds ratios (ORs) were computed to identify the risk for RA associated with the presence of GG genotype in comparison with the GC or CC genotypes. Results. The genotype −174GG occurred at a higher frequency in cases and controls (77.4% versus 78.4%, P = 0.845). We found similar results for the genotype −572GG (54% in patients versus 60.8% in controls, P = 0.295). Conclusions. This is the first study to evaluate the association of −174G/C and −572G/C polymorphisms of the IL-6 gene with RA in Mexican mestizo patients. These two polymorphisms were not associated with RA in the studied sample. Additional studies are required to evaluate if these IL-6 polymorphisms have relevance to the development of more severe disease. PMID:24223608

  5. The −174G/C and −572G/C Interleukin 6 Promoter Gene Polymorphisms in Mexican Patients with Rheumatoid Arthritis: A Case-Control Study

    Directory of Open Access Journals (Sweden)

    S. A. Zavaleta-Muñiz

    2013-01-01

    Full Text Available Objective. There is a lack of information about the genotype frequencies of IL-6 −174G/C and −572G/C polymorphisms in Mexicans with rheumatoid arthritis (RA. Therefore, the aim of this study was to evaluate the association of the IL-6 −174G/C and −572G/C polymorphisms in Mexican mestizo with RA. Methods. We included 137 patients with RA and 102 healthy controls. Patients were assessed for clinical characteristics. IL-6 −174G/C and −572G/C polymorphisms were genotyped using PCR-RFLP analysis. Allele and genotype frequencies and the Hardy-Weinberg equilibrium were computed. Odds ratios (ORs were computed to identify the risk for RA associated with the presence of GG genotype in comparison with the GC or CC genotypes. Results. The genotype −174GG occurred at a higher frequency in cases and controls (77.4% versus 78.4%, P=0.845. We found similar results for the genotype −572GG (54% in patients versus 60.8% in controls, P=0.295. Conclusions. This is the first study to evaluate the association of −174G/C and −572G/C polymorphisms of the IL-6 gene with RA in Mexican mestizo patients. These two polymorphisms were not associated with RA in the studied sample. Additional studies are required to evaluate if these IL-6 polymorphisms have relevance to the development of more severe disease.

  6. Digital Holographic Tomography and Fluorescence Used to Localize sGC in HEK293 Cells

    Science.gov (United States)

    Sheldrake, Eric; Mann, Christopher; Gage, Matthew

    2014-03-01

    Digital Holographic Tomography (DHT) is used to analyze and localize the intracellular protein soluble guanylate cyclase (sGC) in human embryonic kidney 293 (HEK293) cells. DHT is a non-invasive phase microscopy technique that provides three dimensional quantitative information of HEK293 cells including variance of index of refraction or physical thickness. A fluorescence component will be added to the microscope to further studies of sGC localization. The signaling pathway including nitric oxide (NO) and sGC is studied and has been linked to various cardiovascular diseases, platelet aggregation, and variations in blood pressure via vasodilation. sGC will be labeled using a fluorescent antibody and analyzed using the DHT microscope. DHT will be used to analyze changes in sGC localization in its natural environment and when stimulated by NO. An understanding of how sGC interacts with its surroundings is vital to further research in cardiovascular disease.

  7. Determination of drugs in hair using GC/MS/MS.

    Science.gov (United States)

    Uhl, M

    1997-01-17

    An important task for the forensic toxicologist and expert witness is the detection of the noxa in biological matrices. Because of this, the identification and quantification of residues of illegal drugs in human hair is still of growing interest. Utilizing the advantages of GC/MS/MS testing human hair is performed for most common drugs of abuse like heroin and other opioides, cocaine, cannabis and amphetamine derivatives. Analyzing hair specimens for substances that present a toxicological risk is another challenge. Several quality control parameters must be observed to avoid false positive or false negative results and to gain additional information. Blank sample, blank hair as well as the combined wash extracts are tested for the presence of the relevant compounds within every series. Careful evaluation of the findings can provide an approximate measure of the intensity of drug use in the majority of cases.

  8. Mechanism of Xylan Pyrolysis by Py-GC/MS

    Institute of Scientific and Technical Information of China (English)

    WANG Shu-rong; LIANG Tao; RU Bin; GUO Xiu-juan

    2013-01-01

    In order to investigate the decomposition behavior of hemicellulose,xylan was chosen as the representative of hemicellulose to study the fast pyrolysis on the combination system of analytical pyrolyzer and gas chromatograph coupled with mass spectrometer(Py-GC/MS).The main condensable products of xylan pyrolysis consisted of acids,aldehydes,and ketones; while gas products contained CO2,CO,CH4 and H2.Acetic acid and furfural were the most abundant products with the highest contents of 20.11% and 20.24% respectively.While furfural and acetic acid were formed competitively with residence time and temperature increases,the distribution of xylan pyrolysis products did not vary with the residence time and temperature,while the total content of several kinds of products changed a lot.According to the analysis of experimental data,a reaction pathway of xylan decomposition was deduced so as to illustrate the formation mechanism of main products.

  9. Improved Lower Bounds for Constant GC-Content DNA Codes

    CERN Document Server

    Chee, Yeow Meng

    2008-01-01

    The design of large libraries of oligonucleotides having constant GC-content and satisfying Hamming distance constraints between oligonucleotides and their Watson-Crick complements is important in reducing hybridization errors in DNA computing, DNA microarray technologies, and molecular bar coding. Various techniques have been studied for the construction of such oligonucleotide libraries, ranging from algorithmic constructions via stochastic local search to theoretical constructions via coding theory. We introduce a new stochastic local search method which yields improvements up to more than one third of the benchmark lower bounds of Gaborit and King (2005) for n-mer oligonucleotide libraries when n <= 14. We also found several optimal libraries by computing maximum cliques on certain graphs.

  10. Characterization of Aroma Active Compounds in Fruit Juice and Peel Oil of Jinchen Sweet Orange Fruit (Citrus sinensis (L.) Osbeck) by GC-MS and GC-O

    OpenAIRE

    Si Yi Pan; Xiao Lin Yao; Gang Fan; Yun Zhang; Yan Zhang; Bi Jun Xie; Yu Qiao

    2008-01-01

    Gas chromatography-mass spectrometry (GC-MS) and gas chromatographyolfactometry (GC-O) were used to determine the aromatic composition and aroma active compounds of fruit juice and peel oil of Jinchen sweet orange fruit. Totals of 49 and 32 compounds were identified in fruit juice and peel oil, respectively. GC-O was performed to study the aromatic profile of Jinchen fruit juice and peel oil. A total of 41 components appeared to contribute to the aroma of fruit juice and peel oil. Twelve comp...

  11. Quantificação de ácido (-) hidroxicítrico em extratos comerciais de Garcinia cambogia por cromatografia líquida de alta eficiência

    OpenAIRE

    Klein Júnior, Luiz C.; Antunes,Marina V.; Linden,Rafael; Vasques, Carlos A. R.

    2010-01-01

    O extrato de Garcinia cambogia (GC), utilizado no tratamento da obesidade, é padronizado por quantificação de ácido hidroxicítrico (AHC) em sua forma salina (CaAHC). Assim, objetivou-se quantificar AHC em duas amostras comerciais de GC (A e B) com 50 % de AHC, de acordo com os laudos de origem. O rendimento extrativo por maceração foi 23,83 % (A) e 22,37 % (B). O teor do analito, quantificado por CLAE-DAD utilizando calibração com padrão de CaAHC, foi 36,09 % (A) e 41,57 % (B) sob...

  12. Efeitos de diferentes volumes correntes e da pressão expiratória final positiva sobre a troca gasosa na fístula broncopleural experimental Effects of different tidal volumes and positive end expiratory pressure on gas exchange in experimental bronchopleural fistula

    Directory of Open Access Journals (Sweden)

    Maria Gabriela Cavicchia Toneloto

    2008-09-01

    Full Text Available OBJETIVO: O presente estudo foi desenhado para identificar o efeito da pressão expiratória final positiva (PEEP e o volume corrente pulmonar ideal para ventilar animais com fístula broncopleural produzida cirurgicamente, com o intuito de reduzir a vazão da fístula sem afetar a troca gasosa. MÉTODOS: Avaliação hemodinâmica e respiratória da troca gasosa foi obtida em cinco porcos jovens, saudáveis, da linhagem Large White, ventilados mecanicamente no modo ventilatório volume controlado com FiO2 de 0.4 e relação inspiração:expiração em torno de 1:2, com freqüência respiratória mantida em 22 cpm. A fístula broncopleural foi produzida pela ressecção da língula. Um sistema de drenagem a selo d'água foi instalado e o tórax foi hermeticamente fechado. A troca gasosa e o débito da fístula broncopleural foram medidos com animais ventilados sequencialmente com volumes correntes de 4 ml/kg, 7 ml/kg e 10 ml/Kg alternando zero de pressão expiratória final positiva (ZEEP e PEEP de 10 cmH2O, sempre na mesma ordem. RESULTADOS: Esses dados são atribuídos à ventilação alveolar reduzida e às anormalidades da ventilação/perfusão que foram atenuadas com volumes correntes mais altos. PEEP aumentou o vazamento de ar pela fístula, mesmo com baixos volumes, de 2.0 ± 2,8mL para 31 ± 20,7mL (p= 0,006 e diminuiu a ventilação alveolar em todos os volumes correntes. A ventilação alveolar melhorou com altos volumes correntes, mas aumentou o débito da fístula (4 ml/kg - 2,0 ± 2,8mL e 10 mL/kg - 80,2 ± 43,9mL; p=0,001. Baixos volumes correntes resultaram em hipercapnia (ZEEP - 83,7± 6,9 mmHg e com PEEP 10 -93 ± 10,1mmHg e diminuição significativa da saturação de oxigênio arterial, em torno de 84%. CONCLUSÃO: O volume corrente de 7 ml/kg com ZEEP foi considerado o melhor volume corrente, visto que, apesar da hipercapnia moderada, a saturação de oxigênio arterial é sustentada em torno de 90%. A ventilação alveolar

  13. CPAP at 10 cm H2O during cardiopulmonary bypass does not improve postoperative gas exchange CPAP de 10 cmH2O durante a circulação extracorpórea não melhora a troca gasosa pós-operatória

    Directory of Open Access Journals (Sweden)

    Luciana Castilho de Figueiredo

    2008-06-01

    Full Text Available OBJECTIVE: To compare postoperative (PO pulmonary gas exchange indexes in patients submitted to myocardial revascularization (MR with or without the application of continuous positive airway pressure (CPAP during cardiopulmonary bypass (CPB. METHODS: Thirty adult patients submitted to MR with CPB between March and September 2005 were randomly allocated to two groups: CPAP (n=15, patients that received CPAP at 10 cmH2O during CPB, and control (n=15, patients that didn't receive CPAP. PaO²/FiO2 and P(A-aO2 were analyzed at four moments: Pre (just before CPB, with FiO2=1.0 ; Post (30min post-CPB, with FiO2=1.0; immediate PO period (12h post-surgery, with FiO2=0.4 by using a Venturi® facial mask and first PO day (24h post-surgery, with FiO2=0.5 by a facial mask. RESULTS: PaO2/FiO2 and P(A-aO2 tend to get significantly worst as time elapsed during the postoperative period in both groups, but no differences were observed between them at any moment. When PaO2/FiO2 was subdivided into three categories, a greater prevalence of patients with values between 200 mmHg and 300mmHg were observed in CPAP group only at moment Post (30min post-CPB; p = 0.02. CONCLUSION: CPAP at 10cmH2O administered during CPB, although had lightly improved PaO2/FiO2 at 30 minutes post-CPB, had no significant sustained effect on postoperative pulmonary gas exchange. We concluded that in patients submitted to MR, application of 10 cmH2O CPAP does not improve postoperative pulmonary gas exchange.OBJETIVO: Comparar os índices de trocas gasosas no pós-operatório de pacientes submetidos a revascularização do miocárdio (RM que receberam ou não pressão positiva contínua nas vias aéreas (CPAP durante a circulação extracorpórea (CEC. MÉTODOS: Trinta pacientes adultos submetidos a RM com CEC no período de março a setembro de 2005 foram alocados aleatoriamente em dois grupos: CPAP (n=15, pacientes que utilizaram CPAP a 10 cmH2O durante a CEC, e controle (n=15, pacientes que

  14. Comparison of volatile and polyphenolic compounds in Brazilian green propolis and its botanical origin Baccharis dracunculifolia Comparação de volatilidade e compostos polifenólicos na própolis verde brasileira e sua origem botânica Baccharis dracunculifolia

    Directory of Open Access Journals (Sweden)

    Mário Roberto Maróstica Junior

    2008-03-01

    Full Text Available Ethanolic extracts and essential oils from Green Propolis from southeastern Brazil and leaf buds from its botanical origin Baccharis dracunculifolia were analyzed by Reversed Phase High Performance Liquid Chromatography (RP-HPLC, Reversed Phase High Performance Thin Layer Chromatography (RP-HPTLC and Gas Chromatography - Mass Spectrometry (GC-MS. The essential oils were obtained by hydro-distillation. Both ethanolic extracts and essential oils showed similar chromatographic profiles. Thirteen flavonoids were identified by RP-HPLC and RP-HPTLC analyses in both samples. Twenty-three volatile compounds were identified by GC-MS analyses. Seventeen were present in both essential oils. The major flavonoid compound in both extracts was artepillin C. The major volatile compound in both essential oils was nerolidol. The major compounds identified in this work could be used as chemical markers in order to classify and identify botanical origins of propolis.Extratos etanólicos e óleos essenciais de própolis verde do sudeste brasileiro e gemas de sua origem botânica (Baccharis dracunculifolia foram analisados por CLAE-FR (Cromatografia Líquida de Alta Eficiência em Fase Reversa, CCDAE (Cromatografia em Camada Delgada de Alta Eficiência e CG-EM (Cromatografia Gasosa acoplada a Espectrometria de Massas. Os óleos essenciais foram obtidos por hidro destilação. Extratos etanólicos e óleos essenciais de Baccharis dracunculifolia e de própolis mostraram perfis cromatográficos similares entre si. Treze flavonóides foram identificados por CLAE-FR e CCDAE em ambas as amostras. Vinte e três compostos voláteis foram identificados por CG EM, sendo dezessete deles presentes em ambos os óleos essenciais. Artepillin C foi o flavonóide encontrado em maiores concentrações em ambas as amostras, enquanto nerolidol foi o volátil majoritário em ambos os óleos essenciais. Os compostos majoritários identificados neste trabalho podem ser utilizados como

  15. Gc types in one Indian group and one Mestizo Mexican group.

    Science.gov (United States)

    Lisker, R; Pérez-Briceño, R; Ramirez, E; Aizpuru, E

    1985-01-01

    The distribution of Gc types was investigated in an Indian group residing in Cuetzalan, Puebla, and in a Mestizo group from Mexico City. Gc1 and Gc2 gene frequencies were 0.862 and 0.138 in Cuetzalan, and 0.858 and 0.142 in Mexico City. These figures are similar to those obtained by other authors in one Northeastern Mexican City. A literature review showed that there appears to be a pattern of high Gc2 frequency in most Brazilian Indians (above 0.3) in contrast to a low frequency (below 0.2) in most other Amerindian groups studied.

  16. Universal and discriminative detection using a miniaturized pulsed discharge detector in comprehensive two-dimensional GC.

    Science.gov (United States)

    Winniford, Bill L; Sun, Kefu; Griffith, James F; Luong, Jim C

    2006-11-01

    A miniaturized pulsed discharge detector (Mini-PDD) has been successfully demonstrated for comprehensive 2-D GC (GC x GC) analysis of pyrolysis gasoline and the pyrolysis GC x GC analysis of a polyethylene copolymer. The detector cell volume of the Mini-PDD is reduced to 25% of the Valco plug-in PDD D-3. An n-C11 peak width at base is 96 ms for the Mini-PDD, about 23% larger than a peak width of 78 ms detected by a flame ionization detector (FID). The Mini-PDD has sufficient response time for most GC x GC applications. When Mini-PDD is operated in helium photoionization mode (Mini He-PDD), it is a universal detector for both inorganic and organic compounds. This is especially useful when detection of water is needed in GC x GC applications. When krypton is doped in the helium discharge gas (Mini Kr-PDD), it can suppress signals of compounds having higher ionization potentials and enhance relative signal intensities of aromatic compounds. The determination of aliphatic to aromatic hydrocarbon ratios is essential to the operation of petroleum crackers. Comparison of the signal from two modes of the Mini-PDD is a simple and fast way to verify the location of aromatics in comprehensive 2-D gas chromatograms.

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

    Science.gov (United States)

    Ming Li, Wei; Li, An; Ming Ha, Yi; Wang, Feng; Li Zhang, Yan

    2011-03-01

    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.

  18. GC/MS检验不同案件中摇头丸%Ananlysis of ecstasy by GC/MS

    Institute of Scientific and Technical Information of China (English)

    苗翠英; 马立坡

    2014-01-01

    目的 分析不同案件缴获的“摇头丸”主要成分和添加物,为确定“摇头丸”的合成路线、非法来源提供依据.方法 以GC/MS检测法为主要检测方法.结果 检验的14个“摇头丸”主要成分为甲基苯丙胺和咖啡因,其中含有少量的其他杂质如麻黄碱和氯胺酮等.结论 检测的14个“摇头丸”样本其中12个含甲基苯丙胺,实为冰毒成分,1个为咖啡因均不属于摇头丸.

  19. Determinação quantitativa de taninos em três espécies de Stryphnodendron por cromatografia líquida de alta eficiência

    Directory of Open Access Journals (Sweden)

    Gisely Cristiny Lopes

    2009-03-01

    Full Text Available Um método de separação e quantificação por cromatografia líquida de alta eficiência (CLAE em fase reversa foi desenvolvido usando água (0,05% de TFA:acetonitrila (0,05% de TFA como fase móvel, em sistema gradiente para a análise dos flavan-3-óis presentes em extrato semipurificado das cascas de Stryphnodendron adstringens, Stryphnodendron polyphyllum e Stryphnodendron obovatum. A CLAE foi realizada com a fração acetato de etila (FAE sendo submetida à extração em fase sólida (cartucho C18-E com metanol:água (2:8, filtrada por membrana de porosidade 0,5 μm; a pré-coluna e coluna empregadas foram Phenomenex® Gemini C-18 (5 μm, com esta última mantida a 30 ºC, com vazão de 0,8 mL/min e detecção a 210 nm. Utilizaram-se soluções dos padrões de ácido gálico e galocatequina para a obtenção da curva analítica. O método proposto foi validado de acordo com a resolução RE n° 899/2003 da ANVISA. A análise quantitativa da FAE das três espécies mostrou que existe similaridade no teor de galocatequina. S. adstringens possui ácido gálico em uma proporção superior a 60% em relação às outras duas espécies. A metodologia desenvolvida mostrou-se viável à aplicação em plantas ricas em taninos, como nos casos de S. adstringens, S. polyphyllum e S. obovatum.A method of separation and quantification by reverse-phase high-performance liquid chromatography (HPLC was developed, using water (0.05% TFA:acetonitrile (0.05% TFA as the mobile phase in a gradient system. Flavan-3-ols present in a semipurified extract from the stem bark of Stryphnodendron adstringens, Stryphnodendron polyphyllum and Stryphnodendron obovatum were analyzed. The HPLC was performed with the ethyl-acetate fraction (EAF using a solid-phase extraction on cartridges C18-E with methanol:water (2:8, filtered through a membrane of 0.5 μm pore size; the column was Phenomenex® Gemini C-18 (5 μm at 30 ºC, with a flow rate of 0.8 mL/min. The analysis was

  20. Teores de carotenóides em mamão e pêssego determinados por cromatografia líquida de alta eficiência Carotenoid levels in papaya and peach determined by high performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Michelle Andriati Sentanin

    2007-03-01

    Full Text Available Os carotenóides são pigmentos naturais, responsáveis pela cor em muitos alimentos como frutas e vegetais, gema de ovo, pele e músculo de alguns peixes. Porém, sua importância também está relacionada a funções ou ações biológicas nos seres humanos, como atividade pró-vitamínica A, fortalecimento do sistema imunológico, diminuição do risco de doenças degenerativas como câncer, doenças cardiovasculares, degeneração macular e catarata. A determinação da composição de carotenóides em alimentos, portanto, é considerada prioritária mundialmente. O objetivo do presente estudo foi analisar quantitativamente, por cromatografia líquida de alta eficiência, os principais carotenóides presentes em três cultivares de mamão (Formosa, Golden e Sunrise e três cultivares de pêssego (Xiripá, Coral e Diamante. Para cada cultivar, foram analisados cinco lotes durante o ano para mamão e durante a safra para pêssego. Os três cultivares de mamão apresentaram composição parecida com as médias dos conteúdos totais de licopeno, beta-criptoxantina e beta-caroteno variando de 18,5 a 23,9, 8,2 a 11,7 e 0,5 a 1,2 µg.g -1, respectivamente. Em relação ao pêssego, os cultivares Coral e Xiripá tiveram níveis muito baixos de carotenóides. O cultivar Diamante teve um teor total médio de 6,4 µg.g -1 de beta-criptoxantina, o carotenóide principal.Carotenoids are natural pigments responsible for the color of many foods such as fruit, vegetables, egg yolk, skin and the flesh of some fish. However, its importance is also related to biological functions or actions in humans, such as the provitamin A activity, enhancement of the immune system, reduction of the risk of degenerative diseases, such as cancer, cardiovascular diseases, macular degeneration and cataract. The determination of the carotenoid composition of foods is therefore considered a priority worldwide. The objective of the present study was to analyze quantitatively, by

  1. Determination of dissolved anions Cl{sup -}, NO{sup 2-}{sub 4}, SO{sup 2-}{sub 4}, Br{sup -}, F{sup -}, PO{sup 3-}{sub 4}, NO{sup -}{sub 2} by ion chromatography; Determinazione di anioni (cloruro, nitrato, solfato, bromuro, fluoruro, fosfato e nitrito) mediante cromatografia ionica

    Energy Technology Data Exchange (ETDEWEB)

    Camusso, M.; Polesello, S. [Consiglio Nazionale delle Ricerche, Rome (Italy). Ist. di Ricerca sulle Acque

    2000-02-01

    A method is described for the determination of the dissolved anions Cl{sup -}, NO{sup 2-}{sub 4}, SO{sup 2-}{sub 4}, Br{sup -}, F{sup -}, PO{sup 3-}{sub 4}, NO{sup -}{sub 2} in fresh waters (surface, ground, mineral, meteoric), effluents and waste waters by ion chromatography. The validation procedure for the method is also reported. [Italian] Viene descritto un metodo per la determinazione di specie anioniche (Cl{sup -}, NO{sup 2-}{sub 4}, SO{sup 2-}{sub 4}, Br{sup -}, F{sup -}, PO{sup 3-}{sub 4}, NO{sup -}{sub 2}) in campioni di acque superficiali, sotterranee e di scarico mediante cromatografia ionica. Nell'articolo vengono anche riportate le procedure del metodo e la relativa validazione.

  2. Characterization and Comparison of Fast Pyrolysis Bio-oils from Pinewood, Rapeseed Cake, and Wheat Straw Using 13C NMR and Comprehensive GC × GC

    Science.gov (United States)

    2016-01-01

    Fast pyrolysis bio-oils are feasible energy carriers and a potential source of chemicals. Detailed characterization of bio-oils is essential to further develop its potential use. In this study, quantitative 13C nuclear magnetic resonance (13C NMR) combined with comprehensive two-dimensional gas chromatography (GC × GC) was used to characterize fast pyrolysis bio-oils originated from pinewood, wheat straw, and rapeseed cake. The combination of both techniques provided new information on the chemical composition of bio-oils for further upgrading. 13C NMR analysis indicated that pinewood-based bio-oil contained mostly methoxy/hydroxyl (≈30%) and carbohydrate (≈27%) carbons; wheat straw bio-oil showed to have high amount of alkyl (≈35%) and aromatic (≈30%) carbons, while rapeseed cake-based bio-oil had great portions of alkyl carbons (≈82%). More than 200 compounds were identified and quantified using GC × GC coupled to a flame ionization detector (FID) and a time of flight mass spectrometer (TOF-MS). Nonaromatics were the most abundant and comprised about 50% of the total mass of compounds identified and quantified via GC × GC. In addition, this analytical approach allowed the quantification of high value-added phenolic compounds, as well as of low molecular weight carboxylic acids and aldehydes, which exacerbate the unstable and corrosive character of the bio-oil. PMID:27668136

  3. The comparison of solid phase microextraction-GC and static headspace-GC for determination of solvent residues in vegetable oils.

    Science.gov (United States)

    Ligor, Magdalena; Buszewski, Bogusław

    2008-02-01

    The objective of these investigations has been the determination of volatile organic compounds including residue solvents present in vegetable oil samples. Some olive oil, rape oil, sunflower oil, soy-bean oil, pumpkin oil, grape oil, rice oil as well as hazel-nut oil samples were analysed. Among residue solvents the following compounds have been mentioned: acetone, n-hexane, benzene, and toluene. Some experiments for the solid phase microextraction (SPME)-GC-flame ionisation detection (FID) were performed to examine extraction conditions such as fiber exposure time, temperature of extraction, and temperature of desorption. Various SPME fibers such as polydimethylsiloxane, Carboxen/polydimethylsiloxane and polydimethylsiloxane/divinylbenzene coatings were used for the isolation of tested compounds from vegetable oil samples. After optimisation of SPME, real vegetable oil samples were examined using SPME-GC/MS. Based on preliminary experiments the qualitative and quantitative analyses for the determination of acetone, n-hexane, benzene and toluene were performed by SPME-GC-FID and static head-space (SHS)-GC-FID methods. The regression coefficients for calibration curves for the examined compounds were R(2) > or = 0.992. This shows that the used method is linear in the examined concentration range (0.005-0.119 mg/kg for SPME-GC-FID and 0.003-0.728 mg/kg for SHS-GC-FID). Chemical properties of analysed vegetable oils have been characterised by chemometric procedure (cluster analysis).

  4. Characterization and Comparison of Fast Pyrolysis Bio-oils from Pinewood, Rapeseed Cake, and Wheat Straw Using (13)C NMR and Comprehensive GC × GC.

    Science.gov (United States)

    Negahdar, Leila; Gonzalez-Quiroga, Arturo; Otyuskaya, Daria; Toraman, Hilal E; Liu, Li; Jastrzebski, Johann T B H; Van Geem, Kevin M; Marin, Guy B; Thybaut, Joris W; Weckhuysen, Bert M

    2016-09-06

    Fast pyrolysis bio-oils are feasible energy carriers and a potential source of chemicals. Detailed characterization of bio-oils is essential to further develop its potential use. In this study, quantitative (13)C nuclear magnetic resonance ((13)C NMR) combined with comprehensive two-dimensional gas chromatography (GC × GC) was used to characterize fast pyrolysis bio-oils originated from pinewood, wheat straw, and rapeseed cake. The combination of both techniques provided new information on the chemical composition of bio-oils for further upgrading. (13)C NMR analysis indicated that pinewood-based bio-oil contained mostly methoxy/hydroxyl (≈30%) and carbohydrate (≈27%) carbons; wheat straw bio-oil showed to have high amount of alkyl (≈35%) and aromatic (≈30%) carbons, while rapeseed cake-based bio-oil had great portions of alkyl carbons (≈82%). More than 200 compounds were identified and quantified using GC × GC coupled to a flame ionization detector (FID) and a time of flight mass spectrometer (TOF-MS). Nonaromatics were the most abundant and comprised about 50% of the total mass of compounds identified and quantified via GC × GC. In addition, this analytical approach allowed the quantification of high value-added phenolic compounds, as well as of low molecular weight carboxylic acids and aldehydes, which exacerbate the unstable and corrosive character of the bio-oil.

  5. Essential oil from two populations of Echinodorus grandiflorus (Cham. & Schltdl. Micheli (Chapéu de couro

    Directory of Open Access Journals (Sweden)

    Daniel S. Pimenta

    2006-12-01

    Full Text Available Analysis by Gas Chromatography and Gas Chromatography/Mass Spectrometry of the essential oils obtained from leaves of Echinodorus grandiflorus ("Chapéu de couro" from two different populations (Big Leaves and Small Leaves, collected monthly between September 1998 and December 1999 revealed 17 components. Phytol was the major constituent for both populations. The main sesquiterpene representatives are (E-caryophyllene, alpha-humulene and (E-nerolidol.Análise por cromatografia com fase gasosa e cromatografia com fase gasosa acoplada à espectrometria de massas de óleos essenciais obtidos de folhas de Echinodorus grandiflorus ("Chapéu-de-couro" em duas diferentes populações (folhas grandes e folhas pequenas, coletadas mensalmente entre setembro de 1998 e dezembro de 1999, revelou 17 componentes. Fitol foi o constituinte majoritário em ambas populações. Os principais representantes sesquiterpênicos foram (E-cariofileno, alfa-humuleno e (E-nerolidol.

  6. Comparison of GC-MS and GC-FID Results for the Determination of C2/C6 Substitution Ratio of Hydroxyethyl Starch 130/0.4%羟乙基淀粉130/0.4的C2/C6置换比例的GC-MS和GC-FID法测定结果比较

    Institute of Scientific and Technical Information of China (English)

    彭茗; 陆丹; 刘瑾; 杨永健

    2013-01-01

    将羟乙基淀粉130/0.4相继用酸水解、六甲基二硅氧烷衍生化后,分别采用GC-MS和GC-FID法测定并比较羟乙基淀粉C2位和C6位的羟乙基置换比例.结果显示,GC-FID法重复性好、进样精密度高,结果可靠;由于存在C2位和C6位衍生物离子化效率的差异,GC-MS法不适合用作该项目的定量方法,但可作为辅助的色谱峰定性工具.%Hydroxyethyl starch 130/0.4 was hydrolyzed by acid and trimethylsilylized by hexamethyl disiloxane successively. The resulting sample solution was utilized to determine C2/C6 substitution ratio by GC-MS and GC-FID method. The results showed that the GC-FID method had high repeatability, precision and reliability. However, the GC-MS method was unsuited for the quantitative analysis of C2/C6 substitution ratio, due to the discrepancy in ionization efficiency of the C2- and C6-derivatives. Nevertheless, it was a supplementary tool for identifying chromatographic peaks.

  7. Molecular Characterization of Growth Hormone-producing Tumors in the GC Rat Model of Acromegaly.

    Science.gov (United States)

    Martín-Rodríguez, Juan F; Muñoz-Bravo, Jose L; Ibañez-Costa, Alejandro; Fernandez-Maza, Laura; Balcerzyk, Marcin; Leal-Campanario, Rocío; Luque, Raúl M; Castaño, Justo P; Venegas-Moreno, Eva; Soto-Moreno, Alfonso; Leal-Cerro, Alfonso; Cano, David A

    2015-11-09

    Acromegaly is a disorder resulting from excessive production of growth hormone (GH) and consequent increase of insulin-like growth factor 1 (IGF-I), most frequently caused by pituitary adenomas. Elevated GH and IGF-I levels results in wide range of somatic, cardiovascular, endocrine, metabolic, and gastrointestinal morbidities. Subcutaneous implantation of the GH-secreting GC cell line in rats leads to the formation of tumors. GC tumor-bearing rats develop characteristics that resemble human acromegaly including gigantism and visceromegaly. However, GC tumors remain poorly characterized at a molecular level. In the present work, we report a detailed histological and molecular characterization of GC tumors using immunohistochemistry, molecular biology and imaging techniques. GC tumors display histopathological and molecular features of human GH-producing tumors, including hormone production, cell architecture, senescence activation and alterations in cell cycle gene expression. Furthermore, GC tumors cells displayed sensitivity to somatostatin analogues, drugs that are currently used in the treatment of human GH-producing adenomas, thus supporting the GC tumor model as a translational tool to evaluate therapeutic agents. The information obtained would help to maximize the usefulness of the GC rat model for research and preclinical studies in GH-secreting tumors.

  8. DETERMINATION OF 16 LARGEST PEAKS IN COMMERCIAL TECHNICAL TOXAPHENE BY GC/MS

    Science.gov (United States)

    Under typical temperature and high vacuum associated with GC/MS technique, Toxaphene decomposes and produces countless fragments which are impractical to quantify. A GC/MS method has been developed using the lowest possible temperature to resolve more peaks and lower the interfer...

  9. GC/FT-IR ANALYSIS OF THE THERMALLY LABILE COMPOUND TRIS (2,3-DIBROMOPROPYL) PHOSPHATE

    Science.gov (United States)

    A fast and convenient GC method has been developed for a compound [tris(2,3-dibromopropyl)phosphate] that poses a difficult analytical problem for both GC (thermal instability/low volatility) and LC (not amenable to commonly available, sensitive detectors) analysis. his method em...

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

    Directory of Open Access Journals (Sweden)

    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.

  11. IDENTIFICATION OF BIS(2-CHLOROETHYL) ETHER HYDROLYSIS PRODUCTS BY DIRECT AQUEOUS INJECTION GC/FT-IR

    Science.gov (United States)

    Gas chromatography coupled to Fourier-transform infrared spectroscopy (GC/FT-IR) is rapidly becoming an accepted analytical technique complementary to GC/mass spectroscopy for identifying organic compounds in mixtures at low to moderate concentrations. irect aqueous injection (DA...

  12. GC/FT-IR ANALYSIS OF THE THERMALLY LABILE COMPOUND TRIS (2,3-DIBROMOPROPYL) PHOSPHATE

    Science.gov (United States)

    A fast and convenient GC method has been developed for a compound [tris(2,3-dibromopropyl)phosphate] that poses a difficult analytical problem for both GC (thermal instability/low volatility) and LC (not amenable to commonly available, sensitive detectors) analysis. his method em...

  13. 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.

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

    Directory of Open Access Journals (Sweden)

    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.

  15. GC/MS analysis of piperidinocyclohexanecarbonitrile (PCC) smoking products

    Energy Technology Data Exchange (ETDEWEB)

    Lue, L.P.; Scimeca, J.A.; Thomas, B.F.; Martin, B.R.

    1986-03-05

    Piperidinocyclohexanecarbonitrile (PCC), an intermediate in phencyclidine (PCP) synthesis, is a major contaminant of illicit PCP. Due to the frequent abuse of PCP by smoking, this study was conducted to determine the PCC pyrolysis products delivered in smoke. Marihuana placebo cigarettes were impregnated with /sup 3/H-piperidino-/sup 14/C-cyano-PCC (synthesized in the lab and recrystallized twice, m.p. 67/sup 0/C) and burned under conditions which simulated smoking. Mainstream smoke was passed through glass wool filters and H/sub 2/SO/sub 4/ and NaOH traps. Tritium and /sup 14/C were recovered as 83%, and 56%, respectively, of the starting material. Seventy-six percent of the recovered tritium was found in the glass wool trap followed by 13, 7 and 4% in the acid trap, base trap and in the ash/unburned butt, respectively. Seventy-three percent of the recovered /sup 14/C was found in the glass wool filter and 16 and 8% were found in the acid and base traps, respectively. GC/MS analysis revealed the presence of 1-piperidinocyclohexene (30%), PCC (24%), piperidine (7%), and 1-acetyl-piperidine (5%).

  16. GC/MS ANALYSIS OF RHEUM RIBES RHIZOMES

    Directory of Open Access Journals (Sweden)

    DR. RAGHAD DH ABDUL JALILL

    2015-03-01

    Full Text Available Objectives: Rheum ribes is a species of perennial and stout herbs that are distributed in southwest of Asia. Crude extracts of their rhizomes have different medicinal activities. Their pharmacological activity may due to their chemical compositions. Methods: This study was carrying out to determine the qualitative and quantitative analysis of chemical components of Rheum ribes rhizomes using two methods by GC-MS. The level of some elements and total protein was also determined. Result: The results of phytochemical screening showed the presence of sugar, flavonoids, glycosides and alkaloids. Nine compounds were identified using methods (1 while there were six different compounds when method (2 was used. Atomic Absorption Spectrometry determined the levels of Cu, Cd, Mn, K, Fe, Co and Ti. Nitrogen was determined by Macro Kjeldahl method. The amounts of them were (2.584, 3.513, 35.03, 0.0388, 126.85, 1, 0.02 and 0.59 percentage respectively. There were not neither phosphors nor Zinc in rhizomes of this plant. The level of total proteins were 3.688 %. Conclusion: The rhizomes R. ribes contain sixteen different components with different levels of more than eight elements.

  17. DETERMINATION OF PHTHALATES FROM BOTTLED WATER BY GC-MS

    Directory of Open Access Journals (Sweden)

    IRINA DUMITRAȘCU

    2012-03-01

    Full Text Available Determination of phthalates from bottled water by GC-MS. Phthalates are ubiquitous pollutants in the environment, due to their widespread use in the last years. These compounds are used principally as plasticizers, to impact flexibility, workability and durability to polymers but they can also be found in products such as paints, adhesives, inks and cosmetics. Phthalates are not chemically bounded to polymers; hence they are easily released and migrate into foods, beverages and drinking water from the packaging or bottling materials or manufacturing processes. This process accelerates as plastic products age and break down. With respect to their endocrine disrupting potential, phthalates such as benzyl butyl phthalate (BBP, di-butyl phthalate (DBP and di-isobutyl phthalate (DIBP have been found to elicit estrogenic responses in in vitro assays. It is possible that phthalates are a contributory factor to endocrine-mediated adverse effects observed in wildlife and humans over the past few decades. In this experiment we have analyzed the phthalates from different bottled waters purchased from the market. Determination by gas chromatography in combination with mass spectrometry detector (GC–MS in electronic ionization mode (EI with selected-ion monitoring (SIM acquisition method (GC–MS (EI–SIM has been carried out. Methods have been developed for both qualitative and quantitative analysis of phthalates. The base peak (m/z = 149 of all the phthalates was selected for the screening studies. The characteristic ions of each compound were chosen for quantitative studies.

  18. GC-ITMS determination and degradation of captan during winemaking.

    Science.gov (United States)

    Angioni, Alberto; Garau, Vincenzo L; Aguilera Del Real, Ana; Melis, Marinella; Minelli, Elizabeth V; Tuberoso, Carlo; Cabras, Paolo

    2003-11-01

    Captan and its metabolite tetrahydrophthalimide (THPI) were determined in grapes, must, and wine by GC-ITMS. Pesticides were extracted with acetone/petroleum ether (50:50 v/v). Because of the high selectivity of the ITMS detector, no interferent was found and cleanup was not necessary. Recoveries from fortified grapes, must, and wines ranged between 90 and 113% with a maximum coefficient of variation of 11%. Limits of quantitation were 0.01 mg/kg for both compounds. In model systems, captan and its metabolites, THPI, cis-4-cyclohexene-1,2-dicarboxylic acid, and 1,2,3,6-tetrahydrophthalamic acid, were determined by HPLC. The degradation of captan during winemaking was studied. Captan degraded in must, giving 100% THPI, and at the end of fermentation, only THPI was found in wine. The degradation of captan to THPI was due to the acidity in must and wine. This metabolite was present at low levels on grapes, and, unlike captan, it had no negative effect on the fermentative process. Model systems showed that the mechanism of disappearance of captan in grapes was due to photodegradation and codistillation.

  19. PBX 9501 Outgas Analysis by SPME/GC/MS

    Energy Technology Data Exchange (ETDEWEB)

    Chambers, D.M.

    2000-12-11

    The authors used equilibrium headspace gas chromatography/mass spectrometry (GC/MS) to monitor volatile and semivolate species that are expected to migrate through PBX 9501 under environmentally relevant conditions. In this work they screened 11 samples taken from deployed parts. Although a number of chemical permeates were identified, the antioxidant signature provided the most information with regard to decomposition aging. Specifically, they were able to monitor butylated hydroxytoluene (BHT) and other antioxidants, which are apparently added to either the Estane adipate or MDI precursor by the manufacturer. They found that in those parts where diphenylamine (DPA) was used as a stabilizer, BHT response was significantly lower than in those formulations stabilized with Irganox 1010 (Irganox). These results imply that DPA is less efficient as a radical scavenger than Irganox. This lower efficiency might be related to the lack of oxygen in the weapon environment, which is initially < 0.1%. With regard to DPA, it has been reported that radical scavenging activity is proportional to the oxygen pressure. At this time they are uncertain whether the low DPA efficiency is mainly attributed to the oxygen level or if there is another rate limiting step that would lead to the preferential consumption of BHT.

  20. Untargeted Metabolomic Analysis of Capsicum spp. by GC-MS.

    Science.gov (United States)

    Aranha, Bianca Camargo; Hoffmann, Jessica Fernanda; Barbieri, Rosa Lia; Rombaldi, Cesar Valmor; Chaves, Fábio Clasen

    2017-09-01

    In order to conserve the biodiversity of Capsicum species and find genotypes with potential to be utilised commercially, Embrapa Clima Temperado maintains an active germplasm collection (AGC) that requires characterisation, enabling genotype selection and support for breeding programmes. The objective of this study was to characterise pepper accessions from the Embrapa Clima Temperado AGC and differentiate species based on their metabolic profile using an untargeted metabolomics approach. Cold (-20°C) methanol extraction residue of freeze-dried fruit samples was partitioned into water/methanol (A) and chloroform (B) fractions. The polar fraction (A) was derivatised and both fractions (A and B) were analysed by gas chromatography coupled to mass spectrometry (GC-MS). Data from each fraction was analysed using a multivariate principal component analysis (PCA) with XCMS software. Amino acids, sugars, organic acids, capsaicinoids, and hydrocarbons were identified. Outlying accessions including P116 (C. chinense), P46, and P76 (C. annuum) were observed in a PCA plot mainly due to their high sucrose and fructose contents. PCA also indicated a separation of P221 (C. annuum) and P200 (C. chinense), because of their high dihydrocapsaicin content. Although the metabolic profiling did not allow for grouping by species, it permitted the simultaneous identification and quantification of several compounds complementing and expanding the metabolic database of the studied Capsicum spp. in the AGC. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

  1. Improvement of ylang-ylang essential oil characterization by GC×GC-TOFMS.

    Science.gov (United States)

    Brokl, Michał; Fauconnier, Marie-Laure; Benini, Céline; Lognay, Georges; du Jardin, Patrick; Focant, Jean-François

    2013-01-30

    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.

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

    Directory of Open Access Journals (Sweden)

    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.

  3. Desenvolvimento de uma fase extratora com polímeros de impressão molecular para extração em fase sólida de Venlafaxina, O-desmetilvenlafaxina e N-desmetilvenlafaxina em amostras de plasmas e análises por cromatografia líquida de ultra eficiência acoplada à espectometria de massas em tandem (UPLC-MS/MS).

    OpenAIRE

    2015-01-01

    A venlafaxina (VEN), em razão de sua eficácia e brandos efeitos adversos, tem sido um dos antidepressivos mais prescritos no tratamento da depressão e ansiedade. Neste trabalho, um método analítico empregando as técnicas MISPE miniaturizada e cromatografia líquida acoplada à espectrometria de massas em Tandem, foi utilizado para a determinação de VEN e seus principais metabólitos em amostras de plasma para fins de monitorização terapêutica. A fase MIP foi sintetizada via polimerização radical...

  4. Thyroid hormone receptor-beta agonist GC-1 inhibits Met-β-catenin driven hepatocellular cancer.

    Science.gov (United States)

    Puliga, Elisabetta; Min, Qian; Tao, Junyan; Zhang, Rong; Pradhan-Sundd, Tirthadipa; Poddar, Minakshi; Singh, Sucha; Columbano, Amedeo; Yu, Jinming; Monga, Satdarshan P

    2017-08-11

    The thyromimetic agent GC-1 induces hepatocyte proliferation via Wnt/β-catenin signaling and may promoting regeneration in both acute and chronic liver insufficiencies. However, β-catenin activation particularly due to mutations in CTNNB1 is seen in a subset of hepatocellular carcinomas (HCC). Thus, it will be critical to address any effect of GC-1 on HCC growth and development, before its use can be advocated to stimulate regeneration in chronic liver diseases. In the current study, we first examine the effect of GC-1 on β-catenin-TCF4 activity in HCC cell lines harboring wild-type or mutated-CTNNB1. Next, we assess the effect of GC-1 on HCC in FVB mice generated by hydrodynamic tail vein injection of hMet-S45Y-β-catenin, using the sleeping beauty transposon-transposase. Four weeks following injection, mice were fed GC-1- (5mg/kg) or basal-diet for 10 or 21 days. GC-1 treatment showed no effect on β-catenin-TCF4 activity in HCC cells, irrespective of CTNNB1 mutations. Treatment with GC-1 for 10 or 21 days led to a significant reduction in tumor burden, associated with decreased tumor cell proliferation, and dramatic decreases in p-Met (Y1234/1235) p-ERK and p-STAT3 without affecting β-catenin and its downstream targets. GC-1 exerts a notable antitumoral effect on hMet-S45Y-β-catenin HCC, by inactivating Met signaling. GC-1 does not promote β-catenin activation in HCC. Thus GC-1 may be safe for use in inducing regeneration during chronic hepatic insufficiency. Copyright © 2017. Published by Elsevier Inc.

  5. Determinação de bifenilos policlorados em milho através de extração em fase sólida seguida de cromatografia a gás acoplada à espectrometria de massas

    Directory of Open Access Journals (Sweden)

    Thiago Guilherme Schwanz

    2012-01-01

    Full Text Available This paper describes an analytical method for analyzing polychlorinated biphenyls in corn samples using solid phase extraction (SPE followed by determination by GC-MS. All calibration curves proved linear (r> 0.99. Recoveries ranged between 74.1 and 110.6% with relative standard deviation lower than 20% for all compounds. The limits of quantitation for the method were between 0.025 and 0.1 ng g-1. Of the 51 samples analyzed, PCB 180 showed the highest frequency, being detected in more than 39%, followed by PCB 138, detected in more than 33% of samples.

  6. Determinação simultânea de topiramato, carbamazepina, fenitoína e fenobarbital em plasma empregando cromatografia a gás com detector de nitrogênio e fósforo

    OpenAIRE

    Roberta Zilles Hahn; Olyr Celestino Kreutz; Marina Venzon Antunes; Rafael Linden; Juliana da Silva; Cléber Álvares da Silva

    2013-01-01

    Topiramate and the other frequently co-administered antiepileptic drugs carbamazepine, phenytoin and phenobarbital were determined in 100 µL plasma samples by gas chromatography with nitrogen phosphorus detection (GC-NPD), after a one-step liquid-liquid extraction with ethyl acetate, followed by flash methylation with trimethylphenylammonium hydroxide. Total chromatographic run time was 12.5 min. Intra-assay and inter-assay precision was 2.5-7.3% and 1.6-5.2%, respectively. Accuracy was 100.1...

  7. 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.

  8. Constituintes químicos voláteis e não-voláteis de Moringa oleifera Lam., Moringaceae Volatile and non-volatile chemical constituents of Moringa oleifera Lam., Moringaceae

    OpenAIRE

    2009-01-01

    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,...

  9. 芝麻素纯化物的GC-MS分析%Analysis on Purified Sesamin by GC-MS

    Institute of Scientific and Technical Information of China (English)

    刘立业

    2011-01-01

    [目的]对芝麻素纯化物进行定性分析,并确定其中杂质成分.[方法]利用气相色谱-质谱联用仪,对芝麻素纯化物进行定性分析.[结果]得到芝麻素纯化物气相色谱及质谱图,从而确定了芝麻素纯化物的主要成分及杂质.[结论]通过GC-MS分析,确定芝麻素纯化物主要成分为芝麻素,此外还含有少量的芝麻酚林及油脂.%[Objective]To qualitatively analyze the purified sesamin and identify the content of its impurities.[Methods] The purified sesamin was qualitatively analyzed by GG-MC.[Result]The gas chromatogram and mass spectrogram of purified sesamin were obtained,and its basic composition and impurities were determined.[Conclusion] By GG-MC,the basic compositions of purified sesamin were identified,which were pure sesamin and few sesamolin and oil.

  10. Identification of Horizontally-transferred Genomic Islands and Genome Segmentation Points by Using the GC Profile Method.

    Science.gov (United States)

    Zhang, Ren; Ou, Hong-Yu; Gao, Feng; Luo, Hao

    2014-04-01

    The nucleotide composition of genomes undergoes dramatic variations among all three kingdoms of life. GC content, an important characteristic for a genome, is related to many important functions, and therefore GC content and its distribution are routinely reported for sequenced genomes. Traditionally, GC content distribution is assessed by computing GC contents in windows that slide along the genome. Disadvantages of this routinely used window-based method include low resolution and low sensitivity. Additionally, different window sizes result in different GC content distribution patterns within the same genome. We proposed a windowless method, the GC profile, for displaying GC content variations across the genome. Compared to the window-based method, the GC profile has the following advantages: 1) higher sensitivity, because of variation-amplifying procedures; 2) higher resolution, because boundaries between domains can be determined at one single base pair; 3) uniqueness, because the GC profile is unique for a given genome and 4) the capacity to show both global and regional GC content distributions. These characteristics are useful in identifying horizontally-transferred genomic islands and homogenous GC-content domains. Here, we review the applications of the GC profile in identifying genomic islands and genome segmentation points, and in serving as a platform to integrate with other algorithms for genome analysis. A web server generating GC profiles and implementing relevant genome segmentation algorithms is available at: www.zcurve.net.

  11. Delineating relative homogeneous G+C domains in DNA sequences.

    Science.gov (United States)

    Li, W

    2001-10-03

    The concept of homogeneity of G+C content is always relative and subjective. This point is emphasized and quantified in this paper using a simple example of one sequence segmented into two subsequences. Whether the sequence is homogeneous or not can be answered by whether the two-subsequence model describes the DNA sequence better than the one-sequence model. There are at least three equivalent ways of looking at the 1-to-2 segmentation: Jensen-Shannon divergence measure, log likelihood ratio test, and model selection using Bayesian information criterion. Once a criterion is chosen, a DNA sequence can be recursively segmented into multiple domains. We use one subjective criterion called segmentation strength based on the Bayesian information criterion. Whether or not a sequence is homogeneous and how many domains it has depend on this criterion. We compare six different genome sequences (yeast S. cerevisiae chromosome III and IV, bacterium M. pneumoniae, human major histocompatibility complex sequence, longest contigs in human chromosome 21 and 22) by recursive segmentations at different strength criteria. Results by recursive segmentation confirm that yeast chromosome IV is more homogeneous than yeast chromosome III, human chromosome 21 is more homogeneous than human chromosome 22, and bacterial genomes may not be homogeneous due to short segments with distinct base compositions. The recursive segmentation also provides a quantitative criterion for identifying isochores in human sequences. Some features of our recursive segmentation, such as the possibility of delineating domain borders accurately, are superior to those of the moving-window approach commonly used in such analyses.

  12. 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

    Directory of Open Access Journals (Sweden)

    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

  13. Aroma active volatiles in four southern highbush blueberry cultivars determined by gas chromatography-olfactometry (GC-O) and gas chromatography-mass spectrometry (GC-MS).

    Science.gov (United States)

    Du, Xiaofen; Rouseff, Russell

    2014-05-21

    Aroma active volatiles in four southern highbush blueberry cultivars ('Prima Dona', 'Jewel', 'Snow Chaser', and 'Kestrel') were determined using solid phase microextraction (SPME) in combination with gas chromatography-olfactometry (GC-O) and identified via GC-PFPD and GC-MS using retention indices of reference compounds and mass spectral data. The aromas of total, unseparated SPME extracts evaluated using GC-O were rated 8.2-9.0/10 for the four cultivars in terms of similarity to the original blueberry homogenates. In terms of GC-O aroma similarity, those aroma active volatile groups characterized as green, fruity, and floral were most intense. Of the 43 volatiles found to have aroma activity, 38 were identified and 13 had not been previously reported in blueberries. Although linalool and (E)-2-hexenal were common major aroma impact volatiles, dominant aroma-active volatiles were different for each cultivar. Principal component analysis confirmed that each cultivar possessed a unique aroma active profile as each cultivar was clustered into a separate score plot quadrant.

  14. GC-2000Ⅱ型气相色谱仪的故障分析与处理%Fault Analysis and Treatment of GC2000II Gas Chromatograph

    Institute of Scientific and Technical Information of China (English)

    李建军

    2015-01-01

    GC-2000Ⅱ gas chromatograph, which is high performance chromatographic instrument controlled by microcomputer, has widely used in coking industry, and can accurately detect the benzene content in rich and poor oil and coke oven gas. This paper introduces the various faults in the use process of GC-2000Ⅱ gas chromatograph, and puts forward some corresponding treatment measures.%GC-2000Ⅱ气相色谱仪是微机控制的高性能色谱仪器, 配置氢焰FID检测器的GC-2000Ⅱ气相色谱仪在焦化行业大量使用,它可以准确地检测出贫富油含苯和煤气含苯. 介绍了GC-2000Ⅱ气相色谱仪在使用过程中出现的各种故障现象,提出了相应的处理措施.

  15. Association between Gc genotype and susceptibility to TB is dependent on vitamin D status.

    Science.gov (United States)

    Martineau, A R; Leandro, A C C S; Anderson, S T; Newton, S M; Wilkinson, K A; Nicol, M P; Pienaar, S M; Skolimowska, K H; Rocha, M A; Rolla, V C; Levin, M; Davidson, R N; Bremner, S A; Griffiths, C J; Eley, B S; Bonecini-Almeida, M G; Wilkinson, R J

    2010-05-01

    Group-specific component (Gc) variants of vitamin D binding protein differ in their affinity for vitamin D metabolites that modulate antimycobacterial immunity. We conducted studies to determine whether Gc genotype associates with susceptibility to tuberculosis (TB). The following subjects were recruited into case-control studies: in the UK, 123 adult TB patients and 140 controls, all of Gujarati Asian ethnic origin; in Brazil, 130 adult TB patients and 78 controls; and in South Africa, 281 children with TB and 182 controls. Gc genotypes were determined and their frequency was compared between cases versus controls. Serum 25-hydroxyvitamin D (25(OH)D) concentrations were obtained retrospectively for 139 Gujarati Asians, and case-control analysis was stratified by vitamin D status. Interferon (IFN)-gamma release assays were also performed on 36 Gujarati Asian TB contacts. The Gc2/2 genotype was strongly associated with susceptibility to active TB in Gujarati Asians, compared with Gc1/1 genotype (OR 2.81, 95% CI 1.19-6.66; p = 0.009). This association was preserved if serum 25(OH)D was or =20 nmol.L(-1) (p = 0.36). Carriage of the Gc2 allele was associated with increased PPD of tuberculin-stimulated IFN-gamma release in Gujarati Asian TB contacts (p = 0.02). No association between Gc genotype and susceptibility to TB was observed in other ethnic groups studied.

  16. Improvement of g-C3N4 photocatalytic properties using the Hummers method.

    Science.gov (United States)

    Feng, Jing; Chen, Tingting; Liu, Shenna; Zhou, Qihang; Ren, Yueming; Lv, Yanzhuo; Fan, Zhuangjun

    2016-10-01

    In this study, graphitic C3N4 (g-C3N4) with high photocatalytic properties to methylene blue (MB) was synthesized by treating the bulk g-C3N4 using the Hummers method. The bulk g-C3N4 was obtained by calcining dicyandiamide. The g-C3N4 treated by the Hummers method (E-g-C3N4) was characterized and utilized for the photocatalytic removal of MB. The results showed that the Hummers treatment exfoliated the nanosheets bulk g-C3N4 into nanorods and improved the dispersion of E-g-C3N4 in an aqueous solution. It also distinctly enhanced the photocatalytic activity of g-C3N4 to MB, i.e., the removal efficiency increased from 38.45% for the bulk g-C3N4 to 96.61% for the E-g-C3N4.

  17. A primer design strategy for PCR amplification of GC-rich DNA sequences.

    Science.gov (United States)

    Li, Li-Yan; Li, Qiang; Yu, Yan-Hong; Zhong, Mei; Yang, Lei; Wu, Qing-Hong; Qiu, Yu-Rong; Luo, Shen-Qiu

    2011-06-01

    To establish a primer design method for amplification of GC-rich DNA sequences. A group of 15 pairs of primers with higher T(m) (>79.7°C) and lower level ΔT(m) (designed to amplify GC-rich sequences (66.0%-84.0%). The statistical analysis of primer parameters and GC content of PCR products was performed and compared with literatures. Other control experiments were conducted using shortened primers for GC-rich PCR amplifications in this study, and the statistical analysis of shortened primer parameters and GC content of PCR products was performed compared with primers not shortened. A group of 26 pairs of primers were designed to test the applicability of this primer designing strategy in amplifications of non-GC-rich sequences (35.2%-53.5%). All the DNA sequences in this study were successfully amplified. Statistical analyses show that the T(m) and ΔT(m) were the main factors influencing amplifications. This primer designing strategy offered a perfect tool for amplification of GC-rich sequences. It proves that the secondary structures cannot be formed at higher annealing temperature conditions (>65°C), and we can overcome this difficulty easily by designing primers and using higher annealing temperature. Crown Copyright © 2011. Published by Elsevier Inc. All rights reserved.

  18. 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

    2014-12-19

    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.

  19. 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.

  20. 壬基酚的GC-MS定量测试及影响因素%Quantitative Analysis of Nonylphenols by GC-MS and its Influences

    Institute of Scientific and Technical Information of China (English)

    马贺伟; 程飞; 张丹云; 黄新霞

    2009-01-01

    分析了壬基酚的气相色谱-质谱(GC-MS)测定过程的影响因素.二氯甲烷作溶剂时,壬基酚的GC-MS响应值较高;以4-n-壬基酚作为内标物,可有效消除重复测量结果之间的偏差;壬基酚质量浓度在0.8-11μg/mL范围内的工作曲线相关系数R2=0.999,定量检测限为0.3 μg/mL.结论:二氯甲烷适合作为壬基酚的GC-MS分析用溶剂,采用内标法是保证壬基酚准确定量的关键.

  1. GC/MS法测定纺织品中全氟辛基磺酰胺%Determination of perfluorooctylsulfonyamide in textiles with GC/MS method

    Institute of Scientific and Technical Information of China (English)

    王建庆; 林丹丽; 王改侠; 李戎; 雷宁

    2010-01-01

    采用气相色谱质谱联用(GC/MS)技术测定纺织品中N-乙基全氟辛基磺酰胺(N-EtPFOSA).结果表明,采用甲醇为提取溶剂、浸渍法加标、超声波萃取、真空旋转蒸发浓缩加氮吹浓缩可以得到理想的回收效果.通过正交试验对GC/MS检测条件进行优化.该方法的检出限为0.0021 μg/mL,样品回收率82%~112%.GC/MS方法操作简便,准确度和精密度符合检测要求.

  2. A “GC-rich” method for mammalian gene expression:A dominant role of non-coding DNA GC content in the regulation of mammalian gene expression

    Institute of Scientific and Technical Information of China (English)

    Gilbert; Rishton; Matthew; (Mizhou); HUI

    2010-01-01

    High mammalian gene expression was obtained for more than twenty different proteins in different cell types by just a few laboratory scale stable gene transfections for each protein.The stable expression vectors were constructed by inserting a naturally-occurring 1.006 kb or a synthetic 0.733 kb DNA fragment(including intron) of extremely GC-rich at the 5’ or/and 3’ flanking regions of these protein genes or their gene promoters.This experiment is the first experimental evidence showing that a non-coding extremely GC-rich DNA fragment is a super "chromatin opening element" and plays an important role in mammalian gene expression.This experiment has further indicated that chromatin-based regulation of mammalian gene expression is at least partially embedded in DNA primary structure,namely DNA GC-content.

  3. Chemical composition of the essential oil from Corsican Mentha aquatica--combined analysis by GC(RI), GC-MS and 13C NMR spectroscopy.

    Science.gov (United States)

    Sutour, Sylvain; Tomi, Félix; Bradesi, Pascale; Casanova, Joseph

    2011-10-01

    The essential oil (EO) of M. aquatica L. growing wild in Corsica was isolated by dry vapor distillation and submitted to combined analysis by column chromatography over silica gel, GC(RI), GC-MS and 13C NMR spectroscopy. The composition was dominated byoxygenated monoterpenes and characterized by the occurrence of menthofuran (50.7%) as the major component. In parallel, seven laboratory-distilled oil samples isolated from individual plants collected in Corsica were analyzed by GC(RI) and 13C NMR spectroscopy. Onlyquantitative differences were observed between the samples. Beside the usual terpenes, various p-menthane lactones (mintlactone, isomintlactone, hydroxymintlactone, menthofurolactone and epimenthofurolactone) have been identified in all the oil samples.

  4. Pyrolysis Synthesized g-C3N4 for Photocatalytic Degradation of Methylene Blue

    Directory of Open Access Journals (Sweden)

    Gang Xin

    2013-01-01

    Full Text Available Graphitic carbon nitride (g-C3N4 was synthesized at 520°C by the pyrolysis of cyanamide, dicyandiamide, and melamine. The samples were characterized by X–ray diffraction (XRD, UV-visible diffuse reflectance spectra, Fourier transform infrared spectroscopy (FT-IR, and elemental analyzer. The photocatalytic activity of g-C3N4 was evaluated by the photodegrading experiments of methylene blue (MB. The results indicated that g-C3N4. A photocatalytic mechanism presumed the MB photodegradation over the C3N4 photocatalyst is attributed to photogenerated electron impelled multistep reduction of O2.

  5. Pyrolysis Synthesized g-C3N4 for Photocatalytic Degradation of Methylene Blue

    OpenAIRE

    2013-01-01

    Graphitic carbon nitride (g-C3N4) was synthesized at 520°C by the pyrolysis of cyanamide, dicyandiamide, and melamine. The samples were characterized by X–ray diffraction (XRD), UV-visible diffuse reflectance spectra, Fourier transform infrared spectroscopy (FT-IR), and elemental analyzer. The photocatalytic activity of g-C3N4 was evaluated by the photodegrading experiments of methylene blue (MB). The results indicated that g-C3N4. A photocatalytic mechanism presumed the MB photodegradation o...

  6. 基于GC-MS对皮革特征气味的分析与模拟%Leather Odors Analysis by GC- MS and Simulation

    Institute of Scientific and Technical Information of China (English)

    胡静; 肖作兵; 邓维钧; 刘万龙; 刘佳颖

    2012-01-01

    采用索氏提取法对不同种类皮革中的挥发性成分进行提取,结合气相色谱一质谱联用技术(GC-MS)分析其挥发性物质的主要组成。根据GC-MS测定结果,通过感官分析模拟具有皮革特征气味的香精。结果表明:未涂饰羊服装革、涂饰羊服装革、涂饰牛服装革和涂饰牛汽车坐垫革的特征气味中,挥发性物质种类繁多,包含烃类、酯类、醛类、酸类、醚类和酮类化合物,以烃类物质为主。根据GC-MS分析结果,结合调香实践经验,调配出香气饱满、逼真、协调的皮革特征气味的香精。%The volatile organic components of different leathers were extracted by Soxhlet extraction and determined with gas chromatography and mass spectrometry ( GC - MS). The leather fragrance was simulated by the sensor analysis based on the GC - MS results. The results show that there are many volatile organic components in the ordour of the unfinished arid finished sheep garment leathers, cow garment leather and cow ear seat leather. These components are hydrocarbons, esters, aldehydes, acids, aethers and ketones, etc. Based on the GC - MS results, the leather fragrance is further prepared.

  7. A GC-FID validated method for the quality control of Eucalyptus globulus raw material and its pharmaceutical products, and gc-ms fingerprinting of 12 Eucalyptus species.

    Science.gov (United States)

    Buenoa, Paula Carolina Pires; Junior, Milton Groppo; Bastos, Jairo Kenupp

    2014-12-01

    In this work we have validated a method to standardize and control the quality of Eucalyptus globulus raw material and phytomedicines containing either the essential oil or the fluid extract of this plant in the final formulation. Internal standardization provided a simple, fast, and reproducible GC-FID analytical method that accurately quantified 1,8-cineol in different E. globulus sub-products, such as its essential oil, dried leaves, fluid extract, and syrup. In addition, GC-MS identification of the main compounds ofE. globulus species afforded fingerprints for the qualitative analysis of different Eucalyptus species.

  8. Rhodobacter capsulatus nifA1 Promoter: High-GC −10 Regions in High-GC Bacteria and the Basis for Their Transcription

    OpenAIRE

    Richard, Cynthia L.; Tandon, Animesh; Kranz, Robert G.

    2004-01-01

    It was previously shown that the Rhodobacter capsulatus NtrC enhancer-binding protein activates the R. capsulatus housekeeping RNA polymerase but not the Escherichia coli RNA polymerase at the nifA1 promoter. We have tested the hypothesis that this activity is due to the high G+C content of the −10 sequence. A comparative analysis of R. capsulatus and other α-proteobacterial promoters with known transcription start sites suggests that the G+C content of the −10 region is higher than that for ...

  9. Technical Note: Fast two-dimensional GC-MS with thermal extraction for anhydro-sugars in fine aerosols

    Science.gov (United States)

    A fast two-dimensional gas chromatography (GC-MS) method that uses heart-cutting and thermal extraction (TE) and requires no chemical derivatization is developed for the determination of anhydro-sugars in fine aerosols. Evaluation of the TE-GC-GC-MS method shows high average rela...

  10. Determinação simultânea de topiramato, carbamazepina, fenitoína e fenobarbital em plasma empregando cromatografia a gás com detector de nitrogênio e fósforo

    Directory of Open Access Journals (Sweden)

    Roberta Zilles Hahn

    2013-01-01

    Full Text Available Topiramate and the other frequently co-administered antiepileptic drugs carbamazepine, phenytoin and phenobarbital were determined in 100 µL plasma samples by gas chromatography with nitrogen phosphorus detection (GC-NPD, after a one-step liquid-liquid extraction with ethyl acetate, followed by flash methylation with trimethylphenylammonium hydroxide. Total chromatographic run time was 12.5 min. Intra-assay and inter-assay precision was 2.5-7.3% and 1.6-5.2%, respectively. Accuracy was 100.1-104.2%. The limit of quantitation was 1 µg mL-1 for all analytes, proving suitable for routine application in therapeutic drug monitoring of antiepileptic drugs.

  11. 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.

  12. Simplification of determination method for standard materials using post-column reaction GC/FID.

    Science.gov (United States)

    Watanabe, Takuro; Kato, Kenji; Matsumoto, Nobuhiro; Maeda, Tsuneaki

    2007-07-31

    For the simple and fast preparation of highly reliable standard materials, a post-column reaction GC/FID system was developed and evaluated on the mixture of oxygen-containing organic compounds. The oxygen-containing organic compounds mixing solution were determined with the post-column reaction GC/FID system using n-dodecane as an internal calibration standard. Required value of relative expanded uncertainty as an original source of SI-traceable standard materials was within 1% and it aimed at this value as accuracy of the quantitative analysis. The results showed good agreement between the prepared concentrations and analytical values using post-column reaction GC/FID system. These results indicated that the post-column reaction GC/FID system would be used for getting SI-traceable values.

  13. [GC-FTIR analysis of structural isomers from hydrogenation products of p-phenylphenol].

    Science.gov (United States)

    Xin, Jun-Na; Xu, Qiang; Zhang, Hua; Yang, Xi-Chuan; Lü, Lian-Hai

    2008-04-01

    The hydrogenation of p-phenylphenol is a consecutive and parallel complex reaction. Owing to the difference in the hydrogenation ability of the two benzene rings in pphenylphenol, the hydrogenation products contained several structural isomers, which can not be identified by normal analytical method. However, the reaction mixture was effectively separated and identified by GC-FTIR technique. According to the characteristic wave numbers of benzene ring substituted at different positions, the main product was confirmed to be p-cyclohexylphenol, and the two typical by-products were p-phenylcyclohexanol and p-cyclohexylcyclohexanol, respectively. Each product has several stereo-isomers. GC-MS, melting point measurement and NMR proved the accuracy of GC-FTIR results, indicating that GC-IR is an useful and rapid method for analyzing structural isomers of organic compounds.

  14. Ecological observations and GC-MS analysis of methanolic extract of Sacoglossan Elysia bangtawaensis (Swennen)

    Digital Repository Service at National Institute of Oceanography (India)

    Shenai-Tirodkar, P.S.; Desai, N.M.; Jagtap, T.G.

    respective peak areas to TIC areas from the GC-MS. Significant variations of ecological parameters were investigated by correlation matrix. Difference were considered statistically significant when p<0.05. RESULTS In postmonsoon (November, 2007-January, 2008...

  15. Fast, high temperature and thermolabile GC--MS in supersonic molecular beams

    Science.gov (United States)

    Dagan, Shai; Amirav, Aviv

    1994-05-01

    This work describes and evaluates the coupling of a fast gas chromatograph (GC) based on a short column and high carrier gas flow rate to a supersonic molecular beam mass spectrometer (MS). A 50 cm long megabore column serves for fast GC separation and connects the injector to the supersonic nozzle source. Sampling is achieved with a conventional syringe based splitless sample injection. The injector contains no septum and is open to the atmosphere. The linear velocity of the carrier gas is controlled by a by-pass (make-up) gas flow introduced after the column and prior to the supersonic nozzle. The supersonic expansion serves as a jet separator and the skimmed supersonic molecular beam (SMB) is highly enriched with the heavier organic molecules. The supersonic molecular beam constituents are ionized either by electron impact (EI) or hyperthermal surface ionization (HSI) and mass analyzed. A 1 s fast GC--MS of four aromatic molecules in methanol is demonstrated and some fundamental aspects of fast GC--MS with time limit constraints are outlined. The flow control (programming) of the speed of analysis is shown and the analysis of thermolabile and relatively non-volatile molecules is demonstrated and discussed. The tail-free, fast GC--MS of several mixtures is shown and peak tailing of caffeine is compared with that of conventional GC--MS. The improvement of the peak shapes with the SMB--MS is analyzed with the respect to the elimination of thermal vacuum chamber background. The extrapolated minimum detected amount was about 400 ag of anthracence-d10, with an elution time which was shorter than 2s. Repetitive injections could be performed within less than 10 s. The fast GC--MS in SMB seems to be ideal for fast target compound analysis even in real world, complex mixtures. The few seconds GC--MS separation and quantification of lead (as tetraethyllead) in gasoline, caffeine in coffee, and codeine in a drug is demonstrated. Controlled HSI selectivity is demonstrated in

  16. In vitro characterization of borneol metabolites by GC-MS upon incubation with rat liver microsomes.

    Science.gov (United States)

    Zhang, Rong; Liu, Chang-hui; Huang, Tian-lai; Wang, Ning-sheng; Mi, Sui-qing

    2008-01-01

    The metabolism of borneol is studied by the analysis of incubations of in vitro-prepared rat liver microsomes. A sensitive gas chromatography (GC)-mass spectrometry (MS) method is developed for the identification of borneol and its metabolites. Four novel metabolites, which have not previously been reported, are isolated and confirmed by comparison of the GC-MS method. The biotransformation pathway of borneol in rat liver microsomes is proposed based on the in vitro results.

  17. Prevalence of Anti-Neu5Gc Antibodies in Patients with Hypothyroidism

    Directory of Open Access Journals (Sweden)

    Phaedra Eleftheriou

    2014-01-01

    Full Text Available Background. N-Glycolylneuraminic acid (Neu5Gc is a sialic acid synthesized by animals, but not by humans or birds. However, it can be incorporated in human cells and can trigger immune response. In the present study, we detected anti-Neu5Gc antibodies in samples of the general population and of patients suffering from hypothyroidism/Hashimoto’s disease, which is known to have autoimmune origin. Methods. Antibodies were measured using enzyme-immunosorbent techniques. Results. Serum anti-Neu5Gc IgG antibodies were higher in patients with hypothyroidism (mean: 14.8±15.9 μg/mL, median: 10.0 μg/mL, P=0.0003, Mann-Whitney and even higher in the group with Hashimoto’s thyroiditis (mean: 31.1±16.3 μg/mL, median: 27.2 μg/mL, P=0.0000, Mann-Whitney compared to the general population (mean: 5.3±4.7  μg/mL, median : 4 μg/mL. All anti-TPO positive samples had anti-Neu5Gc antibody concentration higher than the mean value of the general population while anti-TPO concentration was increased as anti-Neu5Gc concentration increased. Low concentrations of IgA and IgM antibodies were measured in both general population and patient groups. Conclusion. The increased values of anti-Neu5Gc antibodies in patients with hypothyroidism/Hashimoto’s disease and the correlation of anti-TPO incidence with increased anti-Neu5Gc concentration raise the possibility of an association between anti-Neu5Gc antibody development and autoimmune hypothyroidism.

  18. 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.

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

    Directory of Open Access Journals (Sweden)

    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.

  20. Fast Sampling Gas Chromatography (GC) System for Speciation in a Shock Tube

    Science.gov (United States)

    2016-10-31

    addition of an extractive, sampling -based measurement technique allows for the measurement of species not yet measureable by optical methods (e.g...SECURITY CLASSIFICATION OF: We have acquired a gas chromatograph (GC) to investigate post-shock sampling of shock-heated hydrocarbon fuels. The GC...ppm-level measurement) of C2 and C3 hydrocarbons, and detection of aromatics and hydrocarbons C4 and larger. A sampling system has been implemented on

  1. Interleukin-6 c.-174G>C Polymorphism and Periodontitis in a Brazilian Population.

    Science.gov (United States)

    Gabriela Teixeira, Fernanda; Mendonça, Samir Andrade; Menezes Oliveira, Kamilla; Barbosa Dos Santos, Djanilson; Miranda Marques, Lucas; Mendonça Amorim, Maise; de Souza Gestinari, Raquel

    2014-01-01

    Aim. Periodontitis is an inflammatory disease that affects the teeth supporting structures, triggered by periodontal pathogens, and is influenced by environmental and genetic factors. Genes encoding molecules related to the immune response, such as cytokine, are the main candidates for polymorphisms analysis and may be possibly associated with this pathology. A G/C promoter polymorphism on the IL6 gene has been shown to affect basal IL-6 levels. The aim of this study was to investigate the association between the IL6 c.-174G>C polymorphism and periodontitis in individuals from Vitória da Conquista, Bahia, Brazil. Material and Methods. Three hundred and thirty individuals (134 cases, 196 controls) were genotyped for the IL6 c.-174G>C by MS-PCR technique. Concentrations of salivary IL-6 were determined by ELISA method. Results. The IL6 c.-174G>C polymorphism was associated with periodontitis when comparing the distribution of genotypes between patients with periodontitis and control subjects. The GC genotype appeared as a protective factor for periodontitis. Results showed increased levels of salivary IL-6 in periodontitis patients. Nevertheless, there was no relationship between the concentrations of IL-6 and genotypes when comparing the case and control groups. Conclusions. Our data indicate an association between IL6 c.-174G>C polymorphism and periodontitis and showed that IL-6 may be considered an important marker for periodontitis.

  2. 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 .

  3. Interleukin-6 c.-174G>C Polymorphism and Periodontitis in a Brazilian Population

    Directory of Open Access Journals (Sweden)

    Fernanda Gabriela Teixeira

    2014-01-01

    Full Text Available Aim. Periodontitis is an inflammatory disease that affects the teeth supporting structures, triggered by periodontal pathogens, and is influenced by environmental and genetic factors. Genes encoding molecules related to the immune response, such as cytokine, are the main candidates for polymorphisms analysis and may be possibly associated with this pathology. A G/C promoter polymorphism on the IL6 gene has been shown to affect basal IL-6 levels. The aim of this study was to investigate the association between the IL6 c.-174G>C polymorphism and periodontitis in individuals from Vitória da Conquista, Bahia, Brazil. Material and Methods. Three hundred and thirty individuals (134 cases, 196 controls were genotyped for the IL6 c.-174G>C by MS-PCR technique. Concentrations of salivary IL-6 were determined by ELISA method. Results. The IL6 c.-174G>C polymorphism was associated with periodontitis when comparing the distribution of genotypes between patients with periodontitis and control subjects. The GC genotype appeared as a protective factor for periodontitis. Results showed increased levels of salivary IL-6 in periodontitis patients. Nevertheless, there was no relationship between the concentrations of IL-6 and genotypes when comparing the case and control groups. Conclusions. Our data indicate an association between IL6 c.-174G>C polymorphism and periodontitis and showed that IL-6 may be considered an important marker for periodontitis.

  4. The bat genome: GC-biased small chromosomes associated with reduction in genome size.

    Science.gov (United States)

    Kasai, Fumio; O'Brien, Patricia C M; Ferguson-Smith, Malcolm A

    2013-12-01

    Bats are distinct from other mammals in their small genome size as well as their high metabolic rate, possibly related to flight ability. Although the genome sequence has been published in two species, the data lack cytogenetic information. In this study, the size and GC content of each chromosome are measured from the flow karyotype of the mouse-eared bat, Myotis myotis (MMY). The smaller chromosomes are GC-rich compared to the larger chromosomes, and the relative proportions of homologous segments between MMY and human differ among the MMY chromosomes. The MMY genome size calculated from the sum of the chromosome sizes is 2.25 Gb, and the total GC content is 42.3%, compared to human and dog with 41.0 and 41.2%, respectively. The GC-rich small MMY genome is characterised by GC-biased smaller chromosomes resulting from preferential loss of AT-rich sequences. Although the association between GC-rich small chromosomes and small genome size has been reported only in birds so far, we show in this paper, for the first time, that the same phenomenon is observed in at least one group of mammals, implying that this may be a mechanism common to genome evolution in general.

  5. Synthesis and photocatalytic performance of g-C3N4 nanosheets via liquid phase stripping

    Science.gov (United States)

    Miao, Jilin; Xu, Guangqing; Liu, Jiaqin; Lv, Jun; Wu, Yucheng

    2017-02-01

    Well dispersed g-C3N4 nanosheets were prepared by exfoliating the bulk g-C3N4 in concentrated sulfuric acid. Phase structures, morphologies and elemental compositions were characterized by X-ray diffractometer, scanning electron microscope, transmission electron microscope and X-ray photoelectron spectrometer, respectively. Optical absorption and photoluminescence were also used to explain the optical performances of samples. NaI, BQ and IPA were used as the sacrificial agents for studying the surface reactions in the photocatalytic process. By the precipitation of g-C3N4 nanosheets in ethanol with different ratios between concentrated sulfuric acid and ethyl alcohol, well dispersed g-C3N4 nanosheets with high specific surface area can be obtained. The optimized g-C3N4 (1:10) nanosheets achieve the highest photocatalytic activities under UV light illumination, which can degrade 10 mg/L RhB about 98% in 60 min, which is 6 times that of bulk g-C3N4 under UV light.

  6. A bioequivalency study of two trifluoperazine tablet formulations using RIA and GC-MS.

    Science.gov (United States)

    Midha, K K; Hawes, E M; Korchinski, E D; Hubbard, J W; McKay, G; Cooper, J K; Roscoe, R M

    1984-01-01

    Two sensitive analytical procedures, a radioimmunoassay (RIA) and a mass fragmentographic (GC-MS) method, were used to quantitate plasma trifluoperazine concentrations over 24 h in five healthy male volunteers following single 5 mg doses of two trifluoperazine tablet formulations (A and B) in a two-way cross-over design. Bioavailability in terms of area under the plasma concentration versus time curve to 24h or extrapolated to infinity, maximum plasma concentration and time to maximum plasma concentration using either RIA or GC-MS was not statistically significantly different from one formulation to the other. Also, there were no statistically significant differences between GC-MS and RIA values for AUC24(0) and Cmax for each of the two formulations examined. However, the mean AUC24(0) RIA/GC-MS ratios for formulations A and B were 3.1 and 3.4, respectively, while the mean Cmax RIA/GC-MS ratios were 1.7 and 2.1, respectively. These differences in AUC and Cmax are probably mainly due to the relative non-specificity of the RIA antiserum. Thus, where GC-MS is preferred for pharmacokinetic studies, both analytical procedures can be used for comparative single-dose bioequivalence studies of trifluoperazine. However, both the methods should be tested in patients in order to establish the suitability of one procedure over the other for the study of plasma level versus clinical response correlations.

  7. Correlation between Formic Acid Oxidation and Oxide Species on Pt(Bi/GC and Pt/GC Electrode through the Effect of Forward Potential Scan Limit

    Directory of Open Access Journals (Sweden)

    Jelena D. Lović

    2017-01-01

    Full Text Available Following earlier works from our laboratory, further experiments on electrochemical behavior in formic acid oxidation at electrodeposited Pt(Bi/GC and Pt/GC electrode were performed in order to examine the effect of successive increase of the forward potential scan limit. Correlation between formic acid oxidation and oxide species on Pt(Bi/GC electrode with increases of forward potential scan limit is based on the dependency of the backward peak potential from backward peak current. The obtained dependency reveals Bi influence for the scan limits up to 0.8 V. Since the Pt(Bi/GC electrode is composed of Bi core occluded by Pt and Bi-oxide surface layer, the observed behavior is explained through the influence of surface metal oxide on easier formation of OHad species. Nevertheless, the influence of electronic modification of Pt surface atoms by underlying Bi is present and leads to the stronger adsorption of OH on Pt. At higher forward potential scan limits (from 0.8 V, Pt has a dominant role in HCOOH oxidation.

  8. Py-GC/MS, GC/MS and FTIR investigations on Late Roman-Egyptian adhesives from opus sectile: new insights into ancient recipes and technologies.

    Science.gov (United States)

    Ribechini, Erika; Orsini, Sibilla; Silvano, Flora; Colombini, Maria Perla

    2009-04-06

    An analytical protocol based on optical microscopy, Fourier transforms infrared spectroscopy (FTIR), analytical pyrolysis in the presence of hexamethyldisilazane followed by gas chromatographic/mass spectrometric analysis (Py-GC/MS) and gas chromatography/mass spectrometry after alkaline hydrolysis, solvent extraction and trimethylsilylation (GC/MS) was used in the chemical characterisation of the original adhesives used to fix monochrome and mosaic glass and stone plaques coming from the Late Roman archaeological site of Antinoopolis (Egypt). FTIR analysis demonstrated the presence of calcite fragments, and Py-GC/MS and GC/MS analyses provided detailed molecular compositions, highlighting the presence of a wide range of compound classes including diterpenoid acids, tricyclic abietanes with a high degree of aromatisation, mid- and long-chain monocarboxylic fatty acids, mono- and di-hydroxy acids, alpha,omega-dicaboxylic fatty acids, n-alkanols, and n-alkanes. Characteristic biomarkers and their distribution patterns indicated the presence of pine pitch in all the adhesives, which in some cases was admixed with beeswax and brassicaceae seed oil. The results provided new insights into the complex recipes used by artisans in ancient Egypt in the production of adhesives and in the sophisticated manufacture of opus sectile decorations.

  9. 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

    Directory of Open Access Journals (Sweden)

    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

  10. Desenvolvimento e validação de método analítico para quantificação de diclofenaco de dietilamônio em pele humana por cromatografia líquida de alta eficiência

    Directory of Open Access Journals (Sweden)

    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.

  11. Molecular structure of kerogens from source rocks of the Tarim Basin: A study by Py-GC-MS and methylation-Py-GC-MS

    Institute of Scientific and Technical Information of China (English)

    JIA; Wanglu; PENG; Ping'an

    2005-01-01

    Flash pyrolysis-gas chromatography-mass spectrometry (Py-GC-MS) and in situ methylation-pyrolysis-gas chromatography-mass spectrometry (methylation-Py-GC-MS) have been employed for a study of molecular structure of kerogens from source rocks of the Tarim Basin. The main products from Py-GC-MS of the Ordovician and Triassic kerogens from the Tarim Basin are n-alkanes and n-alk-1-enes which decrease in relative abundance with increased carbon number. The major products from methylation-Py-GC-MS are normal saturated fatty acid methyl esters which show maxima at C16 and C18. These aliphatic compounds are mainly from lipids of planktonic algae. Moreover, there are more abundant long-chain fatty acids (C20-C26) and normal n-alkanes and n-alk-1-enes (C15-C25) in pyrolysates of Triassic kerogens than that of Ordovician kerogens, reflecting the discrepancies in sources of the Triassic kerogens and the Ordovician kerogens. Besides these aliphatic compounds, methoxyl benzoic acid methyl esters were detected only in products from methylation-Py-GC-MS of late Ordovician kerogen TAC1-1, which possibly was the first molecular evidence for the appearance of moss or other terrestrial plants in the Tarim Basin. In addition, the relative intensity of 17β(H)-trisnorhopane17 β(H),21 α(H)-30-normoretane and 17 β(H)-moretane is lower, but 17α(H)-trisnorhopane and17 α(H)-30-norhopane is higher in the pyrolysates of the Ordovician kerogens in comparison with the pyrolysates of the Triassic kerogens. Moreover, Pr-1-ene has been detected in pyrolysates of Triassic kerogens. These differences in pyrolysates consist with maturity of kerogens. In conclusion, combination of methylation-Py-GC-MS and Py-GC-MS are useful tools to investigate the molecular structure of geomacromolecules and can be subject to type the organic matter, compare the maturity of kerogens and carry out the oil-source correlation.

  12. 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

  13. Isomerization of octadecapentaenoic acid (18:5n-3) in algal lipid samples under derivatization for GC and GC-MS analysis.

    Science.gov (United States)

    Svetashev, Vasily I; Imbs, Andrey B

    2014-04-01

    During gas chromatography (GC) analysis of fatty acid (FA) composition of the dinoflagellate Gymnodinium kowalevskii, we found unex-pectedly low and irreproducible content of all-cis-3,6,9,12,15-octadecapentaenoic acid (18:5n-3), which is an important chemotaxonomic marker of several classes of microalgae. We compared chromatographic behavior of 18:5n-3 methyl ester and other GC derivatives obtained using different conventional methods of derivatization. The use of methods based on saponification or base-catalyzed transesterification resulted in a mixture of double-bond positional isomers of 18:5. On a SUPELCOWAX 10 column, the equivalent chain length (ECL) value for authentic 18:5n-3 methyl ester was 20.22, whereas the main component after base-catalyzed methylation had ECL 20.88. Attempts to prepare N-acyl pyrrolidides or 4,4-dimethyloxazoline (DMOX) derivatives of 18:5n-3 also gave inadequate results. These derivatives also showed a main peak corresponding to isomerized 18:5. Mass spectra for both DMOX and pyrrolidide derivatives of this compound showed the base peak at m/z 139, probably corresponding to 2,6,9,12,15-18:5 acid. Of all methods tested for methylation, only derivatization with 5% HCl or 1% sulphuric acid in methanol gave satisfactory results. Therefore, GC or GC-mass spectrometry analyses of algal lipids containing 18:5n-3 may be inaccurate when base-catalyzed methods of FA derivatization are applied. The best and simplest way to avoid incorrect GC results is to use standard acid-catalyzed methylation.

  14. Uncertainty Evaluation of Determination of Chloral in Water with GC/MS%GC/MS测定水中三氯乙醛的不确定度评定

    Institute of Scientific and Technical Information of China (English)

    杭培红; 徐巍

    2012-01-01

    系统介绍了吹扫捕集气相色谱/质谱法测定水中三氯乙醛不确定度评定过程,对吹扫捕集气相色谱/质谱法测定水中三氯乙醛的测定过程进行分析,通过数学模型分析并计算测试过程中的不确定度分量,最后计算出相对合成标准不确定度和相对扩展不确定度。结果表明,吹扫捕集气相色谱/质谱法测定水中三氯乙醛的不确定度主要有四个来源:标准样品浓度及稀释过程,标准曲线及回归偏差,样品取样量,仪器稳定性。%The uncertainty of determining chloral in water was evaluated by purge and trap-gas chromatography-mass spectrometry(purge trap-GC-MS).The determination process of chloral in water was analyzed by purge trap-GC-MS.The uncertainty factors in analyzing process were determined and calculated by mathematic model,and the relative synthesis standard uncertainty and the relative expansion standard uncertainty were calculated out.The four main sources were the uncertainty of standard samples and by dilution process,the uncertainty of linear and regression variance,the uncertainty brought in the sampling process,and the uncertainty resulted from the instrument stability of purge trap-GC-MS.Four main sources of the uncertainty of determining chloral in water by purge trap-GC-MS was determined.The uncertainty evaluation process of determining chloral in water by purge trap-GC-MS was introduced systematically.

  15. Identification of unknown impurity of azelaic acid in liposomal formulation assessed by HPLC-ELSD, GC-FID, and GC-MS.

    Science.gov (United States)

    Han, Stanisław; Karłowicz-Bodalska, Katarzyna; Potaczek, Piotr; Wójcik, Adam; Ozimek, Lukasz; Szura, Dorota; Musiał, Witold

    2014-02-01

    The identification of new contaminants is critical in the development of new medicinal products. Many impurities, such as pentanedioic acid, hexanedioic acid, heptanedioic acid, octanedioic acid, decanedioic acid, undecanedioic acid, dodecanedioic acid, tridecanedioic acid, and tetradecanedioic acid, have been identified in samples of azelaic acid. The aim of this study was to identify impurities observed during the stability tests of a new liposomal dosage form of azelaic acid that is composed of phosphatidylcholine and a mixture of ethyl alcohol and water, using high-performance liquid chromatography with evaporative light-scattering detector (HPLC-ELSD), gas chromatography-flame ionisation detection (GC-FID), and gas chromatography-mass spectrometry (GC-MS) methods. During the research and development of a new liposomal formulation of azelaic acid, we developed a method for determining the contamination of azelaic acid using HPLC-ELSD. During our analytical tests, we identified a previously unknown impurity of a liposomal preparation of azelaic acid that appeared in the liposomal formulation of azelaic acid during preliminary stability studies. The procedure led to the conclusion that the impurity was caused by the reaction of azelaic acid with one of the excipients that was applied in the product. The impurity was finally identified as an ethyl monoester of azelaic acid. The identification procedure of this compound was carried out in a series of experiments comparing the chromatograms that were obtained via the following chromatographic methods: HPLC-ELSD, GC-FID, and GC-MS. The final identification of the compound was carried out by GC with MS.

  16. An experimental study to compare inflammatory response due to liquid or gas joint distension in horses submitted to arthroscopy Estudo experimental para comparar a resposta inflamatória decorrente da distensão líquida ou gasosa em cavalos submetidos à artroscopia

    Directory of Open Access Journals (Sweden)

    Renata Bello Rossetti

    2012-12-01

    Full Text Available PURPOSE: To assess comparatively the inflammatory response that follows CO2 or Ringer's lactate joint capsular distension of horses submitted to experimental arthroscopy METHODS: Each animal was submitted to a bilateral tarsocrural arthroscopy employing gas distention in one joint and fluid distention in the contralateral joint. Synovial fluid was evaluated at 0, six, 12, 24 and 48 hours post-operative. RESULTS: The use of CO2 for arthroscopy causes an acute and mild synovitis alike to the liquid capsular distension, showing similar synovial fluid increase of leukocytes, TP, and TNF-α. Although synovial fluid PGE2 content was higher in joints submitted to CO2 distension, lower levels of hemoglobin and leukocytes oxidative burst after surgery indicates that CO2 arthroscopy decreased intra-articular bleeding and activation of infiltrating leukocytes. CONCLUSIONS: The use of CO2 for arthroscopic examination causes acute and mild synovitis that is similar to the effects caused by the liquid capsular distension. CO2 also seems to decrease intra-articular bleeding and activation of leukocytes.OBJETIVO: Avaliar comparativamente a resposta inflamatória decorrente da distensão líquida ou gasosa em cavalos submetidos ao exame artroscópico. MÉTODOS: Cada animal foi submetido a uma artroscopia bilateral tarsocrural empregando uma distensão com gás em uma articulação e líquido na articulação contralateral. O líquido sinovial foi avaliado as zero, seis, 12, 24 e 48 horas do pós-operatório. RESULTADOS: A utilização de CO2 para a artroscopia provoca uma sinovite aguda e leve tal como a distensão capsular por líquido, mostrando um aumento similar de leucócitos, TP (proteína total e TNF-a. Embora no líquido sinovial a quantidade de PGE2 tenha sido maior nas articulações submetidas à distensão por CO2, níveis mais baixos de hemoglobina e explosão oxidativa de leucócitos após a cirurgia indica que a artroscopia com CO2 diminuiu o

  17. Deficiência hídrica, trocas gasosas e crescimento de raízes em laranjeira ‘Valência’ sobre dois tipos de porta-enxertos Water deficit, gas exchange and root growth in 'Valencia' orange tree budded on two rootstocks

    Directory of Open Access Journals (Sweden)

    José Rodrigues Magalhães Filho

    2008-01-01

    Full Text Available 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 rizotrons, que permitiam a visualização das raízes, sendo 16 para cada porta-enxerto e submetidas ou não à irrigação. A deficiência hídrica às plantas foi aplicada pela interrupção do fornecimento de água às plantas. A condutância estomática decaiu após o quarto dia sem irrigação, causando redução da fotossíntese, da transpiração e da eficiência de carboxilação. O teor de carboidrato total (sacarose + açúcares redutores + amido em plantas sem estresse foi maior em 'Trifoliata', e entre os tratamentos com deficiência hídrica foi sempre inferior. As massas secas das plantas sem deficiência hídrica foram maiores, em ambos os porta-enxertos. Entre os tratamentos irrigados e não irrigados, o comprimento das raízes dentro de um mesmo tipo de porta-enxerto foram semelhantes. Porém, o comprimento das raízes de laranjeira 'Valência' sobre 'Cravo' foi significativamente maior. Mesmo sob deficiência hídrica e grande queda da produção fotossintética, as raízes permaneceram crescendo, possivelmente às expensas de substrato mobilizado de outros órgãos.The growth and distribution of the root system affect the response of the plants to water deficit. This work aim at the to evaluation of 'Valencia' orange budded on 'Rangpur¢ lime and Poncirus trifoliata ('Trifoliata' as to root growth, gas exchange (CO2 and H2O, leaf water potential and distribution of carbohydrates in several organs, in plants submitted to water deficit

  18. Trocas gasosas, características das folhas e crescimento de plantas jovens de Cupania vernalis Camb. submetidas a diferentes níveis de sombreamento Gas exchange and initial growth of young leaves of Cupania vernalis camb. submitted to different shading levels

    Directory of Open Access Journals (Sweden)

    Érico de Castro Lima Junior

    2005-10-01

    Full Text Available Cupania vernalis Camb. é uma espécie arbórea pertencente à família sapindaceae, conhecida popularmente como camboatá, camboatã. É uma espécie de grande importância pelo seu uso em plantios mistos destinados à recuperação de áreas degradadas e preservação permanente. Este estudo teve como objetivo básico caracterizar o desempenho ecofisiológico desta espécie sob condições de viveiro. Avaliou-se o efeito de quatro níveis de irradiância (Pleno sol, 30%, 50% e 70% de sombreamento sobre as trocas gasosas, concentração de nitrogênio, clorofilas foliares e crescimento de plantas jovens de Cupania vernalis. As plantas submetidas a 50% de sombreamento acumularam maior massa seca de folha, caule e massa seca total em comparação com as cultivadas a pleno sol, não sendo observada diferença quanto à massa seca de raízes. A maior taxa fotossintética e condutância estomática foram observadas em folhas de plantas crescidas sob pleno sol e 30% de sombreamento. Plantas sob condições mais sombreadas apresentaram teores mais elevados tanto de clorofilas quanto de nitrogênio nas folhas. Fato semelhante ocorreu com outras características como altura, diâmetro de caule e área foliar. Essas últimas características constituem fatores determinantes da qualidade de mudas. Os resultados possibilitaram concluir que as mudas desta espécie devem ser formadas sob condições de viveiro com sombreamento de 50% ou 70% para que se obtenham mudas de melhor qualidade.Cupania vernalis Camb. is an arboreal species belonging to the sapindaceae family, known popularly as "Camboatá", "Camboatã". This species has great economical importance by its use in mixed plantings trying to recovery permanent degraded and preservation areas. This study aimed, basically, at characterizing the ecophysiological aspects of this species under nursery conditions. The effect of four levels of irradiance (Full sunshine, 30%, 50% and 70% of shading on the gas

  19. Embolia gasosa por dióxido de carbono durante cirurgia laparoscópica: relato de caso Embolia gaseosa por dióxido de carbono durante cirugía laparoscópica: relato de caso Carbon dioxide embolism during laparoscopic surgery: case report

    Directory of Open Access Journals (Sweden)

    Tania Berger

    2005-02-01

    Full Text Available JUSTIFICATIVA E OBJETIVOS: A embolia venosa por CO2 durante cirurgias laparoscópicas é uma complicação rara, porém fatal na maioria dos casos. O objetivo deste relato é descrever um caso não fatal de embolia venosa por CO2 durante cirurgia laparoscópica. RELATO DO CASO: Paciente hipertensa foi submetida à anestesia geral para laparoscopia para exploração de colédoco. Após 150 minutos de pneumoperitôneo, a paciente evoluiu com taquicardia e hipotensão refratária ao uso de vasopressor. A gasometria arterial revelou grande diferença entre a pCO2 e a P ET CO2. Frente à hipótese de embolia gasosa, foi desinsuflado o pneumoperitôneo, e a cirurgia terminada pela técnica convencional. A paciente evoluiu com melhora do quadro hemodinâmico, sendo extubada ao término da cirurgia e encaminhada para sala de recuperação pós-anestésica (SRPA. CONCLUSÕES: O diagnóstico precoce e o tratamento imediato foram fundamentais na boa evolução do caso descrito.JUSTIFICATIVA Y OBJETIVOS: La embolia venosa por CO2 durante cirugías laparoscópicas es una complicación rara, sin embargo fatal en la mayoría de los casos. El objetivo de este relato es describir un caso no fatal de embolia venosa por CO2 durante cirugía laparoscópica. RELATO DEL CASO: Paciente hipertensa fue sometida a la anestesia general para laparoscopia y para exploración del colédoco. Después de 150 minutos de pneumoperitoneo, la paciente evolucionó con taquicardia e hipotensión refractaria al uso de vasopresor. La gasometría arterial reveló grande diferencia entre la pCO2 y la P ET CO2. De frente a la hipótesis de embolia gaseosa, fue desinsuflado el pneumoperitoneo, y la cirugía terminada por la técnica convencional. La paciente evolucionó con mejoría del cuadro hemodinámico, siendo extubada al término de la cirugía y encaminada para la sala de recuperación pos-anestésica (SRPA. CONCLUSIONES: El diagnóstico precoz y el tratamiento inmediato fueron

  20. COMPOSICIÓN MOLECULAR DE ACIDOS HUMICOS EVALUADA MEDIANTE PIRÓLISIS -CROMATOGRAFIA DE GASES- MASAS E HIDRÓLISIS TÉRMICA ASISTIDA Y METILACIÓN, EN SUELOS ALTOANDINOS – COLOMBIA

    Directory of Open Access Journals (Sweden)

    Claudia Martinez

    2014-07-01

    Full Text Available Se determinó la composición  molecular de ácidos húmicos (AH, extraídos del horizonte A de suelos altoandinos, Colombia dedicados a tres usos: bosque primario, cultivo y pastura. Los AH se obtuvieron mediante extracción secuencial de la materia orgánica humificada (MOH con soluciones de tetraborato, pirofosfato e hidróxido de sodio (0,1N, y fueron purificados por diferentes procesos analíticos. Su composición molecular se determinó  por Py-GC/MS y THMA. Los diferentes productos de la pirolisis se clasificaron atendiendo a la familia química a la que pertenecen,  prevalecieron los ácidos grasos (FA como el producto más abundante en los AH de todos los usos, mientras que  los fenoles, esteroles, S-compuestos y terpenos se encontraron en menor abundancia. Se presentaron diferencias en los porcentajes de abundancia relativa de los grupos identificados, demostrando que el cambio de uso de suelo influye en las propiedades físicas, químicas y biológicas del suelo por lo que se perciben diferentes grados de transformación, que afectan la composición de los AH y su reactividad en el suelo.

  1. Fast GC-FID based metabolic fingerprinting of Japanese green tea leaf for its quality ranking prediction.

    Science.gov (United States)

    Jumtee, Kanokwan; Bamba, Takeshi; Fukusaki, Eiichiro

    2009-07-01

    There is a need of reliable, rapid, and cost-effective analysis technique to evaluate food and crop compositions, which are important to improve their qualities and quantities. Prior to fast GC-FID development, metabolic fingerprints, and predictive models obtained from a conventional GC-FID were evaluated by comparison to those derived from GC-TOF-MS. A similar chromatographic pattern with higher sensitivity of polyphenol compounds including epicatechin gallate (ECg) and epigallocatechin gallate (EGCg) had been achieved by using conventional GC-FID. Fast gas chromatograph coupled with flame ionization detector (GC-FID) has been carried out with 10 m x 0.18 mm id x 0.20 microm df capillary column. The analysis time per sample was reduced to less than 14 min compared to those of a conventional GC-FID (38 min) and GC-TOF-MS (28 min). The fast GC-FID also offered reliable retention time reproducibility without significant loss of peak resolution. Projections to latent structures by means of partial least squares (PLS) with orthogonal signal correction filtering (OSC) was applied to the fast GC-FID data. The predictive model showed good model fit and predictability with RMSEP of 3.464, suggesting that fast GC-FID based metabolic fingerprinting could be an alternative method for the prediction of Japanese green tea quality.

  2. 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 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.

  3. 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.

  4. 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

  5. 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

  6. Investigation of electro-oxidation activity of Pt-CNTs/GC electrodes

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    The morphology and structure of Pt-CNTs/GC electrodes were characterized via Transmission Electron Microscopy (TEM) and selected area electron diffraction.The electro-oxidation behavior of CO and methanol on Pt-CNTs/GC electrodes were studied with cyclic voltommograms or chronoamperometry.Three oxidation peaks were observed for CO absorbed on PtCNTs/GC electrodes.Methanol was found to be dissociated spontaneously on the electrode to produce a strong absorbed intermediate CO.Among the three oxidation peaks,peak Ⅰ was presumed to be due to the bridged CO absorption while peaks Ⅱ and Ⅲ were attributed to the split in the linear CO which is absorbed on the PtCNTs/GC nanocluster with different particle size and Pt film.The oxidation current of methanol on the Pt-CNTs/GC electrode did not always increase with the increase in the amount of Pt loading,The result indicates that there is an optimal Pt loading for methanol oxidation.It is necesSary to select the catalyst with proper Pt loading when the anode of a direct-methanol fuel cell is prepared.

  7. A review on g-C3N4-based photocatalysts

    Science.gov (United States)

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

    2017-01-01

    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-C3N4-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-C3N4-based photocatalysts, including fundamental mechanism of heterogeneous photocatalysis, advantages, challenges and the design considerations of g-C3N4-based photocatalysts. The versatile properties of g-C3N4-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 (H2 evolution and overall water splitting), degradation of pollutants, carbon dioxide reduction, selective organic transformations and disinfection. Through reviewing the important state-of-the-art advances on this topic, it may provide new opportunities for designing and constructing highly effective g-C3N4-based photocatalysts for various applications in photocatalysis and other related fields, such as solar cell, photoelectrocatalysis, electrocatalysis, lithium battery, supercapacitor, fuel cell and separation and purification.

  8. Recently developed GC/MS and LC/MS methods for determining NSAIDs in water samples.

    Science.gov (United States)

    Farré, M; Petrovic, M; Barceló, D

    2007-02-01

    Pharmaceuticals have become major targets in environmental chemistry due to their presence in aquatic environments (following incomplete removal in wastewater treatment or point-source contaminations), threat to drinking water sources and concern about their possible effects to wildlife and humans. Recently several methods have been developed for the determination of drugs and their metabolites in the lower nanogram per litre range, most of them using solid-phase extraction (SPE) or solid-phase microextraction (SPME), derivatisation and finally gas chromatography mass spectrometry (GC-MS), gas chromatography tandem mass spectrometry (GC-MS/MS) and liquid chromatography electrospray tandem mass spectrometry (LC-ES/MS/MS). Due to the elevated polarity of non-steroidal anti-inflamatory drugs (NSAIDs), analytical techniques based on either liquid chromatography coupled to mass spectrometry (LC-MS) and gas chromatography coupled to mass spectrometry (GC-MS) after a previous derivatisation step are essential. The most advanced aspects of current GC-MS, GC-MS/MS and LC-MS/MS methodologies for NSAID analysis are presented.

  9. Design considerations for pulsed-flow comprehensive two-dimensional GC: dynamic flow model approach.

    Science.gov (United States)

    Harvey, Paul McA; Shellie, Robert A; Haddad, Paul R

    2010-04-01

    A dynamic flow model, which maps carrier gas pressures and carrier gas flow rates through the first dimension separation column, the modulator sample loop, and the second dimension separation column(s) in a pulsed-flow modulation comprehensive two-dimensional gas chromatography (PFM-GCxGC) system is described. The dynamic flow model assists design of a PFM-GCxGC modulator and leads to rapid determination of pneumatic conditions, timing parameters, and the dimensions of the separation columns and connecting tubing used to construct the PFM-GCxGC system. Three significant innovations are introduced in this manuscript, which were all uncovered by using the dynamic flow model. A symmetric flow path modulator improves baseline stability, appropriate selection of the flow restrictors in the first dimension column assembly provides a generally more stable and robust system, and these restrictors increase the modulation period flexibility of the PFM-GCxGC system. The flexibility of a PFM-GCxGC system resulting from these innovations is illustrated using the same modulation interface to analyze Special Antarctic Blend (SAB) diesel using 3 s and 9 s modulation periods.

  10. GC/MS based identification of skunk spray maliciously deployed as "biological weapon" to harm civilians.

    Science.gov (United States)

    Wennig, Robert; Schneider, Serge; Meys, François

    2010-05-15

    Our laboratory has been asked to elucidate the origin of a strong "toxic smell" present in a prominent politician's office, private house and motorcar. This stinky and pungent atmosphere has caused serious nausea and vomiting to several individuals. Urine samples were collected from the persons presenting symptoms of nausea for toxicological analysis. Drops, paper and cotton swabs of an oily liquid found at the implicated places were submitted by police to our laboratory for investigation. Methanol extracts of the drops were acetylated for gas chromatography/mass spectrometry (GC/MS) analysis in the electron impact mode; the cotton and paper swabs were analysed using headspace-gas chromatography/mass spectrometry (HS-GC/MS). The GC/MS analysis of the acetylated methanol extracts revealed that the major peaks of the chromatogram could be attributed to 2-methylquinoline, to 2-quinolinemethanethiol, to S-2-quinolinemethyl thioacetate, to 2-phenylethanethiol, to bis(E)-2-butenyl disulphide and to bis(3-methylbutyl) disulphide. Several volatile sulphur-containing compounds have been identified with the HS-GC/MS system. Detailed examination of the spectra as well as GC/MS analysis of commercially available skunk secret allowed us to relate the identified compounds to those present in the defence spray of skunks. No health sequels were observed for any of the persons implicated in this case.

  11. Urinary metabolomics of pregnant women at term: a combined GC/MS and NMR approach.

    Science.gov (United States)

    Caboni, Pierluigi; Meloni, Alessandra; Lussu, Milena; Carta, Emanuela; Barberini, Luigi; Noto, Antonio; Deiana, Sara Francesca; Mereu, Rossella; Ragusa, Antonio; Paoletti, Anna Maria; Melis, Gian Benedetto; Fanos, Vassilios; Atzori, Luigi

    2014-10-01

    Physiological changes leading to parturition are not completely understood while clinical diagnosis of labour is still retrospective. Gas chromatography mass spectrometry (GC/MS) and nuclear magnetic resonance spectroscopy (NMR) represent two of the main analytical platforms used in clinical metabolomics. Metabolomics might help us to improve our knowledge about the biochemical mechanisms underlying labour. Urine samples (n = 59), collected from pregnant women at term of gestation before and/or after the onset of labour, were analysed by GC/MS and NMR techniques in order to identify the metabolic profile. Both GC/MS and NMR data matrices containing the identified metabolites were analysed by multivariate statistical techniques in order to characterise the discriminant variables between labour (L) and not labour (NL) status. 18 potential metabolites (11 with (1)H-NMR, eight with GC-MS: glycine was relevant in both) were found discriminant in urine of women during labour. Taken together, the identified metabolites produced a composite biomarker pattern, a sort of barcode, capable of differentiating between labour and not labour conditions. Major discriminant metabolites for NMR and GC/MS analysis were: alanine, glycine, acetone, 3-hydroxybutiyric acid, 2,3,4-trihydroxybutyric acid and succinic acid, giving a urine metabolite signature on the late phase of labour. The metabolomics analysis evidenced clusters of metabolites involved in labour condition able to discriminate between urine samples collected before the onset and during labour, potentially offering the promise of a robust screening test.

  12. Vertebrate codon bias indicates a highly GC-rich ancestral genome.

    Science.gov (United States)

    Nabiyouni, Maryam; Prakash, Ashwin; Fedorov, Alexei

    2013-04-25

    Two factors are thought to have contributed to the origin of codon usage bias in eukaryotes: 1) genome-wide mutational forces that shape overall GC-content and create context-dependent nucleotide bias, and 2) positive selection for codons that maximize efficient and accurate translation. Particularly in vertebrates, these two explanations contradict each other and cloud the origin of codon bias in the taxon. On the one hand, mutational forces fail to explain GC-richness (~60%) of third codon positions, given the GC-poor overall genomic composition among vertebrates (~40%). On the other hand, positive selection cannot easily explain strict regularities in codon preferences. Large-scale bioinformatic assessment, of nucleotide composition of coding and non-coding sequences in vertebrates and other taxa, suggests a simple possible resolution for this contradiction. Specifically, we propose that the last common vertebrate ancestor had a GC-rich genome (~65% GC). The data suggest that whole-genome mutational bias is the major driving force for generating codon bias. As the bias becomes prominent, it begins to affect translation and can result in positive selection for optimal codons. The positive selection can, in turn, significantly modulate codon preferences.

  13. Study on the Fingerprints of Bergamot Volatile Oil by GC-MS%佛手挥发油GC-MS指纹图谱研究

    Institute of Scientific and Technical Information of China (English)

    金宏; 公衍玲; 赵文英

    2009-01-01

    采用超临界CO2流体萃取法提取佛手挥发油,进一步用GC-MS技术对其进行指纹图谱测定,并采用中药指纹图谱计算软件进行计算,建立了佛手挥发油的特征指纹图谱.结果表明,该方法有较好的重复性、精密度和稳定性(RSD 均小于3%),得到较好的佛手挥发油GC-MS指纹图谱.该方法快速准确,可用于佛手药材的质量控制.

  14. Detailed analysis of the essential oil from Cistus albidus L. by combination of GC/RI, GC/MS and 13C-NMR spectroscopy.

    Science.gov (United States)

    Paolini, Julien; Tomi, Pierre; Bernardini, Antoine-François; Bradesi, Pascale; Casanova, Joseph; Kaloustian, Jacques

    2008-01-01

    The composition of the essential oil of Cistus albidus (L.) obtained from plants growing wild in Provence (France) has been investigated using GC-RI (RI = retention indices), GC/MS and (13)C-NMR. Eighty-eight components were reported accounting for 81.8% of the essential oil. This essential oil was characterized by a high content of sesquiterpenes with alpha-zingiberene (12.8%), alpha-curcumene (7.7%), (E)-beta-caryophyllene (5.9%), alpha-cadinol (5.4%), alpha-bisabolol (4.1%), caryophyllene oxide (3.8%), allo-aromadendrene (3.4%), delta-cadinene (3.4%), and germacrene D (3.1%) being the main components.

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

    Directory of Open Access Journals (Sweden)

    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.

  16. Analysis of Aroma Components in Spice by GC/MS%香辛料调味品香气成分的GC/MS分析

    Institute of Scientific and Technical Information of China (English)

    刘素梅; 李雁; 刘欣

    2013-01-01

    利用GC/MS联用对香辛料调味品的香气成分进行分离分析,共分离鉴定出48种香气成分,其相对含量较高的是烯类,占42.49%;其次是酯类,占17.36%;含量最少的是苯类,占0.65%.

  17. Extraction and preconcentration technique for triazole pesticides from cow milk using dispersive liquid-liquid microextraction followed by GC-FID and GC-MS determinations.

    Science.gov (United States)

    Farajzadeh, Mir Ali; Djozan, Djavanshir; Mogaddam, M R Afshar; Bamorowat, Mehdi

    2011-06-01

    A simple and rapid dispersive liquid-liquid microextraction (DLLME) technique coupled with gas chromatography-flame ionization detection (GC-FID) and gas chromatography-mass spectrometry (GC-MS) was developed for the extraction, preconcentration, and analysis of triazole pesticides (penconazole, hexaconazole, tebuconazole, triticonazole, and difenoconazole) in cow milk samples. Initially to 5 mL milk sample, NaCl and acetonitrile were added as salting-out agent and extraction solvent, respectively. After manual shaking, the mixture was centrifuged. In the presence of sodium chloride, a two-phase system was formed: upper phase, acetonitrile containing triazole pesticides and lower phase, aqueous phase containing soluble compounds and the precipitated proteins. After the extraction of pesticides from milk, a portion of supernatant phase (acetonitrile) was removed, mixed with chloroform at microliter level and rapidly injected by syringe into 5 mL distilled water. In this process, triazole pesticides were extracted into fine droplets of chloroform (as extraction solvent). After centrifugation, the fine droplets of chloroform were sedimented in bottom of the conical test tube. Finally, GC-FID and GC-MS were used for the separation and determination of analytes in the sedimented phase. Some important parameters like type of solvent for extraction of pesticides from milk, salt amount, the volume of extraction solvent, etc., which affect the extraction efficiency, were completely studied. Under the optimum conditions, enrichment factors were in the range of 156-380. The linear ranges of calibration curves were wide and limits of detection (LODs) and limits of quantification (LOQs) were between 4-58 and 13-180 μg/L, respectively. This method is very simple and rapid, requiring <15 min for sample preparation.

  18. 巴豆种子油的GC-MS分析%Analysis of Oil from Seeds of Croton Tiglium By GC-MS

    Institute of Scientific and Technical Information of China (English)

    梁英; 潘英明

    2002-01-01

    巴豆种子经石油醚和无水乙醇提取得巴豆种子油,通过气相色谱-质谱联用仪(GC-MS)测定其中的化学成分,结果显示,巴豆种子油中含有26个组分,本文确定了其中22个组分的结构.

  19. Determination of Formaldehyde and Acetaldehyde in Beer by GC-MS%GC-MS法快速测定啤酒中的甲醛和乙醛

    Institute of Scientific and Technical Information of China (English)

    闫吉昌; 初人合; 李晓坤; 闫福成; 陈大伟; 王悦宏

    2006-01-01

    报道了用GC-MS法同时测定无甲醛工艺啤酒中微量甲醛和乙醛的含量.用选择离子检测法定性,标准曲线法定量,方法的检出限可达0.01×10-6g/L.该方法快速、简便,结果重现性良好.

  20. Characterization of aroma active compounds in fruit juice and peel oil of Jinchen sweet orange fruit (Citrus sinensis (L.) Osbeck) by GC-MS and GC-O.

    Science.gov (United States)

    Qiao, Yu; Xie, Bi Jun; Zhang, Yan; Zhang, Yun; Fan, Gang; Yao, Xiao Lin; Pan, Si Yi

    2008-06-12

    Gas chromatography-mass spectrometry (GC-MS) and gas chromatography-olfactometry (GC-O) were used to determine the aromatic composition and aroma active compounds of fruit juice and peel oil of Jinchen sweet orange fruit. Totals of 49 and 32 compounds were identified in fruit juice and peel oil, respectively. GC-O was performed to study the aromatic profile of Jinchen fruit juice and peel oil. A total of 41 components appeared to contribute to the aroma of fruit juice and peel oil. Twelve components were the odorants perceived in both samples. The aromatic compositions of fruit juice were more complex than that of peel oil. Ethyl butanoate, beta-myrcene, octanal, linalool, alpha-pinene, and decanal were found to be responsible for the aromatic notes in fruit juice and peel oil. Nineteen components have been perceived only in the juice and ten compounds were described as aromatic components of only the peel oil by the panelists. These differences lead to the different overall aroma between fruit juice and peel oil.

  1. Determination of Low-molecular Aldehydes and Ketones by GC-MS%低分子醛酮类物质的GC-MS测定

    Institute of Scientific and Technical Information of China (English)

    马贺伟

    2015-01-01

    采用GC-MS对甲醛、乙醛、丙醛、丁酮、戊醛五种物质的2,4-二硝基苯肼(DNPH)衍生物进行测定.结果表明,DNPH的热分解产物的色谱峰与甲醛-DNPH衍生物重叠,对甲醛-DNPH衍生物的检测应采用选择离子监测模式.除甲醛衍生物外,其它四种衍生物的色谱峰均表现为双峰形貌,其对应于各衍生物分子结构中的顺反异构体.衍生物的出峰顺序随碳原子数增加而增加,甲醛衍生物流出最快,戊醛衍生物流出最慢.各衍生物的分子离子峰强度较高.DNPH衍生化、GC-MS法适用于低分子醛酮的GC-MS鉴别.

  2. GC-MS and GC-MS/MS in PCI mode determination of mescaline in peyote tea and in biological matrices.

    Science.gov (United States)

    Gambelunghe, Cristiana; Marsili, Remo; Aroni, Kyriaki; Bacci, Mauro; Rossi, Riccardo

    2013-01-01

    Peyote, a cactus containing the hallucinogen mescaline, is used to induce altered states of consciousness in religious ceremonies or for recreational purpose. This study reports a case of an underage boy suspected of mescaline abuse. For this purpose, we analyzed a dark green liquid sample found in the bedroom of the boy whose urine and hair samples were collected shortly after the drink was found. A method by gas chromatography-mass spectrometry tandem mass spectrometry (GC-MS/MS) in positive chemical ionization mode was developed and validated in terms of linearity, specificity, accuracy, and sensitivity for mescaline determination at the low concentrations present in hair. GC-MS analysis of the liquid identified mescaline, while urine was negative; GC-MS/MS segmental hair analysis identified mescaline in the proximal segment (root to 2 cm), while the distal segments were negative. Although peyote was uncommonly encountered, its use was confirmed by segmental hair analysis that can provide long-term information about drugs use.

  3. GC/Mass analysis of the volatile compounds of P. hyrcanicum diethyl ether extract and GC profiling of some Iranian Polygonum species

    Directory of Open Access Journals (Sweden)

    S. Saeidnia

    2014-01-01

    Full Text Available In this study, the relationship among four species of Polygonum (including P. hyrcanicum (three samples, P. persicaria, P. avicular, and P. hydropiper was investigated by GC profiling. Furthermore, the major compounds of the ethylic ether extract of P. hyrcanicum were identified by GC/MS as: α-bisabolol (17.5%, cedrol (15.9%, sesquisabinene hydrate (13.0%, α-elemol (10.5% and trans-longipinocarveol (10.1%. All the identified compounds were sesquiterpenes and no monoterpene, fatty acid and/or hydrocarbone were detected in the extract. Chemical distances among the mentioned species were calculated in order to construct the dendrogram of closely related samples. Results indicated that the distance between two samples of P. hyrcanicum was considered to be short and their GC profiles were quite similar to each other and also there was a close relationship between the two samples of Polygonum with P. avicular. P. hydropiper was observed far from the two samples of P. hyrcanicum in comparison to other samples. Interestingly, P. hyrcanicum, gathered from Veresk, had no close relationship with other pairs of P. hyrcanicum.The results of this study support the phylogenetic relationships among these Polygonum species which was previously reported.

  4. The g-C3 N4 /C2 N Nanocomposite: A g-C3 N4 -Based Water-Splitting Photocatalyst with Enhanced Energy Efficiency.

    Science.gov (United States)

    Wang, Huimin; Li, Xingxing; Yang, Jinlong

    2016-07-01

    Water-splitting photocatalysts with good energy efficiency are highly desirable, among which metal-free graphitic carbon nitride (g-C3 N4 ) is considered to be very promising and has been intensively studied in recent years. However, its practical application is hindered by the relatively low efficiencies of visible-light absorption and electron-hole separation. Herein, based on first-principles calculations, it is predicted that, by forming nanocomposites with another carbon nitride (C2 N), the energy efficiency of g-C3 N4 can be significantly improved. On one hand, C2 N has a wide, strong optical absorption in the visible-light region, which acts as a photosensitizer and enhances the photoabsorption efficiency of the composite photocatalyst. On the other hand, C2 N forms a type II heterojunction with g-C3 N4 , which leads to efficient separation of photogenerated electron-hole pairs through the chemical potential difference between the two components. These results provide a potential route to achieve highly efficient metal-free photocatalysts for water splitting.

  5. Sample Preparation for Headspace GC Analysis of Residual Solvents in Hyaluronic Acid Derivative Fiber

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Hoon Joo; Kim, Dong Min; Yang, Jeong Soo [LG life Sciences, Ltd./R and D Park, Daejeon (Korea, Republic of); Kim, Chan Wha [Korea University, Seoul (Korea, Republic of)

    2006-02-15

    The aim of this study is to develop efficient sample preparation method for HS-GC analysis of residual solvents in HA derivative fiber. Compared to direct extraction of residual solvents from HA derivative fiber, the extraction through the hydrolysis of HA derivative fiber by HAse gave more complete and higher reproducible quantification of residual solvent. To validate HS-GC analysis method of residual solvents, specificity, limits of detection and quantification, linearity, accuracy and precision are investigated in the study. HA derivative fiber was hydrolyzed using HAse for headspace gas chromatographic analysis of residual solvents of ethanol, acetone and isopropanol in HA derivative fiber. This study showed that the developed method had specificity, linearity, accuracy and precision. In addition, it demonstrated that HS-GC coupled with matrix-breaking method such as hydrolysis was available for the determination of residual solvents in a matrix like HA derivative fiber.

  6. 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.

  7. Metabolomics and Trace Element Analysis of Camel Tear by GC-MS and ICP-MS.

    Science.gov (United States)

    Ahamad, Syed Rizwan; Raish, Mohammad; Yaqoob, Syed Hilal; Khan, Altaf; Shakeel, Faiyaz

    2017-06-01

    Camel tear metabolomics and elemental analysis are useful in getting the information regarding the components responsible for maintaining the protective system that allows living in the desert and dry regions. The aim of this study was to correlate that the camel tears can be used as artificial tears for the evaluation of dryness in the eye. Eye biomarkers of camel tears were analyzed by gas chromatography-mass spectroscopy (GC-MS) and inductively coupled plasma mass spectroscopy (ICP-MS). The major compounds detected in camel tears by GC-MS were alanine, valine, leucine, norvaline, glycine, cadaverine, urea, ribitol, sugars, and higher fatty acids like octadecanoic acid and hexadecanoic acid. GC-MS analysis of camel tears also finds several products of metabolites and its associated metabolic participants. ICP-MS analysis showed the presence of different concentration of elemental composition in the camel tears.

  8. GC-MS determination of isoflavonoids in seven red Cuban propolis samples.

    Science.gov (United States)

    Campo Fernández, Mercedes; Cuesta-Rubio, Osmany; Rosado Perez, Arístides; Montes De Oca Porto, Rodny; Márquez Hernández, Ingrid; Piccinelli, Anna Lisa; Rastrelli, Luca

    2008-11-12

    In the present study, the phenolic composition analysis of seven red varieties of propolis, collected in different regions of Cuba, was evaluated by gas chromatography/mass spectrometry (GC-MS). Seventeen compounds were identified in all samples by the interpretation of their mass spectra. This appears to be the first report on the GC-MS analysis of isoflavonoids in the propolis. The results confirmed the presence of the main isoflavonoids isolated previously and suggested the general structure for the other five isoflavonoids. Vestitol, 7-O-methylvestitol, and medicarpin were present in high amounts in all propolis samples analyzed. This result indicates that propolis samples rich in isoflavonoids are not exclusively found in Pinar del Rio province and proves that GC-MS technique is a useful and alternative tool for the chemical analysis of tropical red propolis.

  9. GC/GCMS analysis of the petroleum ether and dichloromethane extracts of Moringa oleifera roots

    Institute of Scientific and Technical Information of China (English)

    Shaheen Faizi; Saima Sumbul; Muhammed Ali Versiani; Rubeena Saleem; Aisha Sana; Hira Siddiqui

    2014-01-01

    Objective:To explore the phytochemical constituents from petroleum ether and dichloromethane extracts of Moringa oleifera (M. oleifera) roots using GC/GC-MS. Methods: A total of 5.11 kg fresh and undried crushed root of M. oleifera were cut into small pieces and extracted with petroleum ether and dichloromethane (20 L each) at room temperature for 2 d. The concentrated extracts were subjected to their GC-MS analysis. Results:The GC-MS analysis of the petroleum ether and dichloromethane extracts of M. oleifera roots, which showed promising biological activities, has resulted in the identification 102 compounds. These constituents belong to 15 classes of compounds including hydrocarbons, fatty acids, esters, alcohols, isothiocyanate, thiocyanate, pyrazine, aromatics, alkamides, cyanides, steroids, halocompounds, urea and N-hydroxyimine derivatives, unsaturated alkenamides, alkyne and indole. GC/GC-MS studies on petroleum ether extract of the roots revealed that it contained 39 compounds, belonging to nine classes. Cyclooctasulfur S8 has been isolated as a pure compound from the extract. The major compounds identified from petroleum ether extract were trans-13-docosene (37.9%), nonacosane (32.6%), cycloartenol (28.6%) nonadecanoic acid (13.9%) and cyclooctasulfur S8 (13.9%). Dichloromethane extract of the roots was composed of 63 compounds of which nasimizinol (58.8%) along with oleic acid (46.5%), N-benzyl-N-(7-cyanato heptanamide (38.3%), N-benzyl-N-(1-chlorononyl) amide (30.3%), bis [3-benzyl prop-2-ene]-1-one (19.5%) and N, N-dibenzyl-2-ene pent 1, 5-diamide (11.6%) were the main constituents. Conclusions:This study helps to predict the formula and structure of active molecules which can be used as drugs. This result also enhances the traditional usage of M. oleifera which possesses a number of bioactive compounds.

  10. 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.

  11. 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.

  12. Evolution of genome size and genomic GC content in carnivorous holokinetics (Droseraceae).

    Science.gov (United States)

    Veleba, Adam; Šmarda, Petr; Zedek, František; Horová, Lucie; Šmerda, Jakub; Bureš, Petr

    2017-02-01

    Studies in the carnivorous family Lentibulariaceae in the last years resulted in the discovery of the smallest plant genomes and an unusual pattern of genomic GC content evolution. However, scarcity of genomic data in other carnivorous clades still prevents a generalization of the observed patterns. Here the aim was to fill this gap by mapping genome evolution in the second largest carnivorous family, Droseraceae, where this evolution may be affected by chromosomal holokinetism in Drosera METHODS: The genome size and genomic GC content of 71 Droseraceae species were measured by flow cytometry. A dated phylogeny was constructed, and the evolution of both genomic parameters and their relationship to species climatic niches were tested using phylogeny-based statistics. The 2C genome size of Droseraceae varied between 488 and 10 927 Mbp, and the GC content ranged between 37·1 and 44·7 %. The genome sizes and genomic GC content of carnivorous and holocentric species did not differ from those of their non-carnivorous and monocentric relatives. The genomic GC content positively correlated with genome size and annual temperature fluctuations. The genome size and chromosome numbers were inversely correlated in the Australian clade of Drosera CONCLUSIONS: Our results indicate that neither carnivory (nutrient scarcity) nor the holokinetism have a prominent effect on size and DNA base composition of Droseraceae genomes. However, the holokinetic drive seems to affect karyotype evolution in one of the major clades of Drosera Our survey confirmed that the evolution of GC content is tightly connected with the evolution of genome size and also with environmental conditions. © The Author 2016. Published by Oxford University Press on behalf of the Annals of Botany Company. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  13. Extraction of pure components from overlapped signals in gas chromatography-mass spectrometry (GC-MS

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    Likić Vladimir A

    2009-10-01

    Full Text Available Abstract Gas chromatography-mass spectrometry (GC-MS is a widely used analytical technique for the identification and quantification of trace chemicals in complex mixtures. When complex samples are analyzed by GC-MS it is common to observe co-elution of two or more components, resulting in an overlap of signal peaks observed in the total ion chromatogram. In such situations manual signal analysis is often the most reliable means for the extraction of pure component signals; however, a systematic manual analysis over a number of samples is both tedious and prone to error. In the past 30 years a number of computational approaches were proposed to assist in the process of the extraction of pure signals from co-eluting GC-MS components. This includes empirical methods, comparison with library spectra, eigenvalue analysis, regression and others. However, to date no approach has been recognized as best, nor accepted as standard. This situation hampers general GC-MS capabilities, and in particular has implications for the development of robust, high-throughput GC-MS analytical protocols required in metabolic profiling and biomarker discovery. Here we first discuss the nature of GC-MS data, and then review some of the approaches proposed for the extraction of pure signals from co-eluting components. We summarize and classify different approaches to this problem, and examine why so many approaches proposed in the past have failed to live up to their full promise. Finally, we give some thoughts on the future developments in this field, and suggest that the progress in general computing capabilities attained in the past two decades has opened new horizons for tackling this important problem.

  14. 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.

  15. 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.

  16. 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.

  17. On GC fingerprint analysis of fennel volatile constituents%小茴香挥发性成分 GC 指纹图谱研究

    Institute of Scientific and Technical Information of China (English)

    杨丽萍; 云琦; 高晓黎

    2015-01-01

    Objective To establish a GC fingerprint analysis method for the quality control of fennel.Meth-ods Fennel oil was extracted by steam distillation method.The fingerprint analysis of volatile oil was con-ducted by GC and the fingerprint peaks were identified with GC-MS.Results The batch of fennel were an-alyzed by GC,and ten common peaks were shown in the fingerprints,nine of which were identified.The established fingerprint analysis method was validated .The similarities of samples were over 0.95.Conclu-sion The fingerprint analysis method is simple,practical and suitable for the quality control of fennel.%目的:建立小茴香挥发性成分气相色谱指纹图谱分析方法,对挥发油成分进行分析,为控制小茴香挥发油质量提供依据。方法采用水蒸气蒸馏法提取小茴香挥发油,对10个产地小茴香进行气相色谱分析,用气相色谱建立挥发油指纹图谱分析法,并用 GC-MS 对指纹峰进行鉴别。结果指纹图谱中共有10个共有峰,其中8个成分得到鉴定,所建立指纹图谱分析方法学各项目符合规定,各批样品相似度>0.95。结论所建立指纹图谱方法分析简便易行,为更好控制小茴香的质量提供了新的方法。

  18. 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

    Directory of Open Access Journals (Sweden)

    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.

  19. Composição química e atividade antifúngica do óleo essencial de poejo em diferentes estágios de desenvolvimento

    Directory of Open Access Journals (Sweden)

    Ana Paula do Amaral Mônaco Foganholi

    2015-10-01

    Full Text Available  O objetivo deste estudo foi comparar o rendimento, a composição química e a atividade antifúngica do óleo essencial de Mentha pulegium (poejo em diferentes estágios de desenvolvimento, cultivada sob condições controladas no sul do Brasil. A hidrodestilação de folhas frescas de M. pulegium, coletadas aos 60, 70 e 85 dias após o transplante, apresentou rendimento de óleo essencial de 0,17 %, 0,23 % e 0,17 %, respectivamente. Todas as amostras de óleo apresentaram atividade contra Cladosporium herbarum. Através das análises de cromatografia gasosa (GC e GC/MS do óleo essencial, foram identificados onze constituintes, sete (mentona, isomentona, neoisomentol, pulegona, piperitona, 1.1- dimetoxi-2- nonino e piperitenona comuns às três amostras, enquanto dois outros (mentofurano, mirtenal foram detectados somente nas amostras da primeira e segunda coletas. A pulegona foi o principal constituinte nas duas primeiras amostras (26,65 %, seguida pela piperitenona (20,41; 12,60 %. A concentração de pulegona aumentou para 31,05 % na última coleta, porém o constituinte majoritário foi a piperitenona (36,32 %. Os resultados demonstraram que o óleo essencial de M. pulegium apresenta potencial como agente antifúngico e sua composição química depende do estágio de desenvolvimento da planta.

  20. 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.

  1. Variação da quantidade de β-cariofileno em óleo essencial de Plectranthus amboinicus (Lour. Spreng., Lamiaceae, sob diferentes condições de cultivo Variation in the amount of β-caryophyllene in essential oil of Plectranthus amboinicus (Lour. Spreng. Lamiaceae under different conditions of cultivation

    Directory of Open Access Journals (Sweden)

    Fabíola B. Carneiro

    2010-09-01

    Full Text Available O presente trabalho teve como objetivo avaliar a influência do adubo, da irrigação, da incidência solar, do horário de coleta e da idade da planta na quantidade de β-cariofileno no óleo essencial de Plectranthus amboinicus (Lour. Spreng., Lamiaceae. As plantas foram cultivadas em canteiros experimentais entre os meses de dezembro de 2006 a setembro de 2007. O substrato utilizado foi adubo orgânico (esterco bovino, adubo mineral 1 [NPK (nitrogênio, fósforo e potássio] e adubo mineral 2 (NPK com calcário sob diferentes tratamentos. A técnica analítica quantitativa utilizada foi a cromatografia gasosa (GC/FID. De acordo com os resultados obtidos nos meses de menor precipitação de chuvas obteve-se maior rendimento de óleo essencial, e os meses de maior precipitação de chuvas mostraram uma tendência de baixos rendimentos.This study aimed to evaluate the influence of fertilizer, irrigation, the incidence sun, the time of collection and the plant in the amount of β-caryophyllene in the essential oil of Plectranthus amboinicus (Lour. Spreng., Lamiaceae. The plants were grown in experimental beds between the months of December 2006 to September 2007. The substrate was used organic fertilizer (esterco veal, fertilizer mineral 1 [NPK (nitrogen, phosphorus and potassium] and fertilizer mineral 2 (NPK with limestone under different treatments. The quantitative analytical technique was used to gas chromatography (GC/FID. According to the results obtained in months of lower precipitation of rainfall received are higher yield of essential oil, and the months of highest precipitation of rain showed a trend of low income.

  2. Nitrogen-fixing aerobic bacteria have higher genomic GC content than non-fixing species within the same genus

    OpenAIRE

    McEwan, Catriona E.; Gatherer, Derek; McEwan, Neil R.

    1998-01-01

    The genomic GC contents of both nitrogen-fixing and non-fixing members of eight genera of bacteria are investigated. Analysis by t-tests showed that in the two aerobic genera investigated (Aquaspirillum and Vibrio) there is a significantly higher GC content in the nitrogen-fixing members of the genus than in those unable to Fix nitrogen, whilst in anaerobic genera there is either no GC bias, or in the case of two genera (Rhodospirillum and Clostridium) there is a significantly higher GC conte...

  3. Cyclophosphamide identification in wipe test by GC-MS and solid phase extraction Identificação de ciclofosfamida em wipe teste por CG-EM com prévia extração em fase sólida

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    Isarita Martins

    2004-03-01

    Full Text Available In this study cyclophosphamide was quantified after adapting a prior analytical method using gas chromatography-mass spectrometry after solid phase purification and derivatization with trifluoroacetic anhydride. The analyte was measured by analysis in wipe test from infusion bags, which may be contaminated by contact with the gloves used during preparation of the drugs. Surface of bag contaminated may be an important source of contamination for workers in the others chemoterapy handling areas, such as administration rooms. This drug, in fact, is one of the most frequently used alkylating antineoplastic agents for different types of tumors and it is furthermore classified as a human carcinogen by IARC. Ifosfamide was used as internal standard and the quantification was carried out by reference to calibration curves within a range from 1 to 100 ng/mL. The limit of detection was 0.4 ng/mL. The values of the variation coefficient varied from 0.5 to 10% (intra-assay and from 0 to 19% (interassay. Frozen reference wipe samples containing cyclophosphamide were analysed over one month and no significant loss was observed. The range obtained for bias assay was 83-116% and the recovery was 98.9%. Cyclophosphamide was measured in 36 of 42 infusion bags collected from different hospitals with values ranging from 90 to 41874 ng (median= 607.5 ng. The results, well related to those reported in the literature, suggest that this method can be used to identify cyclophosphamide from wipe samples and can be considered useful in exposure assessment to this drug.A ciclofosfamida é uma agente alquilante freqüentemente utilizado na prática clínica para diferentes tipos de tumores e, é classificado como carcinógeno para humanos pelo IARC. Neste estudo, o fármaco foi quantificado, após adaptação de um método analítico, utilizando a cromatografia gasosa acoplada à espectrometria de massa com prévia extração em fase sólida e derivação com anidrido

  4. Development of a fast GC/MS-system for airborne measurements of Volatile Organic Compounds

    Science.gov (United States)

    Wenk, Ann-Kathrin; Wegener, Robert; Hofzumahaus, Andreas; Wahner, Andreas

    2010-05-01

    Volatile Organic Compounds (VOC) determine the radical chemistry of the atmosphere. They can serve both as sources, or sinks for radicals. Mass spectrometry linked to gas chromatography (GC/MS) is a widespread technique in environmental analysis since it can be used to separate and analyze any compound which can be evaporated and pass the analytical column with very high precision and a good sensitivity. The use of special chromatographic phases and long capillary columns enables the quantification of a wide range of compounds with little interference from other sample constituents. An in situ GC/MS consists in principle of three compartments, 1) a preconcentration unit where the sample is extracted from the air, focussed onto a small volume and volatilized, 2) a chromatographic system where the analytes are separated on the analytical column and 3) a mass spectrometer where the compounds are ionized and detected. VOC have to be preconcentrated due to their low concentration level and in order to get enough sensitivity for analysis. The aim of this project was to develop an in situ GC/MS system to analyze volatile Nonmethane Hydrocarbons (NMHC) and Oxygenated Volatile Organic Compounds (OVOC) for the High Altitude and LOng Range Research Aircraft (HALO). In contrast to other analytical instruments a GC/MS works discontinuously. The preconcentration unit is either heated up when the compounds are volatilized or cooled down when substances are adsorbed. The same is true for the GC oven. It is heated up when the compounds are separated or it is cooled down to be ready for the next injection. On a system with a single GC oven, these processes will inevitably lengthen the whole analytical procedure. To speed up the analytical process the GC/MS system described here was equipped with two GC ovens and two adsorption units. While the components are adsorbed in one adsorption unit, in the other unit the components are desorbed and transferred to the GC unit. The second GC

  5. 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.

  6. A GC-FID method for quantitative analysis of N,N-carbonyldiimidazole.

    Science.gov (United States)

    Lee, Claire; Mangion, Ian

    2016-03-20

    N,N-Carbonyldiimidazole (CDI), a common synthetic reagent used in commercial scale pharmaceutical synthesis, is known to be sensitive to hydrolysis from ambient moisture. This liability demands a simple, robust analytical method to quantitatively determine reagent quality to ensure reproducible performance in chemical reactions. This work describes a protocol for a rapid GC-FID based analysis of CDI.

  7. GC-MS analysis of bioactive compounds in the methanol extract of Clerodendrum viscosum leaves

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    Pritipadma Panda

    2015-01-01

    Full Text Available Background: Clerodendrum viscosum is commonly found in India and Bangladesh. Previously, various parts of this plant were reported for treatment of different types of diseases and there was no report on GC-Ms analysis. Objective: To analyze and characterize the phytochemical compounds of methanol extract of Clerodendrum viscosum using GC-MS. Materials and Methods: The preliminary phytochemical screening of methanol extract was carried out according to standard procedures described in WHO guidelines. Various bioactive compounds of the extract were determined by GC-MS technique. Results: The presence of steroids, triterpenoids, alkaloids, saponins, flavonoids, tannins and carbohydrate was found on phytochemical screening of methanol extract of the leaves. The GC-MS analysis showed 16 peaks of different phytoconstituents namely acetamide,N,N-carbonylbis-, 4-Pyranone,2,3-dihydro-, alpha-D-Galactofuranoside, methyl 2,3,5,6-tetra-O-methyl-, Glycerin, Xylitol, N,N-Dimethylglycine, 4H-Pyran-4-one,2,3-dihydro-3, 5-dihydroxy-6-methyl-, Benzofuran,2,3-dihydro-, 5-Hydroxymethylfurfural, 2(1HPyrimidinone,1-methyl-, 2,4-Dihydroxy-5,6-dimethylpyrimidine, 3-Deoxy-d-mannoic lactone, 1,3-Methylene-d-arabitol, Orcinol, n-Hexadecanoic acid and Phenol,4,4′-(1-methyl ethylidene bis etc. Conclusion: The bioactive compounds present in the methanol extract of Clerodendrum viscosum suggest the application of this extract for the treatment of various diseases by the aborigine tribes.

  8. Field portable detection of VOCs using a SAW/GC system

    Energy Technology Data Exchange (ETDEWEB)

    Staples, E.J. [Amerasia Technology, Inc., Westlake Village, CA (United States)

    1995-10-01

    This paper describes research on a fast gas chromatography (GC) vapor analysis system which uses a new type of Surface Acoustic Wave detector technology to characterize organic contamination in soil and groundwater. The project was sponsored by the Department of Energy, Morgantown Energy Technology Center. The instrument was field tested at the Savannah River Plant.

  9. [Study on supercritical CO2 extraction of xiaoyaosan and its GC-MS fingerprint].

    Science.gov (United States)

    Zuo, Ya-Mei; Tian, Jun-Sheng; Guo, Xiao-Qing; Zhou, Yu-Zhi; Gao, Xiao-Xia; Qin, Xue-Mei

    2014-02-01

    To determine the optimum conditions of supercritical CO2 extraction of Xiaoyaosan, and establish its fingerprint by gas chromatography-mass spectrometry (GC-MS), the yield of extract were investigated, an orthogonal test was used to quantify the effects of extraction temperature, pressure, CO2 flow rate and time, and fingerprint analysis of different batches of extracts were by GC-MS. The optimal extraction conditions were determined as follows: extraction pressure 20 MPa, extraction temperature 50 degrees C, CO2 flow rate 25 kg x h(-1), extraction time 3 h, and average yield 2.2%. The GC-MS fingerprint was established and 27 common peaks were found, whose contents add up to 81.89% of the total peak area. Among them, 21 compounds were identified, accounting for 53.20% of the total extract. The extraction process is reasonable and favorable for industrial production. The GC-MS method is accurate, reliable, reproducible, and can be used for quality control of supercritical CO2 extract from Xiaoyaosan.

  10. Identification and Determination of Nicorandil and its Degradation Products by HPLC and GC/MS

    Institute of Scientific and Technical Information of China (English)

    Zhong Zhou CHENG; Ze Hui JIA; Yan CHEN; Li Ying CHEN; Hua LI

    2006-01-01

    A rapid and sensitive HPLC-DAD method is developed for simultaneous determination of nicorandil and its degradation products, N-(2-hydroxyethyl) nicotinamide, nitrate ion and nicotinic acid, using nicotinamide (NT) as internal standard, at wavelength 204 nm. Nicotinic acid is identified by HPLC and GC/MS. The method can also be applied to study kinetic of degradation processes of nicorandil in storage.

  11. Photocatalytic oxidation of aromatic amines using MnO2@g-C3N4

    Data.gov (United States)

    U.S. Environmental Protection Agency — An efficient and direct oxidation of aromatic amines to aromatic azo-compounds has been achieved using a MnO2@g-C3N4 catalyst under visible light as a source of...

  12. Identification and quantification of isoquinoline alkaloids in the genus Sarcocapnos by GC-MS.

    Science.gov (United States)

    Suau, R; Cabezudo, B; Valpuesta, M; Posadas, N; Diaz, A; Torres, G

    2005-01-01

    Six cularine alkaloids, cularicine, O-methylcularicine, celtisine, cularidine, cularine and celtine, three isocularine alkaloids, sarcophylline, sarcocapnine and sarcocapnidine, and five non-cularine alkaloids, glaucine, protopine, ribasine, dihydrosanguinarine and chelidonine, were identified and quantified by GC-MS in nine taxa of the genus Sarcocapnos (Fumariaceae). The chemotaxonomic significance of the results is discussed.

  13. Identification of VX type nerve agents using cryodeposition GC-FTIR

    Science.gov (United States)

    Söderström, Martin T.

    1998-06-01

    Analysis of VX type nerve agents with a gas chromatography-Fourier transform infrared spectroscopy (GC-FTIR) system using cryodeposition of the eluents is described. An interpretation system based on comparison of characteristic spectral features to the features in reference spectra, is used to characterize side chains in VX type nerve agents.

  14. Application of LPME/GC-ECD for determination of PCP in water

    Institute of Scientific and Technical Information of China (English)

    李萍; 刘俊新

    2003-01-01

    Liquid-phase microextraction (LPME) followed by gas chromatography (GC) coupled with an electron capture detector (ECD) was applied for the analysis of pentachlorophenol (PCP) in aqueous samples. After alkalization with Na2CO3 solution, PCP was acetylated with acetic anhydride. The pentachlorophenyl acetate derivative was then extracted with n-hexane by LPME. 1.5 μL organic drop exposed to the aqueous sample solution at 15℃ for 5 min, stirring rate at 100 r/min was chosen as the optimum extraction condition. Under this condition, LPME provided a very simple, fast and solvent-less procedure to collect PCP from aqueous sample for GC determination. The linearity of LPME/GC-ECD for PCP in distilled water was investigated at the range of 2-200 μg/L with a coefficient of correlation 0.998. The repeatability of this method was determined at the level of 50 μg/L with the average of relative standard deviations (RSDs) 7%. Detection limit was obtained at less than 0.5 μg/L levels. When LPME/GC-ECD was applied to the determination of PCP in municipal sewage, the average of relative recoveries and RSDs were 70% and 6.5%, respectively.

  15. GC-MS Analysis of [gamma]-Hydroxybutyric Acid Analogs: A Forensic Chemistry Experiment

    Science.gov (United States)

    Henck, Colin; Nally, Luke

    2007-01-01

    An upper-division forensic chemistry experiment is described. It involves using glycolic acid and sodium glycolate as analogs of [gamma]-hydroxybutyric acid and its sodium salt. The experiment shows the use of silylation in GC-MS analysis and gives students the opportunity to work with a commonly used silylating reagent,…

  16. Development of a LSSVM-GC model for estimating the electrical conductivity of ionic liquids

    DEFF Research Database (Denmark)

    Gharagheizi, Farhad; Ilani-Kashkouli, Poorandokht; Sattari, Mehdi

    2014-01-01

    In this communication, an extensive set of 1077 experimental electrical conductivity data for 54 ionic liquids (ILs) was collected from 21 different literature sources. Using this dataset, a reliable least square support vector machine-group contribution (LSSVM-GC) model has been developed, which...

  17. Maximizing Chromatographic Information from Environmental Extracts by GCxGC-ToF-MS

    NARCIS (Netherlands)

    Skoczynska, E.M.; Korytar, P.; Boer, de J.

    2008-01-01

    Comprehensive two-dimensional gas chromatography (GCxGC) coupled with a time-of-flight (ToF) detector allows the separation of many constituents of previously unresolved complex mixtures (UCM) of contaminants in sediment samples. In addition to the powerful chromatographic resolution, automated mass

  18. The ν2GC simulations: Quantifying the dark side of the universe in the Planck cosmology

    Science.gov (United States)

    Ishiyama, Tomoaki; Enoki, Motohiro; Kobayashi, Masakazu A. R.; Makiya, Ryu; Nagashima, Masahiro; Oogi, Taira

    2015-08-01

    We present the evolution of dark matter halos in six large cosmological N-body simulations, called the ν2GC (New Numerical Galaxy Catalog) simulations on the basis of the ΛCDM cosmology consistent with observational results obtained with the Planck satellite. The largest simulation consists of 81923 (550 billion) dark matter particles in a box of 1.12 h-1 Gpc (a mass resolution of 2.20 × 108 h-1 M⊙). Among simulations utilizing boxes larger than 1 h-1 Gpc, our simulation yields the highest resolution simulation that has ever been achieved. A ν2GC simulation with the smallest box consists of eight billion particles in a box of 70 h-1 Mpc (a mass resolution of 3.44 × 106 h-1 M⊙). These simulations can follow the evolution of halos over masses of eight orders of magnitude, from small dwarf galaxies to massive clusters. Using the unprecedentedly high resolution and powerful statistics of the ν2GC simulations, we provide statistical results of the halo mass function, mass accretion rate, formation redshift, and merger statistics, and present accurate-fitting functions for the Planck cosmology. By combining the ν2GC simulations with our new semianalytic galaxy formation model, we are able to prepare mock catalogs of galaxies and active galactic nuclei, which will be publicly available in the near future.

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

    Energy Technology Data Exchange (ETDEWEB)

    Guidotti, M.; Ravaioli, G. [Presidio Multizonale di Prevenzione, Rieti (Italy). Settore Ambiente

    1999-12-01

    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.

  20. Identification of volatile degradants in formulations containing sesame oil using SPME/GC/MS.

    Science.gov (United States)

    Chen, Wencan; Zhou, Pengzu; Wong-Moon, Kirby C; Cauchon, Nina S

    2007-06-28

    Solid-phase microextraction (SPME), in combination with gas chromatography/mass spectrometry (GC/MS), was used to identify an unknown degradant observed during stability studies of a pharmaceutical formulation containing sesame oil. SPME is a solvent-less, rapid, sensitive, and inexpensive extraction method that minimizes sample preparation. SPME combined with GC is a widely used technique in certain fields, such as food, environmental analysis, forensics, and consumer products, but has only rarely been used for the analysis of pharmaceutical formulations. Hexanal, octanal, 2-octenal, 2-decenal, 2-undecenal, and 2,4-decadienal can be detected and identified by GC/MS, but they cannot be detected by LC/MS due to their volatility and low ionization efficiency under atmospheric pressure ionization conditions. Combining the MS data from the GC/MS with LC/DAD data resulted in the identification of the unknown degradant in the formulation as 2,4-decadienal. The presence of this and other aldehydes was attributed to the oxidative degradation of the unsaturated fatty-acid component in vegetable oils.

  1. Determination of Cinnamaldehyde in Cinnamon by SPME-GC-MS: An Instrumental Analysis Experiment

    Science.gov (United States)

    Wang, Yimin; Ocariz, Jessica; Hammersand, Jennifer; MacDonald, Evan; Bartczak, Ashley; Kero, Frank; Young, Vaneica Y.; Williams, Kathryn R.

    2008-01-01

    Students analyze "trans"-cinnamaldehyde in commercial cinnamon using solid-phase microextraction and GC-MS with ethyl benzoate as the internal standard. Aside from the instrumentation, the experiment utilizes readily available low hazard materials and can be completed within one four-hour laboratory period. (Contains 2 figures.)

  2. Selecting parameters for the environmental interpretation of peat molecular chemistry - A pyrolysis-GC-MS study

    NARCIS (Netherlands)

    Schellekens, J.F.P.; Buurman, P.; Pontevedra Pombal, X.

    2009-01-01

    A number of samples from a deep peat bog in Tierra del Fuego were analyzed using pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) in order to extract parameters that might be used to interpret the peat chemistry in terms of vegetation change, anaerobic and aerobic decomposition, and fire in

  3. Measurement of selected halogenated contaminants in human serum and milk using GCxGC-IDTOFMS

    Energy Technology Data Exchange (ETDEWEB)

    Focant, J. [Liege Univ. (Belgium); Sjoedin, A.; Turner, W.; Patterson, D. [Centers for Disease Control and Prevention, Atlanta, GA (United States)

    2004-09-15

    A new method using comprehensive two-dimensional gas chromatography and isotope dilution time-of-flight mass spectrometry (GCxGC-IDTOFMS) for the simultaneous measurement of selected polychlorinated biphenyls (PCBs), organochlorine pesticides (OCPs), and brominated flame retardants (BFRs) is presented. Conversely to reference methods based on classical GC-MS, a single injection of the extract containing all species of interest conducts to accurate identification and quantification. GCxGC ensures the chromatographic separation of most compounds and TOFMS allows mass spectral deconvolution of co-eluting compounds as well as the use of {sup 13}C-labeled internal standards for quantification. Isotope ratio measurements of the most intense ions for both natives and labels ensure the required specificity. Potentially interfering matrix compounds are usually kept away from the compounds to be measured in the chromatographic space. The use of this new method with automated sample preparation procedures developed at the Centers for Disease Control and Prevention (CDC) for the analysis of human serum and milk compared favorably to conventional isotope-dilution one-dimensional gas chromatography-high resolution mass spectrometry (GC-IDHRMS) for the different sample pools that were tested.

  4. Comparison of GC-MS and FTIR methods for quantifying naphthenic acids in water samples.

    Science.gov (United States)

    Scott, Angela C; Young, Rozlyn F; Fedorak, Phillip M

    2008-11-01

    The extraction of bitumen from the oil sands in Canada releases toxic naphthenic acids into the process-affected waters. The development of an ideal analytical method for quantifying naphthenic acids (general formula C(n)H(2n+Z)O(2)) has been impeded by the complexity of these mixtures and the challenges of differentiating naphthenic acids from other naturally-occurring organic acids. The oil sands industry standard FTIR method was compared with a newly-developed GC-MS method. Naphthenic acids concentrations were measured in extracts of surface and ground waters from locations within the vicinity of and away from the oil sands deposits and in extracts of process-affected waters. In all but one case, FTIR measurements of naphthenic acids concentrations were greater than those determined by GC-MS. The detection limit of the GC-MS method was 0.01 mg L(-1) compared to 1 mg L(-1) for the FTIR method. The results indicated that the GC-MS method is more selective for naphthenic acids, and that the FTIR method overestimates their concentrations.

  5. Rapid Py-GC/MS assessment of the structural alterations of lignins in genetically modified plants

    NARCIS (Netherlands)

    Rencoret, Jorge; Del Río, José Carlos; Nierop, Klaas G J|info:eu-repo/dai/nl/182329895; Gutiérrez, Ana; Ralph, John

    Genetic modifications for perturbing the lignin pathway in three different species of angiosperm plants, including non-woody (Arabidopsis and alfalfa) and woody (poplar) plants, were readily evaluated by analytical pyrolysis coupled to gas chromatography-mass spectrometry (Py-GC/MS). Pyrolysis

  6. 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…

  7. GC-MS Analysis of [gamma]-Hydroxybutyric Acid Analogs: A Forensic Chemistry Experiment

    Science.gov (United States)

    Henck, Colin; Nally, Luke

    2007-01-01

    An upper-division forensic chemistry experiment is described. It involves using glycolic acid and sodium glycolate as analogs of [gamma]-hydroxybutyric acid and its sodium salt. The experiment shows the use of silylation in GC-MS analysis and gives students the opportunity to work with a commonly used silylating reagent,…

  8. GC-O与GC-MS结合鉴定天然乳脂风味中的特征致香成分%The identification of specific aroma in flavor of natural milk fat using the cooperation of GC-O and GC-MS

    Institute of Scientific and Technical Information of China (English)

    侯园园; 王兴国; 刘元法

    2008-01-01

    利用GC-O与GC-MS结合鉴定天然乳脂风味中的特征致香成分,鉴定出有十种物质对于乳脂的风味是有较大贡献的,分别是辛醛(水果味)、2-壬酮(酒味)、辛酸乙酯(奶油味)、丁酸(奶油味,有点酸)、戊酸(奶油味)、2-十三酮(木香味)、己酸(奶油味,有点酸)、庚酸(奶油味,有点酸)、辛酸(花香味,有点酒味)、还有一种未知化合物(具有奶油味和酒味).实验证明,GC-O与GC-MS结合的方法来分析天然乳脂的风味是非常敏锐和高效的.

  9. 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...

  10. 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...

  11. Methods for sequencing GC-rich and CCT repeat DNA templates

    Science.gov (United States)

    Robinson, Donna L.

    2007-02-20

    The present invention is directed to a PCR-based method of cycle sequencing DNA and other polynucleotide sequences having high CG content and regions of high GC content, and includes for example DNA strands with a high Cytosine and/or Guanosine content and repeated motifs such as CCT repeats.

  12. 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.

  13. Genome-wide analysis of Epstein-Barr virus (EBV) isolated from EBV-associated gastric carcinoma (EBVaGC).

    Science.gov (United States)

    Liu, Ying; Yang, Wenjun; Pan, Yaqi; Ji, Jiafu; Lu, Zheming; Ke, Yang

    2016-01-26

    Epstein-Barr virus (EBV) is linked to the development of a variety of malignancies, including EBV-associated gastric carcinoma (EBVaGC). In this study, EBVaGC was detected in 15 (7.3%) of 206 GC cases. To identify the EBV genomic variation, EBV genomic sequences isolated from 9 EBVaGC biopsy specimens were successfully retrieved, designated EBVaGC1 to EBVaGC9. By comparative analysis of these strains with another 6 completely sequenced EBV strains, EBV-wild type, B95-8, AG876, GD1, GD2, and HKNPC1, it was demonstrated that EBVaGC1 to 9 were most closely related to the GD1 strain. Phylogenetic analysis of the GC biopsy specimen-derived EBV (GC-EBV) genomes was subsequently performed to assess their genomic diversity and it exhibited the greatest divergence from the type 2 strain, AG876. Compared with the reference EBV strain GD1, they harbored 961 variations in total, including 919 substitutions, 23 insertions, and 19 deletions. Single nucleotide polymorphism (SNP) density varied substantially across all known open reading frames and was highest in latency-associated genes. Moreover, we identified 2 interstrain recombinants at the EBNA1 locus, which provided a further mechanism for the generation of diversity. Some T-cell epitope sequences in EBNA1 and LMP2A genes showed extensive variation across strains, which implied their importance in the development of vaccines and T-cell therapy. In conclusion, we reported the first genome-wide view of sequence variation of EBV isolated from primary EBVaGC biopsy specimens, which might serve as an effective method for further understanding the genomic variations contribute to EBVaGC carcinogenesis and treatment.

  14. 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.

  15. 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.

  16. Genome Size and GC Content Evolution of Festuca: Ancestral Expansion and Subsequent Reduction

    Science.gov (United States)

    Šmarda, Petr; Bureš, Petr; Horová, Lucie; Foggi, Bruno; Rossi, Graziano

    2008-01-01

    Background and Aims Plant evolution is well known to be frequently associated with remarkable changes in genome size and composition; however, the knowledge of long-term evolutionary dynamics of these processes still remains very limited. Here a study is made of the fine dynamics of quantitative genome evolution in Festuca (fescue), the largest genus in Poaceae (grasses). Methods Using flow cytometry (PI, DAPI), measurements were made of DNA content (2C-value), monoploid genome size (Cx-value), average chromosome size (C/n-value) and cytosine + guanine (GC) content of 101 Festuca taxa and 14 of their close relatives. The results were compared with the existing phylogeny based on ITS and trnL-F sequences. Key Results The divergence of the fescue lineage from related Poeae was predated by about a 2-fold monoploid genome and chromosome size enlargement, and apparent GC content enrichment. The backward reduction of these parameters, running parallel in both main evolutionary lineages of fine-leaved and broad-leaved fescues, appears to diverge among the existing species groups. The most dramatic reductions are associated with the most recently and rapidly evolving groups which, in combination with recent intraspecific genome size variability, indicate that the reduction process is probably ongoing and evolutionarily young. This dynamics may be a consequence of GC-rich retrotransposon proliferation and removal. Polyploids derived from parents with a large genome size and high GC content (mostly allopolyploids) had smaller Cx- and C/n-values and only slightly deviated from parental GC content, whereas polyploids derived from parents with small genome and low GC content (mostly autopolyploids) generally had a markedly increased GC content and slightly higher Cx- and C/n-values. Conclusions The present study indicates the high potential of general quantitative characters of the genome for understanding the long-term processes of genome evolution, testing evolutionary

  17. 川芎挥发油的GC-MS指纹图谱研究%Study on the Fingerprints of Volatile Oil from Ligusticum chuanxiong by GC-MS

    Institute of Scientific and Technical Information of China (English)

    刘洪玲; 于良生; 纪恒胜; 金宏; 孙伟

    2012-01-01

    OBJECTIVE: To establish GC-MS fingerprints of volatile oil from Ligusticum chuanxiong. METHODS: The volatile oil was extracted from L. chuanxiong by supercritical CO2 fluid extraction. The chromatographic fingerprints was established by GC-MS, SGE-30QC 3/AC 225 fused-silica capillary (30 m×0.32 mm×0.25 μm) column, injector temperature of 280 ℃, temperature programming, carrier gas of helium, injection volume of 1 μL, split ratio of 10 :1, ion source of El, ion source temperature of 200℃, interface temperature of 250℃ , detection voltage of 0.8 kV, scanning range of ion mass from 30 amu to 400 amu. The similarity was calculated with "TCM fingerprint computer aided similarity evaluation sofetware". RESULTS: The reproducibility, accuracy and stability of the method were very good in the tests (all RSD<3%); the volatile oil fromi. chuanxiong mainly included α-pinene, carotol, Chuanxiong lactone, ligustilide and palmitic acid. They made up of GC-MS fingerprints of volatile oil from L. chuanxiong; the similarity of volatile oil from 10 batches of L. chuanxiong was more than 0.92. CONCLUSION: The study can provide reference for quality control of L. chuanxiong.%目的:建立川芎挥发油的气相色谱-质谱(GC-MS)指纹图谱.方法:采用超临界CO2流体萃取法提取川芎挥发油,用GC-MS联用技术对其进行指纹图谱研究,色谱柱为SGE-30QC 3/AC 225弹性石英毛细管柱(30 m×0.32 mm×0.25μm),进样口温度为280℃,程序升温,载气为氦气,进样量为1μL,分流比为10∶1;采用电子轰击离子源(EI),离子源温度为200℃,接口温度为250℃,检测电压为0.8 kV,质量扫描范围为30~400amu;并采用“中药指纹图谱计算机辅助相似度评价软件”计算相似度.结果:本方法有较好的重复性、精密度和稳定性(RSD均<3%);川芎挥发油主要含有α-蒎烯、胡萝卜烯醇、川芎内酯、藁本内酯、棕榈酸,这5种成分构成了川芎挥发油GC-MS特征指纹图谱;10

  18. GC-biased gene conversion impacts ribosomal DNA evolution in vertebrates, angiosperms, and other eukaryotes.

    Science.gov (United States)

    Escobar, Juan S; Glémin, Sylvain; Galtier, Nicolas

    2011-09-01

    Ribosomal DNA (rDNA) is one of the most conserved genes in eukaryotes. The multiples copies of rDNA in the genome evolve in a concerted manner, through unequal crossing over and/or gene conversion, two mechanisms related to homologous recombination. Recombination increases local GC content in several organisms through a process known as GC-biased gene conversion (gBGC). gBGC has been well characterized in mammals, birds, and grasses, but its phylogenetic distribution across the tree of life is poorly understood. Here, we test the hypothesis that recombination affects the evolution of base composition in 18S rDNA and examine the reliability of this thoroughly studied molecule as a marker of gBGC in eukaryotes. Phylogenetic analyses of 18S rDNA in vertebrates and angiosperms reveal significant heterogeneity in the evolution of base composition across both groups. Mammals, birds, and grasses experience increases in the GC content of the 18S rDNA, consistent with previous genome-wide analyses. In addition, we observe increased GC contents in Ostariophysi ray-finned fishes and commelinid monocots (i.e., the clade including grasses), suggesting that the genomes of these two groups have been affected by gBGC. Polymorphism analyses in rDNA confirm that gBGC, not mutation bias, is the most plausible explanation for these patterns. We also find that helix and loop sites of the secondary structure of ribosomal RNA do not evolve at the same pace: loops evolve faster than helices, whereas helices are GC richer than loops. We extend analyses to major lineages of eukaryotes and suggest that gBGC might have also affected base composition in Giardia (Diplomonadina), nudibranch gastropods (Mollusca), and Asterozoa (Echinodermata).

  19. Combined analysis of the essential oil of Chenopodium ambrosioides by GC, GC-MS and 13C-NMR spectroscopy: quantitative determination of ascaridole, a heat-sensitive compound.

    Science.gov (United States)

    Cavalli, Jean-François; Tomi, Félix; Bernardini, Antoine-François; Casanova, Joseph

    2004-01-01

    A commercial sample of the essential oil of Chenopodium ambrosioides L. from Madagascar was analysed by GC, GC-MS and 13C-NMR. By GC analysis, the major constituents were found to be ascaridole (1) (41.8%), isoascaridole (2) (18.1%), p-cymene (16.2%), alpha-terpinene (9.7%) and limonene (3.8%). However, ascaridole undergoes a partial thermal isomerisation to 2 and hence the amount of 1 is under-estimated by GC analysis. The actual contents of 1 and 2 (55.3 and 4.6%, respectively) were obtained following combined analysis of the sample by GC and 13C-NMR. Several hydroxy- and polyhydroxy-menthanes were identified by 13C-NMR.

  20. Analysis of Dissolved Organic Contaminants in Yeast Wastewater by GC-MS%酵母废水中可溶性有机物的GC-MS分析

    Institute of Scientific and Technical Information of China (English)

    刘秀英; 周旋; 周春芳

    2008-01-01

    随着酵母工业的快速发展,酵母废水对环境的污染程度日趋严重,已成为制约酵母企业发展的瓶颈.当前,废水中有机污染物的污染程度主要以综合指标五日生化需氧量(BOD5)和化学需氧量(COD)来表述.这些综合指标并不能客观地反映废水中有机污染物的组成与含量.用毛细管气相色谱一质谱(GC-MS)联用仪能快速、灵敏地分析废水中的有机污染物.本文首次将酵母废水中可溶性有机物分为可吹脱有机物、液液萃取(LLE)可萃取有机物等,分别采用吹脱捕集-GC-MS、LLE-GC-MS等方法进行分析,确定了该废水中可溶性有机污染物的主要种类.其中,碳氢化合物、酯、芳香烃、醇、有机羧酸和杂环化合物较高,酮与醛含量较低.

  1. GC-MS测定苯并三唑类紫外线吸收剂%Determination of benzotriazole ultraviolet absorber in textiles by GC-MS

    Institute of Scientific and Technical Information of China (English)

    薛建平

    2013-01-01

    通过优化萃取方法和仪器条件,建立了气相色谱-质谱法(GC-MS)测定纺织品中2-(2′-羟基-3′,5′-二叔丁基苯基)-苯并三唑的含量,并分析了该物质的质谱图和主要离子的可能裂解途径.结果表明,该方法的平均回收率为90.3%~103.0%,相对标准偏差小于10%,方法检测限可达0.05 mg/kg.该方法操作简单可靠,适用于纺织品中2-(2′-羟基-3′,5′-二叔丁基苯基)-苯并三唑含量的日常检测.%A gas chromatography/mass spectrometry (GC-MS) method for determination of 2-(2'-hydroxy-3',5'-di-tert-butyl-phenyl) benzotriazole in textiles is developed by improving the extraction method and GC-MS conditions.Mass spectra of the substance and the possible fragmentation pathway of main ion are analyzed.The results show that, satisfactory recoveries are from 90.3% to 103.0%, relative standard deviation is less than 10% and method detection limit is 0.05 mg/kg.The method is simple and reliable, and can meet the requirements of determination of 2-(2'-hydroxy-3',5'-di-tert-butylphenyl)benzotriazole in textiles.

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

    Science.gov (United States)

    Du, Xiaofen; Plotto, Anne; Baldwin, Elizabeth; Rouseff, Russell

    2011-12-14

    Most strawberry flavor studies have examined berries grown in temperate regions with long summer days. Few studies have examined berries harvested in winter months from subtropical regions with shorter photoperiods. Fruits harvested in February and March from two strawberry cultivars, 'Strawberry Festival' and 'Florida Radiance', were examined. Thirty odor active compounds were detected using time-intensity GC-O. Twenty-nine were identified. The major odor active volatiles in both cultivars were 2,5-dimethyl-4-methoxy-3(2H)-furanone (DMMF), 2,5-dimethyl-4-hydroxy-3(2H)-furanone (DMHF), methyl butanoate, γ-decalactone, unknown (grassy, LRI 1362, wax), (E)-2-hexenal, linalool, (E,Z)-2,6-nonadienal, geraniol, butanoic acid, methyl 2-methylbutanoate, and ethyl hexanoate. Over 90 volatiles were identified and 54 quantified using GC-MS including 33 esters, 6 alcohols, 5 acids, 3 aldehydes, 3 lactones, 2 ketones, and 2 furanones. Odor activity values (OAVs) were determined for 46 volatiles, of which 22 had OAV > 1. The highest OAVs for 'Strawberry Festival' were ethyl butanoate (461), DMHF (424), methyl butanoate (358), and linalool (102). A 14-member trained panel evaluated quartered fruit using quantitative descriptive analysis to quantify seven sensory attributes. Sensory "strawberry flavor" scores were positively correlated with sensory "sweetness" (R(2) = 0.83) as well as GC-MS methyl 3-methylbutanoate (R(2) = 0.90) and ethyl butanoate (R(2) = 0.96). These cultivars lacked methyl anthranilate and possessed an aroma pattern different from summer-grown strawberries.

  3. GC-MS Analysis of Volatile Constituents of Lasiosphaera fenzlii%脱皮马勃挥发性成分的GC-MS分析

    Institute of Scientific and Technical Information of China (English)

    徐淑楠; 司攀; 高玉琼; 刘建华; 杨广成

    2012-01-01

    Objective: To provide the foundation for reasonable utilization by analyzing the volatile constituents of Lasiosphaera fenzlii. Method: The volatile oil was extracted from L. fenzlii by team distillation. The chemical constituents were analyzed by GC-MS. Result: Eighty nine compounds were separated and forty nine of them were identified, which accounted for 70.713% of all the volatile oil. The major components were acenaphthylene (16.836%), ar-curcumene (7.800%), caryophyllene oxide (5.448%), beta-tumerone (2. 814% ) , beta-cadinene (2. 771% ). Conclusion: This paper reported, for the first time, the composition of volatile oils of L. fenzlii by GC-MS.%目的:分析脱皮马勃的挥发性成分,为脱皮马勃的开发利用提供实验依据.方法:利用水蒸气蒸馏法提取脱皮马勃(Lasiosphaera fenzlii Reich)挥发油,采用气相色谱-质谱联用(GC-MS)技术对挥发油进行分析.结果:共分离出89个化学成分,鉴别出49个化学成分,占挥发油总量的70.713%,其主要成分为苊(16.836%);芳-姜黄烯(7.800%);丁香烯环氧物(5.448%);β-姜黄酮(2.814%);β-杜松萜烯(2.771%).结论:首次采用气相色谱-质谱联用法对脱皮马勃的挥发性成分进行研究.

  4. Analysis of biofluids for gamma-hydroxybutyrate (GHB) and gamma-butyrolactone (GBL) by headspace GC-FID and GC-MS.

    Science.gov (United States)

    LeBeau, M A; Montgomery, M A; Miller, M L; Burmeister, S G

    2000-09-01

    The past few years have seen a dramatic increase in the abuse of gamma-hydroxybutyrate (GHB) and gamma-butyrolactone (GBL) in the United States. The abuse stems primarily from their euphoric and sedative properties, but these substances are also misused by bodybuilders as steroid alternatives. Recently there has been an alarming increase in the use of GHB and GBL in crimes of drug-facilitated sexual assault. A rapid and sensitive procedure was developed for the analysis of biofluids containing GHB and GBL. Two separate aliquots of a biological specimen were spiked with an alpha-methylene-gamma-butyrolactone internal standard solution. One of the aliquots was treated with concentrated sulfuric acid for cyclization of GHB to GBL and the other remained untreated. Both aliquots were extracted with methylene chloride and concentrated. Extracts were screened using automated headspace gas chromatography-flame-ionization detection (GC-FID). Qualitative findings were quantitated and confirmed in a manner similar to the GC-FID procedure with some modifications. A calibrated solution of GHB-d6 (or GBL-d6, when warranted) was added to the aliquots at a concentration approximating the level determined by the GC-FID screen. The extraction was as described with conversion of GHB to GBL, but analysis was by full-scan gas chromatography-mass spectrometry (El). Quantitation was performed by comparison of the area of the molecular ion of the parent drug (m/z 86) to that of the calibrated deuterated analogue (m/z 92). This analytical procedure allows for the rapid detection of GHB and GBL in biofluids. Its sensitivity has proven useful for the toxicological investigation of cases of drug-facilitated sexual assault.

  5. GC-MS Analysis of Volatile Components of Marsdenia tenacissima%GC-MS分析测定乌骨藤挥发性成分

    Institute of Scientific and Technical Information of China (English)

    李浡; 王晓杰; 李双石; 曹奇光; 谢国莉

    2012-01-01

    Objective: To study volatile components of Marsdenia tenocissima. Method; Soxhlet extraction method with petroleum ether and ethyl ether were accompanied with gas chromatography mass spectrometry (GC-MS) to analyze the volatile components respectively. Result; 24 compounds identified by GC-MS with petroleum ether accounted for 55. 43% of all volatile components; fatty acids were 75. 10% and alkanes were 11.91% ; 24 compounds identified with ethyl ether accounted for 60.43% ; fatty acids were 38.98% and alkanes were 39. 27% . Conclusion; The study provides useful data for further analysis of components of Marsdenia tenocissima.%目的:研究乌骨藤挥发性成分.方法:采用石油醚和乙醚作为溶剂,用索氏提取法提取挥发性成分,气相色谱-质谱联用技术(GC-MS)鉴定其化学成分.结果:采用石油醚作为溶剂鉴定出24种化合物,占挥发成分的55.43%,其中脂肪酸占75.10%,烷烃类占11.91%;乙醚作为溶剂提取鉴定出24种化合物,占60.43%,脂肪酸占38.98%,烷烃类占39.27%.结论:测定了乌骨藤挥发性成分,为进一步研究乌骨藤成分提供了理论依据.

  6. Analysis of the composition of Brazilian propolis extracts by chromatography and evaluation of their in vitro activity against gram-positive bacteria Análise da composição de extratos de própolis brasileiros por cromatografia e avaliação de sua atividade in vitro sobre bactérias

    Directory of Open Access Journals (Sweden)

    Alexandra C. H. F. Sawaya

    2004-06-01

    Full Text Available Brazilian propolis from São Paulo state was submitted to extraction using several solvents, resulting in extracts with different composition. These extracts were submitted to Thin Layer Chromatography (TLC. Bioauthographic analysis of the TLC plates identified fractions with inhibitory activity, which were then analysed by High Performance Liquid Chromatography (HPLC. In vitro assays, commonly used to evaluate the activity of propolis against Gram-positive bacteria, were compared to determine which rendered the most consistent results. The bactericidal activity of these extracts were analysed by Serial Dilution in Tubes and Agar Plate Diffusion. Serial Dilution in Tubes obtained the most consistent results, with the Minimal Bactericidal Concentration of the extracts ranging between 2.5 and 20.0 mg/mL, for the species of Gram-positive bacteria tested. The results of the Agar Plate Diffusion were directly proportional to the hydro-solubility of the extracts and did not evaluate their bactericidal activity correctly. The bactericidal activity of this sample of propolis was due to the combined effect of several components that were identified by HPLC and were best extracted using 50% ethanol as a solvent.Própolis brasileira, proveniente do estado de São Paulo, foi submetida à extração usando vários solventes, resultando em extratos com diferentes composições. Estes extratos foram submetidos à Cromatografia em Camada Delgada (CCD. Análise bioautográfica das placas de CCD permitiu identificar as frações com atividade antimicrobiana, que foram então analisadas por Cromatografia Líquida de Alta Eficiência (CLAE. Ensaios in vitro freqüentemente utilizados para avaliar a atividade de própolis frente a bactérias Gram-positivas foram comparados para determinar qual renderia os resultados mais consistentes. A atividade bactericida destes extratos foi analisada por Diluição Seriada em Tubos e por testes de Difusão em Agar. O método de

  7. Analysis of Cucurbita Moschata Duch Oil by GC - MS%南瓜籽油脂肪酸的GC-MS分析

    Institute of Scientific and Technical Information of China (English)

    王晓; 程传格; 马小来; 董富英; 刘建华

    2002-01-01

    用正已烷抽提南瓜籽,然后将样品进行皂化、甲酯化,以毛细管色谱-质谱联用法(GC-MS)测定了南瓜籽油的组成,共鉴定出12种成分,其中主要成分为亚油酸和油酸,其相对含量分别为38.60%和28.63%.

  8. 尿中MDMA和MDA的三氟乙酰化-GC/MS/MS分析法%Determination of MDA and MDMA by TFA Derivatization-GC/MS/MS

    Institute of Scientific and Technical Information of China (English)

    于晓娟; 李国平

    2009-01-01

    建立了尿中MDMA和MDA的、用环己烷提取的、三氟乙酸酐衍生化的、GC/MS/MS检测的分析方法.方法操作简便快速,检测MDMA最灵敏的检出限为4ng/mL,检测MDA最灵敏的检出限为2.0ng/mI.方法的回收率为73%-94%,具有较好的线性关系.

  9. Analysis of volatile components of Ocimum basilicum L. by GC/MS%GC-MS法测定罗勒中芳香成分

    Institute of Scientific and Technical Information of China (English)

    李建文; 陈贵林; 何洪巨

    2003-01-01

    通过"同时蒸馏-萃取"装置(SDE)提取药用植物罗勒中的挥发性物质,经GC-MS分析初步判定,罗勒中含有27种芳香性成分.用峰面积归一化法确定相对百分含量较多的化合物为β-芳樟醇、对烯丙基苯甲醚、丁子香酚、桉树脑.

  10. 毛细管GC-ECD测定环境样品中的PCBs%Determination of PCBs in environmental samples with capillary GC-ECD

    Institute of Scientific and Technical Information of China (English)

    周传光; 徐恒振; 马永安; 李洪; 姚子伟

    2000-01-01

    建立了毛细管柱GC-ECD测定海洋环境样品中的PCBs的分析方法,给出了PCBs和OCPs的Florisil柱层析的分离方法以及回收率,测定了国际互校样品和我国海洋环境样品中的PCBs.结果表明,本方法可用于海洋环境样品中PCBs的分析.

  11. Análise simultânea da mirtazapina e N-desmetilmirtazapina em plasma empregando a cromatografia líquida de alta eficiência Simultaneous analysis of mirtazapine and N-demethylmirtazapine in plasma by high-performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Ana Cecília Coragem Briguenti

    2005-12-01

    Full Text Available Para avaliação das propriedades farmacocinéticas e monitorização terapêutica da mirtazapina, antidepressivo recentemente introduzido no mercado e que vem sendo bastante utilizado, são necessários métodos de análise simples, sensíveis e seletivos. Sendo assim, a cromatografia líquida de alta eficiência com detecção por fluorescência foi empregada para o desenvolvimento de um método para análise simultânea da mirtazapina e de seu metabólito, N-desmetilmirtazapina, em plasma. Após extração líquido-líquido utilizando tolueno como solvente extrator, o fármaco, metabólito e padrão interno (metoprolol foram separados em coluna LiChrospher 100 RP-8 capeada, utilizando fase móvel composta por tampão fosfato de sódio, 0,1 mol/L, pH 3,5-acetonitrila (82:18, v/v. O método apresentou linearidade no intervalo de 2,5 a 500 ng/mL para ambos os compostos, com recuperações médias de 77 e 66% para a mirtazapina e demetilmirtazapina, respectivamente. Os limites de quantificação (2,5 ng/mL, precisão (CV < 15% e exatidão (erros relativos < 15% do método asseguram a sua aplicabilidade em estudos de disposição cinética e para o controle terapêutico da mirtazapina.

  12. 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.

  13. 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...

  14. Efeito da baixa temperatura noturna e do porta-enxerto na variação diurna das trocas gasosas e na atividade fotoquímica de laranjeira 'Val��ncia' Effects of low night temperature and rootstocks on diurnal variation of leaf gas exchange rates and photochemical activity of 'Valência' sweet orange plants

    Directory of Open Access Journals (Sweden)

    Daniela Favero São Pedro Machado

    2010-06-01

    Full Text Available A redução da fotossíntese durante o inverno pode ser induzida por noites frias, mesmo quando as condições durante o dia não são limitantes. Laranjais são formados com plantas enxertadas, sendo o porta-enxerto citrumeleiro 'Swingle' recomendado em áreas onde há ocorrência de baixas temperaturas. Todavia, os mecanismos fisiológicos pelos quais as plantas apresentam melhor crescimento e produção são pouco conhecidos. O objetivo deste estudo foi testar a hipótese de que o efeito da baixa temperatura noturna na fotossíntese de laranjeiras é dependente do porta-enxerto utilizado, com o citrumeleiro 'Swingle' (Citrus paradisi x Poncirus trifoliata induzindo maior tolerância ao frio noturno se comparado ao limoeiro 'Cravo' (Citrus limonia. Laranjeiras 'Valência' (Citrus sinensis com seis meses, cultivadas em sacolas plásticas (5 L, foram expostas por 12 h à temperatura noturna de 20 e 8 ºC. O tratamento térmico foi realizado em câmara de crescimento, sendo apenas a parte aérea das plantas expostas às distintas temperaturas. Medidas do curso diurno das trocas gasosas e da atividade fotoquímica foram realizadas em condições ambientais naturais. O resfriamento noturno causou maior redução da assimilação de CO², da condutância estomática e da transpiração em laranjeira 'Valência' sobre limoeiro 'Cravo' quando comparado às plantas sobre 'Swingle'. Após o tratamento de frio, as eficiências máxima (Fv/Fm e operacional (Fq'/Fm' do fotossistema II diminuíram nas plantas sobre 'Cravo' e mantiveram-se praticamente inalteradas nas plantas enxertadas em 'Swingle'. Portanto, o porta-enxerto 'Swingle' induziu maior eficiência fotossintética em condições de frio noturno às plantas de laranjeira 'Valência' quando comparado ao porta-enxerto 'Cravo'. A queda da assimilação de CO² em plantas resfriadas foi devida à menor condutância estomática e menor eficiência aparente de carboxilação, ou seja, resultante de

  15. Effect of Mn-Zn ferrite on apatite-wollastonite glass-ceramic (A-W GC).

    Science.gov (United States)

    Da Li, Guang; Zhou, Da Li; Pan, Tao Hua; Chen, Guo Sheng; Lin, Yun; Mao, Mao; Yan, Guo

    2009-08-01

    Magnetic bioactive glass-ceramics (M GC) were prepared by doping apatite-wollastonite glass-ceramic (A-W GC) with Mn-Zn ferrite. The effect of different contents of Mn-Zn ferrite on the phase structure, magnetic property and bioactivity of A-W GC was investigated. X-ray powder diffraction results showed that A-W GC exhibited apatite, fluorapatite and wollastonite as the main phases. The doping of Mn-Zn ferrite caused the formation of a new phase Zn(0.75)Mn(0.75)Fe(1.5)O(4) in M GC. The amount of this new phase increased with increasing content of Mn-Zn ferrite. Under a magnetic field of 7.96 x 10(5) A m(-1), the saturation magnetization of M GC increased from 4.63 to 9.7 A m(2) kg(-1), but the coercive forces of M GC decreased from 2.39 x 10(4) to 7.56 x 10(3) A m(-1) as the Mn-Zn ferrite content increased from 5% to 20% in the material. The bioactivity of samples was evaluated by soaking in simulated body fluid (SBF). The results showed that the doping of Mn-Zn ferrite decreased the bioactivity of A-W GC dramatically. It took 7 days for an apatite layer to form on the surface of A-W GC, while at least 30 days was needed for an apatite layer forming on the surface of M GC.

  16. Activation-dependent surface expression of gC1qR/p33 on human blood platelets.

    Science.gov (United States)

    Peerschke, Ellinor I B; Murphy, Tara K; Ghebrehiwet, Berhane

    2003-02-01

    GC1qR/p33 (gC1qR) is expressed by a variety of somatic and cultured cells, including blood platelets. It interacts with several cellular, viral, bacterial, and plasma proteins, suggesting a potential role in thrombosis, inflammation, and infection. Considerable controversy has surrounded the surface membrane localization of gC1qR, however, since its cDNA sequence does not predict a traditional membrane-anchoring domain, and bears a typical mitochondrial targeting sequence. The present study examined gC1qR expression on resting and activated human blood platelets using flow cytometry and confocal microscopy with two monoclonal antibodies, 74.5.2 and 60.11, directed against gC1qR C-terminal amino acids 204-218, and N-terminal amino acids 76-93, respectively. Unstimulated platelets reacted minimally with either antibody. In contrast, platelet activation with TRAP, epinephrine, or ADP produced markedly increased gC1qR expression as reflected by 74.5.2 binding but not 60.11 binding. Platelet activation was verified using PAC-1 and anti CD 62 antibodies. Whereas PAC-1 binding to activated platelets could be reversed following platelet incubation with PGE1, 74.5.2 binding remained unchanged, suggesting the sustained expression of gC1qR following platelet stimulation. The data further demonstrate that detection of cell surface gC1qR may be dependent on antibody specificity. The ability of gC1qR to bind proteins involved in complement, coagulation, and kinin systems, as well as viral and bacterial pathogens including S. aureus protein A, supports the hypothesis that gC1qR expressed on activated platelets may contribute directly to thrombosis, inflammation, and endovascular infections.

  17. Chemical diversity of volatiles of Teucrium orientale L. var. orientale, var. puberulens, and var. glabrescens determined by simultaneous GC-FID and GC/MS techniques.

    Science.gov (United States)

    Ozek, Gulmira; Ozek, Temel; Dinç, Muhittin; Doǧu, Süleyman; Başer, Kemal H C

    2012-06-01

    In the present work, three varieties of Teucrium orientale, var. orientale, var. puberulens, and var. glabrescens, were collected and investigated for chemical composition of the oils. Subsequent gas chromatography (GC-FID) and gas chromatography coupled to mass spectrometry (GC/MS) revealed high abundance of sesquiterpenes in the essential oils analyzed. All the oils contained β-caryophyllene (22.6, 8.5, and 6.3%, resp.) and hexadecanoic acid (7.9, 12.8, and 13.1%). Germacrene D (24.6 and 33.4%) and bicyclogermacrene (6.7 and 8.5%) were found to be the main constituents of var. orientale and var. puberulens, respectively. The high percentages of β-cubebene (26.9%), α-cubebene (9.0%), and α-copaene (7.2%) established the diversity of var. glabrescens. The qualitative difference between the essential oils allowed the differentiation between the varieties in agreement with the morphological observations described in Flora of Turkey for each variety studied. In addition, a cluster analysis of twelve Teucrium taxa based on the essential-oil composition has been carried out. Hovewer, the analysis did not clearly reflect the infrageneric classification of the genus, it largely confirmed the relationships between the infraspecific taxa of Teucrium orientale and T. chamaedrys.

  18. Comparison of Three Solid Phase Materials for the Extraction of Carboxylic Acids from River Water Followed by 2D GC × GC-TOFMS Determination.

    Science.gov (United States)

    Bosire, G O; Ngila, J C; Parshotam, H

    2016-01-01

    The extraction and determination of aliphatic and aromatic carboxylic acids as well as their influence on the aromaticity and molecularity relationship of natural organic matter (NOM) in water are reported in this study. Three solid phase extraction (SPE) sorbents were used and their extraction efficiencies evaluated after chromatographic determinations (using gas chromatography with a time of flight mass spectrometer (GC × GC-TOFMS) and liquid chromatography with organic carbon detector (LC-OCD)). More than 42 carboxylic acids were identified in raw water from the Vaal River, which feeds the Lethabo Power Generation Station, South Africa, with cooling water. The aromatic carboxylic acid efficiency (28%) was achieved by using Strata™ X SPE while the highest aliphatic carboxylic acid efficiency (92.08%) was achieved by silica SPE. The hydrophobic nature of NOM in water depends on the nature of organic compounds in water, whether aromatic or aliphatic. The LC-OCD was used to assess the hydrophobicity levels of NOM as a function of these carboxylic acids in cooling water. The LC-OCD results showed that the aromatic nature of NOM in SPE filtered water followed the order Silica>Strata X>C-18. From the results, the hydrophobicity degree of the samples depended on the type and number of carboxylic acids that were removed by the SPE cartridges.

  19. GC-MS测定水中烷基汞的方法研究%Research on Determination of Alkyl Mercury in Water by GC-MS

    Institute of Scientific and Technical Information of China (English)

    李懿

    2012-01-01

    Alkyl mercury is an organic form of mercury in the nature and widely exists in the atmosphere, water and soil. The paper mainly introduced how to extract alkyl mercury in water by sulfhydryl cotton and determine it by GC-MS. Under the premises that the correctness of the test result is well ensured, the elution rate and elution device has been improved. The determination limit of this method is: Methyl mercury (MMC), 10 ng/L; Ethyl mercury (EMC), 10 ng/L.%烷基汞是汞在自然界中的一种有机物形态。广泛存在于大气环境、水环境及土壤环境中。文章主要介绍了如何使用巯基棉提取水中的烷基汞、并用GC-MS测定烷基汞。在保证测试结果准确的前提下,改进了洗脱速率和洗脱装置,本法的检出限为:甲基汞(MMC)10ng/L,乙基汞(EMC)10ng/L。

  20. GC-MS法测定纺织品中富马酸二甲酯%Determination of dimethyl fumarate in textiles by GC-MS method

    Institute of Scientific and Technical Information of China (English)

    王利; 符有辉; 陈立坚; 孙佩东; 白瑞娟; 张渝

    2016-01-01

    建立了测定纺织品中富马酸二甲酯(DMF)的气相色谱-质谱(GC-MS)的方法.样品采用乙酸乙酯超声萃取,经浓缩处理后,用自制装置净化富集,再经GC-MS测定.在优化条件下,采用外标法测定,线性范围为1.0~50.0 ng/mL,相关系数R2为0.998,检出限为LOQ为0.1 ng/mL (S/N=3),精密度RSD为3.34%(n=7),回收率为93.3%~103.1%,结果满意.该方法具有简单快速,灵敏准确,检出限低,可广泛应用于不同基质中富马酸二甲酯的测定.

  1. Study on Chemical Components of Essential Oil in Leaf of Beta vulgaris by GC-MS%甜菜叶挥发油成分GC-MS分析

    Institute of Scientific and Technical Information of China (English)

    于颖颖; 孙薇; 张晓叶; 曹晨; 孙琦; 孔德新; 刘银燕

    2012-01-01

    The chemical components of the essential oil from leaves of Beta vulgaris were analyzed by GC-MS metod. The essential oil was extracted from leaves of Beta vulgaris by steam distillation, and the amount of the components from the essential oil were determined by normalization method. The chemical components separated were identified by GC-MS method. There were 24 components consisted which were over 76.07% of the total essential oil. The method is reliable, stable and reproducible, and it can be applied to the analysis of chemical components in the essential oil extracted from chinese traditional medicine.%用气相色谱-质谱法对甜菜叶的挥发油进行化学成分分析.采用水蒸气蒸馏法从甜菜叶中提取挥发油,用归一化法测定其百分含量,并用气相色谱-质谱法对化学成分进行鉴定.共鉴定了24种成分,占挥发油总量的76.07%.本方法稳定可靠,重现性好,适合用于中药挥发油的化学成分分析.

  2. 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.

  3. GC-MS法测定涂料中的四溴双酚A%Determination of Tetrabromobisphenol A in Coatings by GC-MS Method

    Institute of Scientific and Technical Information of China (English)

    王云玉; 许志钦; 李丹; 郑建国; 周明辉; 刘莹峰; 肖前; 钟志光

    2014-01-01

    建立了GC-MS法检测涂料中四溴双酚A的分析方法,并对样品前处理条件和GC-MS分析条件进行优化.采用二氯甲烷-丙酮(1∶1)混合溶剂超声提取样品,萃取液经硅胶小柱净化,平行蒸发定量浓缩后采用气相色谱-质谱法测定,外标法定量.结果显示,四溴双酚A标准溶液在1~ 50 mg/L范围内线性关系良好,相关系数大于0.999;方法的定量下限(LOQ)为2 mg/kg,加标回收率为83.2%~104%,相对标准偏差(RSD,n=8)为2.6% ~4.7%.该方法操作简便、分析快速、结果准确,可满足涂料中四溴双酚A的定性定量分析要求.

  4. GC-MS Analysis of the Ethyl Ether Extract from Chinese Tuber indicum%国产松露乙醚提取物的GC-MS分析

    Institute of Scientific and Technical Information of China (English)

    蔡佳仲; 黄珍珍; 周娟; 李兆生; 胡英杰

    2012-01-01

    The chemical components of the ethyl ether extract from Tuber indicum originated in Yunnan of China, were analyzed by GC-MS. The results showed that 56 compounds accounting for 87. 39% of the extract were identified. The major constituents were identified as fatty acids (59.98% ). While alcohols (7.96% ) .esters (2.79% ) .aldehydes (2. 44% ) ,hydrocarbons (13.12% ) .and benzene derivatives (1.08% ) were co-existing components.%采用气相色谱-质谱(GC-MS)法分析我国云南产黑松露(Tuber indicum)乙醚提取物的化学成分.从中鉴定了56个化合物,占提取物总含量的87.37%,化合物组成特征:以脂肪酸类化合物为主,占59.98%,其中含亚油酸达26.51%;醇、酯、醛和烃类化合物分别占7.96%、2.79%、2.44%和13.12%,另外还含有少量的苯衍生物,占1.08%.

  5. Recent Progress in Photocatalysis of g-C3N4%g-C3N4光催化性能的研究进展

    Institute of Scientific and Technical Information of China (English)

    楚增勇; 原博; 颜廷楠

    2014-01-01

    利用光催化剂将太阳能转化为人类可以直接利用的能量,并用其解决地球资源的枯竭和生存环境的恶化是可再生清洁能源研究的一个方向。g-C3N4的独特结构赋予其良好的光催化性能,使之成为光催化领域的研究热点。目前在光催化领域, g-C3N4主要用于催化污染物分解、水解制氢制氧、有机合成及氧气还原。在实际应用中,为进一步提高 g-C3N4的光催化效果,科研工作者开发了多种改进方法,例如物理复合改性、化学掺杂改性、微观结构调整等。本文主要论述了 g-C3N4在光催化领域的应用以及光催化性能的改进方法,简要阐述了光催化和各种改进方法的机理,分析了目前g-C3N4在光催化领域面临的问题和挑战,展望了g-C3N4的应用前景。%Based on photocatalysts, solar energy can be converted into the energy that human can directly utilize, so as to solve the problems such as the depletion of the Earth’s resources and the deterioration of living environments. The unique structure of g-C3N4 gives it good photocatalytic performance. Its development and utilization have been a research hotspot recently. Generally, g-C3N4 can be used in the degradation of pollutions, hydrolysis to generate hy-drogen and oxygen, organic synthesis and oxygen reduction. However, in practical, its performance is not satisfactory. Researchers have tried many new methods to improve its photocatalysis, which include physical coupling modification, chemical bonding modification and microstructural modification. The review summarizes its photocatalysis and im-proving methods, briefly illustrates the catalysis mechanism, and presents detailed discussions and analysis on the ex-isting problems as well as potential applications.

  6. Analysis of the relationship between genomic GC Content and patterns of base usage, codon usage and amino acid usage in prokaryotes: similar GC content adopts similar compositional frequencies regardless of the phylogenetic lineages.

    Directory of Open Access Journals (Sweden)

    Hui-Qi Zhou

    Full Text Available The GC contents of 2670 prokaryotic genomes that belong to diverse phylogenetic lineages were analyzed in this paper. These genomes had GC contents that ranged from 13.5% to 74.9%. We analyzed the distance of base frequencies at the three codon positions, codon frequencies, and amino acid compositions across genomes with respect to the differences in the GC content of these prokaryotic species. We found that although the phylogenetic lineages were remote among some species, a similar genomic GC content forced them to adopt similar base usage patterns at the three codon positions, codon usage patterns, and amino acid usage patterns. Our work demonstrates that in prokaryotic genomes: a base usage, codon usage, and amino acid usage change with GC content with a linear correlation; b the distance of each usage has a linear correlation with the GC content difference; and c GC content is more essential than phylogenetic lineage in determining base usage, codon usage, and amino acid usage. This work is exceptional in that we adopted intuitively graphic methods for all analyses, and we used these analyses to examine as many as 2670 prokaryotes. We hope that this work is helpful for understanding common features in the organization of microbial genomes.

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

    Directory of Open Access Journals (Sweden)

    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

  8. Impact of the administration of a third-generation cephalosporin (3GC) to one-day-old chicks on the persistence of 3GC-resistant Escherichia coli in intestinal flora: An in vivo experiment.

    Science.gov (United States)

    Baron, Sandrine; Jouy, Eric; Touzain, Fabrice; Bougeard, Stéphanie; Larvor, Emeline; de Boisseson, Claire; Amelot, Michel; Keita, Alassane; Kempf, Isabelle

    2016-03-15

    The aim of the experiment was to evaluate under controlled conditions the impact on the excretion of 3GC-resistant Escherichia coli of the injection of one-day-old chicks with ceftiofur, a third-generation cephalosporin (3GC). Three isolators containing specific-pathogen-free chicks were used. In the first one, 20 birds were injected with ceftiofur then ten of them were orally inoculated with a weak inoculum of a 3GC-resistant E. coli field isolate containing an IncI1/ST3 plasmid encoding a blaCTX-M-1 beta-lactamase. The other chicks were kept as contact birds. None of the 20 birds in the second isolator were injected with ceftiofur, but ten of them were similarly inoculated with the 3GC-resistant strain and the others kept as contact birds. A third isolator contained ten non-injected, non-inoculated chicks. Fecal samples were collected regularly over one month and the E. coli isolated on non-supplemented media were characterized by antimicrobial agar dilution, detection of selected resistance genes and determination of phylogenetic group by PCR. The titers of 3GC-resistant E. coli in individual fecal samples were evaluated by culturing on 3GC-supplemented media. Results showed that the inoculated strain rapidly and abundantly colonized the inoculated and contact birds. The ceftiofur injection resulted in significantly higher percentages of 3GC-resistant E. coli isolates among the analyzed E. coli. No transfer of the 3GC-encoding plasmid to other isolates could be evidenced. In conclusion, these results highlight the dramatic capacity of 3GC-resistant E. coli to colonize and persist in chicks, and the selecting pressure imposed by the off-label use of ceftiofur.

  9. Microwave-assisted Extraction and GC-MS Analysis of Zanthoxylum Oil from Zanthoxylum bungeanum

    Directory of Open Access Journals (Sweden)

    Xiaoguang Wang

    2015-03-01

    Full Text Available The conditions for microwave-assisted extracting oil from Zanthoxylum bungeanum seeds were studied and its chemical composition was analyzed by GC-MS. The effects of extract medium, microwave power, time and ratio of liquid to solid on extraction yield of Zanthoxylum bungeanum oil were investigated, using an orthogonal array design. The experimental results showed that using petroleum ether as extract medium, microwave power 350 w, solid-to-solvent ratio 1:5 (g/mL, 60 sec, can obtained 7.85% of Zanthoxylum bungeanum oil. Thirty-three substances in Zanthoxylum bungeanum oil were authenticated by GC-MS, of which 33 were identified for the first time and its chemical composition was analyzed. Accounting for 97.82% of the total volatile compounds.

  10. Comparison of the results obtained by CALUX bioassay and GC-HRMS for different matrices

    Energy Technology Data Exchange (ETDEWEB)

    Carbonnelle, S.; Loco, J. van; Overmeire, I. van; Windal, I.; Wouwe, N. van; Goeyens, L. [Scientific Institute of Public Health, Brussels (Belgium); Cleuvenbergen, R. van [VITO, Mol (Belgium); Leeuwen, S. van [Netherlands Institute for Fisheries Research, Ijmuiden (Netherlands). Animal Science Group

    2004-09-15

    The reference method used to analyse polychlorodibenzo-p-dioxins (PCDDs), polychlorodibenzofurans (PCDFs) and dioxin-like polychlorinated biphenyls (dl-PCBs) is chromatography with high resolution mass spectrometry (GC-HRMS). It is interesting to check the suitability of screening methods that are faster and less expensive. Different matrices (milk, fish oil, chicken compound feed, pork tissue, chicken tissue, sepiolitic clay, whole egg and herring tissue) were analysed in the frame of the European project DIFFERENCE1. One of the aims of this project is to optimise screening methods. The CALUX bio-assay was one of the screening techniques used. This paper presents the extraction and purification methods used for the analyses. The CALUX results for dioxins and for dl-PCBs were compared to the corresponding GC-HRMS results.

  11. Analysis of Valproic Acid, Salicylic Acid and Ibuprofen in Whole Blood by GC-MS.

    Science.gov (United States)

    Stephenson, Jon B; Flater, Melanie L; Bain, Lisa T

    2016-10-01

    The Georgia Bureau of Investigation utilized a silylation method of analysis for low molecular weight carboxylic acids in the past. Due to the negative impact such derivatizations can have on gas chromatography-mass spectrometry (GC-MS) systems an alternative means of analysis was investigated. The described method is a whole blood solid phase extraction of valproic acid, salicylic acid and ibuprofen utilizing butylation for sensitivity and improved chromatography by GC-MS. The method produced a limit of detection and limit of quantitation at 1 mg/L for valproic acid, 2 mg/L for salicylic acid and 0.25 mg/L for ibuprofen. The variability based upon the middle of the calibration curve estimated to be 7% for valproic acid, 8% for salicylic acid and 11% for ibuprofen established upon a 95% confidence interval, with the highest percent coefficient of variation being 5.3% for ibuprofen.

  12. Preliminary phytochemical screening, Antibacterial potential and GC-MS analysis of two medicinal plant extracts.

    Science.gov (United States)

    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.

  13. GC-MS and spectrophotometric analysis of biodegradation of new disazo dye by Trametes versicolor.

    Science.gov (United States)

    Akdogan, H Ardag; Demircali, A; Aydemir, C; Pazarlioglu, N; Karci, F

    2011-01-01

    In this study; sub-tropical white rot fungi, Trametes versicolor was investigated for its ability to degrade 4-(3'-methyl-4'-(4"-nitrophenyl)azo- 1'H-pyrazol-5'-ylazo)-3-methyl- H-pyrazol-5-on in the mediums containing glucose and different concentrations of degrade dye in batch systems. This dye was synthetized at Pamukkale Universtiy of Organic Chemistry research laboratory. Samples were collected on 10 days, and was detected by Shimadzu UV-1600A spectrophotometry. Decolorization study showed that this disazo dye was removed by more than 70% in 10 days. Laccase enzyme activity was detected in samples and then last sample was analyzed by GC-MS. Metabolites weren't showed in GC-MS result. It was concluded that T. versicolor could achieve the biodegradation of this new disazo dye.

  14. Use of Gas Chromatography-Mass Spectrometry (GC-MS) in Nonscience Major Course Laboratory Experiments

    Science.gov (United States)

    Kostecka, Keith S.; Lerman, Zafra M.; Angelos, Sanford A.

    1996-06-01

    Gas chromatography-mass spectrometry (GC-MS) has been utilized with nonscience majors in the courses: "Modern Methods in Science: Discovering Molecular Secrets"; "The Extraordinary Chemistry of Ordinary Things"; "From Ozone to Oil Spills: Chemistry, the Environment and You"; and "Crime Lab Chemistry: Solving Crime through Analytical Chemistry". Our efforts have centered on introducing prospective science communicators (film, video, radio, television, and journalism majors) to science relative to their majors and personal interests. Quality lecture-discussion topics, "mystery"-based laboratory activities have assisted in introducing and/or explaining specific areas of chemistry that attempt to reduce fear of subject matter. Students have also used GC-MS, as a form of alternative assessment, in course projects that have been based on their majors, personal interests, and cultural backgrounds. Students have also conducted advanced independent work in different areas of chemistry, including the analysis of nail polishes and lacquers and eleven aromatic compounds present in three different brands of gasoline.

  15. 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.

  16. First detection of an NSAID, flunixin, in sheep's wool using GC-MS.

    Science.gov (United States)

    Richards, Ngaio; Hall, Sarah; Scott, Karen; Harrison, Nancy

    2011-05-01

    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.

  17. Identification of the main phenolic compounds in wood of Ceratonia siliqua by GC-MS.

    Science.gov (United States)

    Balaban, Mualla

    2004-01-01

    The tannin composition of wood of Ceratonia siliqua (carob) was studied using GC-MS and classical chemical assays. Aqueous methanolic extracts of carob heartwood and sapwood were fractionated using organic solvents of increasing polarity, and GC-MS analyses were performed before and after hydrolysis. Prior to hydrolysis, gallic acid, catechin and its derivatives, methyl inositol and chalcone were determined as the major compounds found in the free form. Aqueous fractions of both wood types were hydrolysed with hydrochloric acid in methanol and extracted with organic solvents and water. These fractions were rich in methyl inositol, gallic acid, glucose and other monosaccharides. The results show that carob wood contains predominantly gallotannins and proanthocyanidins. The technique employed is shown to be a valuable tool and an alternative method to HPLC determination of hydrolysable tannin composition.

  18. [Determination of diphenyl and o-phenylphenol in agricultural products by GC/MS].

    Science.gov (United States)

    Takahashi, Kunihiko; Horie, Masakazu; Hirose, Yoshihumi

    2008-01-01

    A simple determination method of diphenyl (DP) and o-phenylphenol (OPP) in agricultural products by GC/MS was examined. DP and OPP were extracted with ethyl acetate in the presence of anh. sodium sulfate. After addition of n-butanol, the extract solution was concentrated. Clean-up was achieved by shaking with graphitized bulk carbon (Supelclean ENVI-Carb). Addition of polyethylene glycol sharpened the OPP peak on GC/MS analysis. The recoveries from 9 kinds of agricultural products spiked at 0.01 and 0.5 microg/g each were mostly in the range of 70 to 120%, except for 50% recovery of OPP from barley spiked at 0.01 microg/g. The quantification limits (S/N > or =10) of DP and OPP were 0.0013 and 0.005 microg/g (0.0025 and 0.01 microg/g in barley and soybean), respectively.

  19. Methanol ice VUV photoprocessing: GC-MS analysis of volatile organic compounds

    Science.gov (United States)

    Abou Mrad, Ninette; Duvernay, Fabrice; Chiavassa, Thierry; Danger, Grégoire

    2016-05-01

    Next to water, methanol is one of the most abundant molecules in astrophysical ices. A new experimental approach is presented here for the direct monitoring via gas chromatography coupled to mass spectrometry (GC-MS) of a sublimating photoprocessed pure methanol ice. Unprecedentedly, in a same analysis, compelling evidences for the formation of 33 volatile organic compounds are provided. The latter are C1-C6 products including alcohols, aldehydes, ketones, esters, ethers and carboxylic acids. Few C3 and all C4 detected compounds have been identified for the first time. Tentative detections of few C5 and C6 compounds are also presented. GC-MS allows for the first time the direct quantification of C2-C4 photoproducts and shows that their abundances decrease with the increase of their carbon chain length. These qualitative and quantitative measurements provide important complementary results to previous experiments, and present interesting similarities with observations of sources rich in methanol.

  20. Preliminary Phytochemical Screening and GC- MS Profiling of Ethanolic Flower Extract of Calotropis gigantea Linn. (Apocyanaceae

    Directory of Open Access Journals (Sweden)

    R. Dhivya

    2013-09-01

    Full Text Available Calotropis gigantea Linn is popularly known as the swallow-wort or milkweed and is used as one of the most important drug in Traditional System of Medicine to treat various ailments. The aim of this study is to screen the phytochemicals present in the ethanolic flower extract of Calotropis gigantea and further analysis of the components present in it by GC-MS analysis. Ten grams of flower power was sequentially extracted by ethanol. The results showed the presence of phytochemical compounds of alkaloids, tannins, phenol, flavanoids, sterols, antraquinones, proteins and quinones in the flower extract. The GC-MS analysis of the ethanolic extract revealed the presence of 14 major compounds. This study forms a basis for the biological characterization and importance of the compounds identified and creates a platform to screen many bioactive components to treat many diseases.

  1. Online RPLC-GC via TOTAD method to isolate (+)-methyl epijasmonate from lemon (Citrus limon Burm.).

    Science.gov (United States)

    del Mar Caja, Maria; Blanch, Gracia Patricia; Ruiz del Castillo, Maria Luisa

    2008-07-23

    Pure (+)-methyl epijasmonate was isolated from lemon ( Citrus limon Burm.) for the first time. To that aim, two commercial essential oils and one homemade extract were included in the present paper. First, a study on the appropriate chromatographic conditions to avoid the epimerization from methyl epijasmonate to the more stable methyl jasmonate was accomplished. The results obtained are discussed. The presence of (+)-methyl epijasmonate in the three samples studied was initially established through the direct injection into GC-MS. However, the overlapping of (+)-methyl epijasmonate with other matrix components made it necessary to employ a multidimensional technique. RPLC-GC analysis via through-oven transfer adsorption-desorption (TOTAD) provided the selectivity and sensitivity required, reflecting that the homemade lemon extract was an adequate natural source to obtain pure (+)-methyl epijasmonate by means of the collection of the corresponding RPLC fraction.

  2. GC Method Validation for the Analysis of Menthol in Suppository Pharmaceutical Dosage Form

    Directory of Open Access Journals (Sweden)

    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.

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

    OpenAIRE

    2010-01-01

    Abstract: 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 ...

  4. GC-MS analysis of off-odor volatiles from irradiated pork

    Institute of Scientific and Technical Information of China (English)

    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.

  5. GC-FID法测定水中敌敌畏含量的研究

    Institute of Scientific and Technical Information of China (English)

    范钦华

    2009-01-01

    建立了利用GC-FID法测定水中敌敌畏的色谱条件,比较C18固相萃取、活性炭富集、液-液萃取等3种预处理法测定敌敌畏含量的回收率,C18固相萃取预处理效果最好,回收率达102%.

  6. GC-MS Characterisation of Sapogenins from Sisal Waste and a Method to Isolate Pure Hecogenin

    Directory of Open Access Journals (Sweden)

    Jener David G. Santos

    2014-01-01

    Full Text Available Five steroidal sapogenins (tigogenin, neotigogenina, hecogenin, gloriogenin, and dehydrohecogenin were characterised by gas chromatography coupled with mass spectrometry (GC-MS from a hydrolysed extract of sisal waste. In addition, pure hecogenin, an important raw material for the pharmaceutical industry, was obtained from this waste by selective liquid-liquid extraction of saponins with only hecogenin as aglycone, followed by acid hydrolysis. The yield of pure hecogenin was 460 mg.Kg-1 of sisal waste.

  7. Phytochemical Analysis and GC-MS profiling in the leaves of Sauropus Androgynus (l) MERR

    OpenAIRE

    Senthamarai Selvi. V; Anusha Basker

    2012-01-01

    In the present the phytochemical analysis of Sauropus androgynus was carried out. Phytochemical analysis of the leaves of this plant is reported for the first time. The leaves indicated the presence of proteins, resins, steroids, tannins, glycosides, reducing sugar, carbohydrates, saponins, sterols, terpenoids, acidic compounds, cardiac glycosides, catechol, phenols, alkaloids, flavonoids. In the GC-MS analysis the Sauropus androgynus extract result shows the presence of bioactive compounds w...

  8. GC-HS Method Development for the Estimation of Benzene Content in Lovastatin

    Directory of Open Access Journals (Sweden)

    Patel D

    2013-05-01

    Full Text Available A simple, fast and accurate method has been developed for the estimation of benzene content inLovastatin by Gas Chromatography. The analysis was carried out on Perkin Elmer Clarus 600 GC-HSChromatograph. The column used was DB-624 30m X 0.32 mm X 1.8 μm fused silica analytical column(6% cyanopropylphenyl 94 % dimethylpolysiloxane as a stationary phase.The detector used wasFID detector.

  9. THE STUDY OF PHTHALATES MIGRATION IN WINE PRODUCTS BY GC-MS METHOD

    Directory of Open Access Journals (Sweden)

    Gh. Duca

    2012-12-01

    Full Text Available A number of studies have shown phthalates’ potential impact on human health due to their carcinogenic and endocrinedisrupting effects. More than 2000 analyses for determination of phthalates’ rests in alcoholic beverages were done in the laboratory of National Center for Quality Testing of the Alcoholic Beverages (Republic of Moldova using modern method of analysis like GC-MS. This article is an extended abstract of a communication presented at the Conference Ecological Chemistry 2012

  10. GC-MS ANALYSIS OF THE FATTY ACID METHYL ESTER IN JAPANESE QUAIL FAT

    Directory of Open Access Journals (Sweden)

    Ion Dragalin

    2015-12-01

    Full Text Available The accumulated as production waste fat from Faraon quail breeds has been investigated for the first time by using GC-MS technique, preventively converting it via methanolysis to fatty acid methyl esters. The test results, regarding the content of unsaturated fatty acids having a favorable to human body cis-configuration (77.8%, confirm their nutritional value and the possibility of using this fat in cosmetic, pharmaceutical and food industries.

  11. Efficiency of GC-MS method in detection of beeswax adulterated with paraffin

    OpenAIRE

    Waś Ewa; Szczęsna Teresa; Rybak-Chmielewska Helena

    2016-01-01

    The efficiency of the gas chromatography - mass detector (GC-MS) technique for the detection of beeswax adulterated with paraffin, was evaluated. For this purpose, beeswax samples with paraffin additions (3, 5, 10, 30, 50%) were analysed. Since not enough is known about paraffin compositions, and since it is difficult to detect paraffin in beeswax, the aim of our research was also to compare the hydrocarbon composition of different types of paraffin. The analysis showed that the types of para...

  12. Gas Chromatography-Infrared (GC-IR) Applications In Pesticide Chemistry

    Science.gov (United States)

    Kalasinsky, Kathryn S.

    1981-10-01

    After pesticides in bait formulation have been applied in the field, it is important that the fate of that amount of toxicant which has not been consumed by the pest is known. Many of these substances are not compatible with the environment and it is also important that their biodegradation be understood and controlled to a certain extent. In efforts to monitor and direct these reactions GC-IR has been found to be an invaluable tool.

  13. Preliminary Phytochemical Screening and GC- MS Profiling of Ethanolic Flower Extract of Calotropis gigantea Linn. (Apocyanaceae)

    OpenAIRE

    R.Dhivya; K. Manimegalai

    2013-01-01

    Calotropis gigantea Linn is popularly known as the swallow-wort or milkweed and is used as one of the most important drug in Traditional System of Medicine to treat various ailments. The aim of this study is to screen the phytochemicals present in the ethanolic flower extract of Calotropis gigantea and further analysis of the components present in it by GC-MS analysis. Ten grams of flower power was sequentially extracted by ethanol. The results showed the presence of phytochemical compounds ...

  14. 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.

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

    Directory of Open Access Journals (Sweden)

    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.

  16. Hydrothermal synthesis of In2S3/g-C3N4 heterojunctions with enhanced photocatalytic activity.

    Science.gov (United States)

    Xing, Chaosheng; Wu, Zhudong; Jiang, Deli; Chen, Min

    2014-11-01

    Graphitic carbon nitride (g-C3N4) was hybridized by In2S3 to form a novel In2S3/g-C3N4 heterojunction photocatalyst via a hydrothermal method. TEM and HRTEM results reveal that In2S3 nanoparticles and g-C3N4 closely contact with each other to form an intimate interface. The as-obtained In2S3/g-C3N4 heterojunctions exhibit higher photocatalytic activity than those of pure g-C3N4 and In2S3 for the photodegradation of rhodamine B (RhB) under visible light irradiation. The enhanced photocatalytic performance of In2S3/g-C3N4 heterojunctions could be attributed to its wide absorption in the visible region and efficient electron-hole separation. On the basis of radical scavenger experiments, superoxide radicals and holes are suggested to play a critical role in RhB degradation over In2S3/g-C3N4 heterojunctions.

  17. Characterization of incense smoke by solid phase microextraction—Comprehensive two-dimensional gas chromatography (GC×GC)

    Science.gov (United States)

    Tran, Tin C.; Marriott, Philip J.

    Comprehensive two-dimensional gas chromatography in tandem with flame ionization detection (GC×GC-FID) was used for the qualitative fingerprint characterisation of four different types of powdered incense headspace (H/S), and incense smoke. Volatile organic compounds (VOCs) in the incense powder and smoke were extracted by using solid phase microextraction (SPME) with a polydimethylsiloxane/divinylbenzene (PDMS/DVB) 65 μm fiber. Low-polarity/polar, and polar/non-polar phase combinations were tested to contrast the GC×GC separation of components in these two column sets. A total of 324 compounds were tentatively identified, with more than 100 compounds in incense powders and more than 200 compounds in the incense smoke, by using GC coupled to quadrupole mass spectrometric detection. Identification required at least 90% match with the NIST library; otherwise they were considered as unidentified. The smoke stream comprised compounds originating from the incense powder, and combustion products such as PAH, N-heterocyclics, and furans. However, GC×GC was able to separate many more volatile compounds (possibly hundreds more) present in the complex smoke samples, many of which cannot be separated by conventional 1D-GC; this is a direct consequence of the high-resolution power of GC×GC. GC×GC fingerprint comparison of powder H/S with smoke allows facile subtraction of the former from the latter to assist identification of compounds generated from burning incense.

  18. Determination of Alkylphenol Ethoxylates in Leather and Textile by GC-MS%皮革及纺织品中APEO残留量的GC-MS测定

    Institute of Scientific and Technical Information of China (English)

    马贺伟; 赵立国; 洪新球; 黄新霞

    2011-01-01

    A procedure was developed for determining alkylphenol ethoxylates (APEOn) in leather and textile by gas chromatography - mass detector. The targets were extracted from samples using ultrasonic -assisted acetonitrile extraction. APEOn in the extracts were first converted into AP with aluminum triiodide as cleavage reagent, and the yielded AP were then isolated and detected by GC - MS. The contents of APEOn were calculated by normalizing to APEO9. For the total procedure, the recovery ranged from 91% to 101% and the precision (RSD%) ranged from 5% ~9%. The quantitative detection limits are 2.5mg/kg and 1.2mg/kg for NPEO9 and OPEO9, respectively. This analytical procedure is properly validated, offering a reliable and simple way for monitoring APEOn in leather and textile.%建立了皮革及纺织品中烷基酚聚氧乙烯醚(APEOn)残留量的GC-MS测定方法.采用超声波辅助乙腈对样品中的APEOn进行萃取,萃取液中的APEOn经过三碘化铝裂解后,完全转化为等摩尔量的烷基酚(AP),然后采用气相色谱-质谱(GC-MS)对AP进行测试,最后根据AP的浓度计算样品APEOn的含量,以APEO9表示.结果表明:方法的回收率在91%~101%之间,相对标准偏差在5%~9%之间,壬基酚聚氧乙烯醚(NPEO9)的定量检测限为3.0mg/kg、辛基酚聚氧乙烯醚(OPEO9)为1.2mg/kg.方法的可靠性强、灵敏度高,为皮革及纺织品中APEOn残留量的有效监测提供了简便、可靠的检测技术.

  19. Spectroscopic studies of the binding of Cu(II) complexes of oxicam NSAIDs to alternating G-C and homopolymeric G-C sequences.

    Science.gov (United States)

    Chakraborty, Sreeja; Bose, Madhuparna; Sarkar, Munna

    2014-03-25

    Drugs belonging to the Non-steroidal anti-inflammatory (NSAID) group are not only used as anti-inflammatory, analgesic and anti-pyretic agents, but also show anti-cancer effects. Complexing them with a bioactive metal like copper, show an enhancement in their anti-cancer effects compared to the bare drugs, whose exact mechanism of action is not yet fully understood. For the first time, it was shown by our group that Cu(II)-NSAIDs can directly bind to the DNA backbone. The ability of the copper complexes of NSAIDs namely meloxicam and piroxicam to bind to the DNA backbone could be a possible molecular mechanism behind their enhanced anticancer effects. Elucidating base sequence specific interaction of Cu(II)-NSAIDs to the DNA will provide information on their possible binding sites in the genome sequence. In this work, we present how these complexes respond to differences in structure and hydration pattern of GC rich sequences. For this, binding studies of Cu(II) complexes of piroxicam [Cu(II)-(Px)2 (L)2] and meloxicam [Cu(II)-(Mx)2 (L)] with alternating GC (polydG-dC) and homopolymeric GC (polydG-polydC) sequences were carried out using a combination of spectroscopic techniques that include UV-Vis absorption, fluorescence and circular dichroism (CD) spectroscopy. The Cu(II)-NSAIDs show strong binding affinity to both polydG-dC and polydG-polydC. The role reversal of Cu(II)-meloxicam from a strong binder of polydG-dC (Kb=11.5×10(3) M(-1)) to a weak binder of polydG-polydC (Kb=5.02×10(3) M(-1)), while Cu(II)-piroxicam changes from a strong binder of polydG-polydC (Kb=8.18×10(3) M(-1)) to a weak one of polydG-dC (Kb=2.18×10(3) M(-1)), point to the sensitivity of these complexes to changes in the backbone structures/hydration. Changes in the profiles of UV absorption band and CD difference spectra, upon complex binding to polynucleotides and the results of competitive binding assay using ethidium bromide (EtBr) fluorescence indicate different binding modes in each

  20. Spectroscopic studies of the binding of Cu(II) complexes of oxicam NSAIDs to alternating G-C and homopolymeric G-C sequences

    Science.gov (United States)

    Chakraborty, Sreeja; Bose, Madhuparna; Sarkar, Munna

    2014-03-01

    Drugs belonging to the Non-steroidal anti-inflammatory (NSAID) group are not only used as anti-inflammatory, analgesic and anti-pyretic agents, but also show anti-cancer effects. Complexing them with a bioactive metal like copper, show an enhancement in their anti-cancer effects compared to the bare drugs, whose exact mechanism of action is not yet fully understood. For the first time, it was shown by our group that Cu(II)-NSAIDs can directly bind to the DNA backbone. The ability of the copper complexes of NSAIDs namely meloxicam and piroxicam to bind to the DNA backbone could be a possible molecular mechanism behind their enhanced anticancer effects. Elucidating base sequence specific interaction of Cu(II)-NSAIDs to the DNA will provide information on their possible binding sites in the genome sequence. In this work, we present how these complexes respond to differences in structure and hydration pattern of GC rich sequences. For this, binding studies of Cu(II) complexes of piroxicam [Cu(II)-(Px)2 (L)2] and meloxicam [Cu(II)-(Mx)2 (L)] with alternating GC (polydG-dC) and homopolymeric GC (polydG-polydC) sequences were carried out using a combination of spectroscopic techniques that include UV-Vis absorption, fluorescence and circular dichroism (CD) spectroscopy. The Cu(II)-NSAIDs show strong binding affinity to both polydG-dC and polydG-polydC. The role reversal of Cu(II)-meloxicam from a strong binder of polydG-dC (Kb = 11.5 × 103 M-1) to a weak binder of polydG-polydC (Kb = 5.02 × 103 M-1), while Cu(II)-piroxicam changes from a strong binder of polydG-polydC (Kb = 8.18 × 103 M-1) to a weak one of polydG-dC (Kb = 2.18 × 103 M-1), point to the sensitivity of these complexes to changes in the backbone structures/hydration. Changes in the profiles of UV absorption band and CD difference spectra, upon complex binding to polynucleotides and the results of competitive binding assay using ethidium bromide (EtBr) fluorescence indicate different binding modes in each

  1. 维药香蜂花挥发油的GC-MS分析%Analysis of Essential Oil Components in Melissa officinalis Linn by GC-MS

    Institute of Scientific and Technical Information of China (English)

    杨娟; 哈木拉提·吾甫尔; 赵鹤珊; 张帆

    2012-01-01

    The essential oil components were analyzed in Melissa offciinalis Linn by both GC-MS and retention indices at the same time.Essential oil obtained by hydrodistillation from dried aerial part of M.officinalis Linn collected from Xinjiang province (western China),was analyzed by gas chromatography-flame ionization detector (GC-FID),gas chromatography coupled to mass spectrometry (GC-MS) and all components' retention indices.Twenty-eight constituents were accurately detected from the essential oil,accounting for 99.02% of the total amount.The quantitatively significant constituents of the essential oil were ( E)-3,7-dimethyl-2,6-octadien-1-ol acetate (26.48%),(Z)-citral ( 15.46% ),(E)-nerol (14.51%),(E)-citral (14.43%),isoanisole (7.88%),palmitic acid (6.93% ) and (Z)-nerol (2.56% ).The components of M.officinalis Linn essential oil were complicated and were dominated by mono-and sesquiterpene compounds,which were maybe the main biological activities.%结合气相色谱-质谱联用技术和保留指数对维医常用药材香蜂花挥发油提取物进行了分析.从该挥发油中共准确鉴定出28个化合物,占提取物总量的99.02%.结果发现,主要成分有(E)-3,7-dimethyl-2,6-octadien-1-ol acetate( 26.48%)、(Z)-citral(15.46%)、(E)-nerol(14.51%)、(E)-citral(14.43%)、isoanisole (7.88%)、palmitic acid (6.93%)和(Z)-nerol (2.56%),多为单萜和倍半萜类成分,为维药香蜂花的质量标准制定提供了科学依据.

  2. The Relationship between Interleukin-6 -174 G/C Gene Polymorphism and Chronic Periodontitis

    Directory of Open Access Journals (Sweden)

    Tayebeh Sanchooli

    2012-03-01

    Full Text Available Background: Chronic periodontitis is an inflammatory disease that causes rapid destruction of the tissues supporting the teeth. Genetic and environmental factors are involved in its occurrence. It has been suggested that IL-6 promoter gene polymorphism could affect the severity of chronic periodontitis. This study has examined the relationship between IL-6 (-174G/C gene polymorphism and chronic periodontitis.Materials and Methods: In this case-control study, 100 patients with chronic periodontitis and 100 healthy individuals referring to the clinic of Zahedan Dental School were evaluated. Two ml of peripheral blood was taken from these people. After DNA extraction through salting out method, IL-6 gene polymorphism was determined through T-ARMS-PCR technique using specific primers. The data were analyzed by chi-square test and p<0/05was considered significant.Results: The frequency of genotypes CC, GC, GG was respectively 61%, 35% and 4% in patients and respectively 67%, 31% and 2% in the control group. The frequency of G and C alleles was respectively 78.5% and 21.5% in the patient group, and respectively 82.5% and 17.5% in control group. No statistically significant difference was observed between the two groups in frequency of genotypes and alleles.Conclusion: This study showed no correlation between IL-6-174 G/C gene polymorphism and chronic periodontitis.

  3. Simultaneous analysis of synthetic cannabinoids in the materials seized during drug trafficking using GC-MS.

    Science.gov (United States)

    Choi, Hyeyoung; Heo, Sewoong; Choe, Sanggil; Yang, Wonkyung; Park, Yuran; Kim, Eunmi; Chung, Heesun; Lee, Jaesin

    2013-05-01

    A rapid and simple gas chromatography-mass spectrometry (GC-MS) method was developed and validated to identify and quantify synthetic cannabinoids in the materials seized during drug trafficking. Accuracy and reproducibility of the method were improved by using deuterated JWH-018 and JWH-073 as internal standards. Validation results of the GC-MS method showed that it was suitable for simultaneous qualitative and quantitative analyses of synthetic cannabinoids, and we analyzed synthetic cannabinoids in seized materials using the validated GC-MS method. As a result of the analysis, ten species of synthetic cannabinoids were identified in dried leaves (n = 40), bulk powders (n = 6), and tablets (n = 14) seized in Korea during 2009-2012, as a single ingredient or as a mixture with other active co-ingredients. JWH-018 and JWH-073 were the most frequently identified compounds in the seized materials. Synthetic cannabinoids in the dried leaves showed broad concentration ranges, which may cause unexpected toxicity to abusers. The bulk powders were considered as raw materials used to prepare legal highs, and they contained single ingredient of JWH-073, JWH-019, or JWH-250 with the purity over 70 %. In contrast, JWH-018 and JWH-073 contents in the tablets were 7.1-13.8 and 3.0-10.2 mg/g, respectively. Relatively low contents in the tablets suggest that the synthetic cannabinoids may have been added to the tablets as supplements to other active co-ingredients.

  4. GC-MS analysis of allergens in plant oils meant to cosmetics

    Directory of Open Access Journals (Sweden)

    Kaloustian Jacques

    2007-03-01

    Full Text Available Cutaneous allergy occurs mainly as a result of the use of domestic products and cosmetics. Some fragrances, present in these products, may contain compounds that are responsible for allergy (allergens. The European Council offered a Directive limiting the level of 26 allergens found in cosmetics. GC-MS technique was used to determine the retention times of 25 allergens, determine detection and quantification limits and make calibration with standard solution of each allergen in concentrations ranging from 10 to 200 mgL–1 (21 allergens and 50 to 200 mgL–1 (4 allergens. Quantification was performed by the use of 2 internal standards (tetradecane and hexadecane. Seven oils issued from plants were studied by GC-MS. For all of them, the concentration of potential allergens was lower than their minimum detectable level. The alcoholic solution of extracts issued from different samples of oil did not demonstrate the presence of any quantifiable allergen, even when was concentrated 25 times. GC-MS could be a useful technique in the identification and, if necessary, quantification of allergen in ingredients meant to cosmetics.

  5. Interference of anesthetics in blood alcohol analysis by HS-GC-FID: A case report.

    Science.gov (United States)

    Monteiro, C; Proença, P; Tavares, C; Castañera, A; Corte Real, F

    2016-08-01

    One of the techniques most widely used in ethanol analysis in forensic laboratories is undoubtedly the headspace gas chromatography with flame-ionization detection (HS-GC-FID) since the determination of this substance is carried out directly, without the need for additional purification procedures, which leads to increased productivity. This is a very important factor due to the high number of alcohol analysis requested to these laboratories. The presence of other volatile substances can cause a problem given the fact that they can be interferents in ethanol analysis by HS-GC-FID, which can have legal consequences related with driving under the influence of alcohol. The authors report a case of a routine analysis by HS-GC-FID for the determination of ethanol of a driver who has suffered an accident in which the use of two chromatographic columns with different polarities was essential to obtain an unequivocally identification of this substance in presence of an interfering volatile anesthetic administered in the hospital. The method was validated according to international recommendations before being introduced into routine laboratory in terms of selectivity, limits of detection (LOD), limits of quantification (LOQ), linearity, repeatability, intermediate precision, accuracy, robustness and carryover.

  6. Genome size, GC percentage and 5mC level in the Indonesian coelacanth Latimeria menadoensis.

    Science.gov (United States)

    Makapedua, Daisy Monica; Barucca, Marco; Forconi, Mariko; Antonucci, Niki; Bizzaro, Davide; Amici, Adolfo; Carradori, Maria Rita; Olmo, Ettore; Canapa, Adriana

    2011-09-01

    The living fossil Latimeria menadoensis is important to understand sarcopterygian evolution. To gain further insights into this fish species we studied its genome size, GC% and 5mC level. The genome size and the GC% of the Indonesian coelacanth seem to be very similar to those of the African coelacanth. Moreover the GC%, the CpG frequency and the 5mC level of L. menadoensis are more similar to those of fish and amphibians than to those of mammals, birds and reptiles and this is in line with the hypothesis that two different DNA methylation and CpG shortage equilibria arose during vertebrate evolution. Our results suggest that the genome of L. menadoensis has remained unchanged for several million years, maybe since the origin of the lineage which from lobe-finned fish led to tetrapods. These data fit a conservative evolutionary landscape and suggest that the genome of the extant crossopterygians may be a sort of evolutionarily frozen genome.

  7. Predicting refinery effluent toxicity on the basis of hydrocarbon composition determined by GCxGC analysis

    Energy Technology Data Exchange (ETDEWEB)

    Whale, G. [and others

    2013-04-15

    A high resolution analytical method for determining hydrocarbon blocks in petroleum products by comprehensive two-dimensional gas chromatography (GCxGC) was used for the analysis of petroleum hydrocarbons extracted from refinery effluents. From 105 CONCAWE refineries in Europe 111 refinery effluents were collected in the period June 2008 to March 2009 (CONCAWE, 2010). The effluents were analysed for metals, standard effluent parameters (including Chemical Oxygen Demand (COD), Biochemical Oxygen Demand (BOD), oil in water (OiW), GCxGC speciated hydrocarbons, BTEX (Benzene, Toluene, Ethylbenzene, and Xylenes) and volatile organic compounds. This report describes the subsequent analysis of the GCxGC data, as described in hydrocarbon blocks, and uses the PETROTOX model, to predict the environmental toxicity (i.e. ecotoxicity) of the discharged effluents. A further analysis was undertaken to address the potential environmental impact of these predicted effects initially using default dilution factors and then,when necessary site specific factors. The report describes all the methods used to arrive at the predictions, and shows that for the majority of refinery effluents direct toxicity effects in the effluents are not anticipated. Furthermore, when applying either the EU Risk Assessment Technical Guidance Document (TGD) default dilution factors or site specific dilution factors, none of the refineries are predicted to exerting either acute or chronic toxicity to organisms in the receiving aquatic environment, based on their hydrocarbon composition present in the effluent samples.

  8. Comparison of Two Species of Notopterygium by GC-MS and HPLC

    Directory of Open Access Journals (Sweden)

    Yaping Wang

    2015-03-01

    Full Text Available Notopterygii Rhizoma et Radix (Qianghuo, including Notopterygium incisum Ting ex H. T. Chang (NI and Notopterygium franchetii H. de Boiss (NF, is an important traditional Chinese medicine. Of these two plants, NI, is more commonly used and has a much higher price in the marketplace. To compare these two plants, a combination of gas chromatography-mass spectrometry (GC-MS and high performance liquid chromatography (HPLC was carried out, thus obtaining an overall characterization for both volatile and none-volatile compounds. Combined with hierarchical cluster analysis (HCA and principal component analysis, GC-MS was successfully applied to distinguish NF and NI. The chemical constitutes of volatile oil in NI and NF were firstly compared in detail, and 1R-alpha-pinene, beta-pinene and 4-isopropyl-1-methyl-1,4-cyclohexadiene had great contribution to the discrimination. Fingerprints of 14 batches of Qinghuo samples were also established based on HPLC, and an obvious difference was found between the two species. The chromatographic fingerprints were further analyzed by similarity analysis and HCA. The present study is the first reported evaluation of two origins of Notopterygii Rhizoma et Radix by GC-MS and HPLC, which will facilitate quality control and its clinical application.

  9. Combined ESTs from plant-microbe interactions: using GC counting to determine the species of origin.

    Science.gov (United States)

    Huitema, Edgar; Torto, Trudy A; Styer, Allison; Kamoun, Sophien

    2003-01-01

    A diversity of microorganisms establishes intimate associations with plants. Whether pathogenic or symbiotic, such interactions are the result of complex recognition events between plants and microbes, leading to signaling cascades and regulation of countless genes involved in the interaction. A key step in unraveling the mysteries of plant-microbe interactions lies in defining the transcriptional changes that occur in both the host and the microbe during their association. The sum of the transcripts, from both host and microbe, which are produced during their association, has been defined as the interaction transcriptome. One approach to analyze interaction transcriptomes is to perform large-scale sequencing of cDNAs (expressed sequence tags or ESTs) obtained from infected plant tissue and representing a mixture of host and microbe sequences. In some cases, the two organisms have markedly different GC content, allowing most ESTs to be easily distinguished on this basis. In this chapter, we describe a GC counting method to determine the species of origin of ESTs obtained from interactions between plants and oomycetes or other high GC content microbes.

  10. Opposite GC skews at the 5' and 3' ends of genes in unicellular fungi

    Directory of Open Access Journals (Sweden)

    McLean Malcolm A

    2011-12-01

    Full Text Available Abstract Background GC-skews have previously been linked to transcription in some eukaryotes. They have been associated with transcription start sites, with the coding strand G-biased in mammals and C-biased in fungi and invertebrates. Results We show a consistent and highly significant pattern of GC-skew within genes of almost all unicellular fungi. The pattern of GC-skew is asymmetrical: the coding strand of genes is typically C-biased at the 5' ends but G-biased at the 3' ends, with intermediate skews at the middle of genes. Thus, the initiation, elongation, and termination phases of transcription are associated with different skews. This pattern influences the encoded proteins by generating differential usage of amino acids at the 5' and 3' ends of genes. These biases also affect fourfold-degenerate positions and extend into promoters and 3' UTRs, indicating that skews cannot be accounted by selection for protein function or translation. Conclusions We propose two explanations, the mutational pressure hypothesis, and the adaptive hypothesis. The mutational pressure hypothesis is that different co-factors bind to RNA pol II at different phases of transcription, producing different mutational regimes. The adaptive hypothesis is that cytidine triphosphate deficiency may lead to C-avoidance at the 3' ends of transcripts to control the flow of RNA pol II molecules and reduce their frequency of collisions.

  11. Automated dynamic headspace/GC-MS analyses affect the repeatability of volatiles in irradiated Turkey.

    Science.gov (United States)

    Nam, Ki-Chang; Cordray, Joseph; Ahn, Dong U

    2004-03-24

    Although a dynamic headspace/gas chromatography-mass spectrometry (DH/GC-MS) method is an effective tool for determining volatiles of irradiated turkey meat, the profile of volatiles may be changeable depending upon the availability of oxygen in the sample vial and sample holding time before purge. The objective of this study was to evaluate the effects of helium flushing and sample holding time before purge on the volatiles profiles of irradiated raw and cooked turkey breast meat. Vacuum-packaged turkey breasts were irradiated at 2.5 kGy, and the volatiles of irradiated raw and cooked samples were analyzed using a DH/GC-MS with different holding times up to 280 min. The amounts of dimethyl disulfide and dimethyl trisulfide decreased as sample holding time in an autosampler (4 degrees C) before purge increased, whereas those of aldehdyes increased as holding time increased due to lipid oxidation. Helium flush of sample vials before sample loading on an autosampler retarded lipid oxidation and minimized the changes of sulfur volatiles in raw meat but was not enough to prevent oxidative changes in cooked meat. Although DH/GC-MS is a convenient method for automatic analysis of volatiles in meat samples, the number of samples that can be loaded in an autosampler at a time should be limited within the range that can permit reasonable repeatabilities for target volatile compounds.

  12. Chemical Abundances of the Highly Obscured Galactic Globular Clusters 2MASS GC02 and Mercer 5

    CERN Document Server

    Penaloza, Francisco; Vasquez, Sergio; Borissova, Jura; Kurtev, Radostin; Zoccali, Manuela

    2015-01-01

    We present the first high spectral resolution abundance analysis of two newly discovered Galactic globular clusters, namely Mercer 5 and 2MASS GC02 residing in regions of high interstellar reddening in the direction of the Galactic center. The data were acquired with the Phoenix high-resolution near-infrared echelle spectrograph at Gemini South (R~50000) in the 15500.0 A - 15575.0 A spectral region. Iron, Oxygen, Silicon, Titanium and Nickel abundances were derived for two red giant stars, in each cluster, by comparing the entire observed spectrum with a grid of synthetic spectra generated with MOOG. We found [Fe/H] values of -0.86 +/- 0.12 and -1.08 +/- 0.13 for Mercer 5 and 2MASS GC02 respectively. The [O/Fe], [Si/Fe] and [Ti/Fe] ratios of the measured stars of Mercer 5 follow the general trend of both bulge field and cluster stars at this metallicity, and are enhanced by > +0.3. The 2MASS GC02 stars have relatively lower ratios, but still compatible with other bulge clusters. Based on metallicity and abund...

  13. Performance characteristics of cryofocusing GC/MS system at BWXT Pantex Plant.

    Energy Technology Data Exchange (ETDEWEB)

    Brown, Jason R.; Banet, Judith F.; Ithaca, Jerry (BWXT Pantex Plant, Amarillo, TX); Thornberg, Steven Michael; Woods, Lorelei (BWXT Pantex Plant, Amarillo, TX)

    2006-07-01

    Ensuring the reliability of all components within a weapon system becomes increasingly important as the stockpile ages. One of the most noteworthy surveillance techniques designed to circumvent (or take place alongside) traditional D&I operations is to collect a sample of gas from within the internal atmosphere of a particular region in a weapon. While a wealth of information about the weapon may be encoded within the composition of its gas sample, our access to that information is only as good as the method used to analyze the sample. It has been shown that cryofocusing-GC/MS offers advantages in terms of sensitivity, ease of sample collection, and robustness of the equipment/hardware used. Attention is therefore focused on qualifying a cryo-GC/MS system for routine stockpile surveillance operations at Pantex. A series of tests were performed on this instrument to characterize the linearity and repeatability of its response using two different standard gas mixes (ozone precursor and TO-14) at various concentrations. This paper outlines the methods used and the results of these tests in order to establish a baseline by which to compare future cryo-GC/MS analyses. A summary of the results is shown.

  14. 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.

  15. Mitochondrial Glutamate Carrier GC1 as a Newly Identified Player in the Control of Glucose-stimulated Insulin Secretion*

    Science.gov (United States)

    Casimir, Marina; Lasorsa, Francesco M.; Rubi, Blanca; Caille, Dorothée; Palmieri, Ferdinando; Meda, Paolo; Maechler, Pierre

    2009-01-01

    The SLC25 carrier family mediates solute transport across the inner mitochondrial membrane, a process that is still poorly characterized regarding both the mechanisms and proteins implicated. This study investigated mitochondrial glutamate carrier GC1 in insulin-secreting β-cells. GC1 was cloned from insulin-secreting cells, and sequence analysis revealed hydropathy profile of a six-transmembrane protein, characteristic of mitochondrial solute carriers. GC1 was found to be expressed at the mRNA and protein levels in INS-1E β-cells and pancreatic rat islets. Immunohistochemistry showed that GC1 was present in mitochondria, and ultrastructural analysis by electron microscopy revealed inner mitochondrial membrane localization of the transporter. Silencing of GC1 in INS-1E β-cells, mediated by adenoviral delivery of short hairpin RNA, reduced mitochondrial glutamate transport by 48% (p < 0.001). Insulin secretion at basal 2.5 mm glucose and stimulated either by intermediate 7.5 mm glucose or non-nutrient 30 mm KCl was not modified by GC1 silencing. Conversely, insulin secretion stimulated with optimal 15 mm glucose was reduced by 23% (p < 0.005) in GC1 knocked down cells compared with controls. Adjunct of cell-permeant glutamate (5 mm dimethyl glutamate) fully restored the secretory response at 15 mm glucose (p < 0.005). Kinetics of insulin secretion were investigated in perifused isolated rat islets. GC1 silencing in islets inhibited the secretory response induced by 16.7 mm glucose, both during first (−25%, p < 0.05) and second (−33%, p < 0.05) phases. This study demonstrates that insulin-secreting cells depend on GC1 for maximal glucose response, thereby assigning a physiological function to this newly identified mitochondrial glutamate carrier. PMID:19584051

  16. Estimation of Properties of Pure Components Using Improved Group-Contribution+ (GC+) Based Models and Uncertainty Analysis

    DEFF Research Database (Denmark)

    Hukkerikar, Amol; Sarup, Bent; Abildskov, Jens

    they must be estimated. Predictive methods such as the group-contribution+ (GC+) method (combined group-contribution (GC) method and atom connectivity index (CI) method) are generally suitable to estimate the needed property values. For assessing the quality and reliability of the selected property...... the estimated property values using the GC+ approach, but also the uncertainties in the estimated property values. This feature allows one to evaluate the effects of these uncertainties on the product-process design calculations thereby contributing to better-informed and reliable engineering solutions....

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

    Directory of Open Access Journals (Sweden)

    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

  18. GC determination of N-nitrosamines by supersonic molecular beam MS equipped with triple quadrupole analyzer, GC/SMB/QQQ/MS.

    Science.gov (United States)

    Anna, Voloshenko; Rimma, Shelkov; Lev, Ovadia; Jenny, Gun

    2011-01-31

    The determination of 14 N-nitrosamines by a supersonic molecular beam electron ionization mass spectrometer equipped with triple quadruple analyzer, GC/SMB/EI/QQQ/MS is presented. The supersonic molecular beam electron ionization ion source allows the elucidation of the molecular ion of 13 out of the 14 examined nitrosamines (except for diphenylnitrosamine which was degraded before the analysis). It was possible to use the molecular ions of all the nitrosamines as the parent ions for multiple reactions monitoring mode, which in turn allows significant increase of specificity and lowering of the method limit of detection of the higher molecular weight nitrosamines. The instrumental LOD for different N-nitrosamines was 1-5 pg injection(-1). The proposed method was exemplified by analysis of N-nitrosamines and N-nitrosatables in rubber teats according to the British Standard BS EN 12868:1999. Copyright © 2010. Published by Elsevier B.V.

  19. GC/MS在苯丙胺类药物分析中的应用%Application in the GC/MS analysis of amphetamine

    Institute of Scientific and Technical Information of China (English)

    徐鹏; 邓艳萍; 徐国柱

    2003-01-01

    @@ 苯丙胺类药物的滥用已经成为世界严重的社会问题之一.在过去的几年中,大量的文章报道了血、尿及毛发中苯丙胺类药物的检测和鉴定.通过使用不同的检测器,最低检测浓度已经达到了ng@ml-1.这里我们主要介绍GC/MS在苯丙胺类药物分析中的应用以及还存在的一些不足之处.

  20. 云晓熏醋香味成分的GC-MS分析%Analysis of flavor components in Yunxiao vinegar by GC-MS

    Institute of Scientific and Technical Information of China (English)

    杨晰; 杨继涛; 乔海军

    2010-01-01

    采用同时蒸馏萃取(SDE)提取云晓熏醋的挥发性香味物质,利用气相色谱-质谱联用仪(GC-MS)对其挥发性香味成分进行分离和鉴定,确认了其中50种成分,并用面积归一化法测定了各种成分的质量分数,占总质量分数的93.307%.其主要成分为3-羟基-2-丁酮(38.467%)、糠醛(21.388%)、醋酸(19.228%)、吡嗪类物质(1.970%)和乳酸乙酯(1.736%)等.

  1. Study on chemical comporents in essential on from Citrus Bergamot by GC-MS%金佛手挥发油化学成分的GC-MS研究

    Institute of Scientific and Technical Information of China (English)

    王建英; 施长春; 朱婉萍

    2006-01-01

    目的分析金佛手鲜品与干品挥发油的化学成分与相对含量.方法用色谱-质谱联用法(GC-MS)测定佛手挥发油,结果用计算机检索NIST98数据库.结果从佛手挥发油中检测出30多种化学成分,主要成分是D-柠檬烯和(+)之-蒈烯,鲜品挥发油中分别为40.02%,21.35%,干品挥发油中分别为38.63%,18.17%.结论金佛手挥发油的主要成分是柠檬烯与蒈烯.

  2. 皮革中富马酸二甲酯GC-MS测定%Determinaton of dimethyl fumarate in leather by GC-MS

    Institute of Scientific and Technical Information of China (English)

    马贺伟; 张丹云; 程飞; 黄新霞

    2009-01-01

    建立了皮革中富马酸二甲酯的萃取及气相色谱-质谱(GC-MS)检测方法. 萃取过程以乙酸乙酯作为萃取剂, 超声波辅助萃取;萃取液经过中性氧化铝净化处理. 加标回收率为85.1%~89.3%, 相对标准偏差为5.6%~9.1%. 方法适合于皮革中富马酸二甲酯含量的测定.

  3. Analysis of suspended organic substances in yeast wastewater by GC-MS%酵母废水中颗粒性有机物的GC-MS分析

    Institute of Scientific and Technical Information of China (English)

    周旋; 梁玉倩; 刘秀英; 刘慧; 史郁

    2009-01-01

    酵母废水成分复杂,可生化性差,对其成份进行剖析对于酵母废水的有效处理很有必要.本文将酵母废水中颗粒性有机物与可溶性有机物分离后采用索氏萃取-GC/MS的分析方法进行分析,确定了该废水中颗粒性有机物中的中等极性以下的有机物主要有48种,主要类别为酚类、酯类、含苯杂环类、长链烷烃、醇类、酮类、烯烃等.

  4. GC-MS DETERMINATION OF PESTICIDE RESIDUES IN TEXTILES SEPARATED BY SPME%GC/MS法测定生态纺织品中多种农药残留

    Institute of Scientific and Technical Information of China (English)

    陈军

    2003-01-01

    采用GC/MS法测定棉、麻及织毛物等生态纺织品中农药残留.方法的测定重现性为75%~100%,该方法对有机氯(OCPs)检出限小于0.01mg@kg-1,回收率在97.8%~99.6%之间,相对标准偏差在5.0%~6.0%;对五氯苯酚(PCP)的检出限为0.05mg@kg-1,回收率为75.6%和86.2%,相对标准偏差为5.2%~12.9%.

  5. GC-MS analysis of fatty acids in three kinds of natural beeswax%3种天然蜂蜡中脂肪酸的GC-MS分析

    Institute of Scientific and Technical Information of China (English)

    杜婧; 李超; 邱芳萍

    2014-01-01

    利用气相色谱-质谱联用技术(GC-MS)对蜜盖蜡、新巢蜡、老巢蜡3种天然蜂蜡中的脂肪酸进行分离鉴定,并采用峰面积归一化法测定各组分的相对含量.结果显示,3种天然蜂蜡共分离出9种脂肪酸,相对含量较高的包括棕榈酸、油酸、蜡酸、硬脂酸等,其中大部分为饱和脂肪酸,约占总脂肪酸的86.2%;3种天然蜂蜡中的脂肪酸组成基本一致,但相对含量有一定差异.

  6. GC/MS Analysis of Tea Tree Oil Purified by Molecular Distillation%茶树油的分子蒸馏精制及其GC/MS分析

    Institute of Scientific and Technical Information of China (English)

    翟淑红; 黄少烈; 顾志伟

    2008-01-01

    利用新型、特殊分离技术--分子蒸馏对茶树油进行精制,并对精制后的茶树油进行GC/MS定性分析及其总离子流图的面积归一法定量分析.结果从粗茶树油中分离出了61种化合物,鉴定出36种组分,占总量的98.67 %,其中4-松油醇高达49.56 %,并且精制的茶树油符合国际标准(ISO 4730-1996).

  7. 洋芫荽挥发油成分的GC-MS分析%Extraction of Essential Oil from Coriander and its Ingredient Analysis by GC-MS

    Institute of Scientific and Technical Information of China (English)

    刘顺珍; 张丽霞; 刘红星

    2011-01-01

    采用水蒸汽蒸馏法提取洋芫荽叶中的挥发油,GC-MS技术检测其挥发部分的有效成分,共检测出35个峰,鉴定了其中的22种化合物,占挥发油含量的82.34%.其主要成分为月桂醇(33.5%),2.烯-十二酸(10.06%),月桂酸(6.7%),反-7-烯-十四醛(6.30%),月桂醛(5.44%),桃醛(3.70%)等.

  8. Analysis of volatile oil from shaddock exocarp by GC/MS%柚皮蒸馏产物的GC/MS分析

    Institute of Scientific and Technical Information of China (English)

    唐课文; 朱政斌; 阎建辉; 易健民

    2004-01-01

    用水蒸气蒸馏法对柚皮外果皮进行了挥发性成分提取.用GC/MS分析法进行了分离鉴定,初步分离出50余个峰,鉴定了44种物质,用面积归一法测定其质量分数.在被测物质中,烃类化合物有13种和含氧有机化合物有31种,主要物质为柠檬烯(75.09%),α-蒎烯(0.84%),β-月桂烯(6.71%),芳樟醇(1-08%),芳樟酯(1.43%),萘酮(4.89%).

  9. GC-MS法测定香蕉及土壤中戊唑醇残留量%GC-MS Determination of Residue Tebuconazole in Banana and Soil

    Institute of Scientific and Technical Information of China (English)

    吴琼; 林靖凌; 张月; 谢德芳; 吕岱竹

    2012-01-01

    [Objective] To establish GC-MS analysis method for tebuconazole in banana. [Method] Residual amounts of tebuconazole in banana and soil was determined by gas chromatography and mass spectrometry in hyphenation; The above mentioned pesticides were extracted from the sample with acetonitrile and purified by using SPE Tube. The final extract was injected into GC for separation and followed by MS detection under El ionization and synchronous SIM/SCAN data acquisition mode. [ Result ] The detection limit found for tebuconazole in banana and soil were 0.005 mg/kg. Values of RSD' S found in the whole fruit were in the range of 2.4% -11. 0% ,and values of recovery were in the ranges of 80% - 120% ; values of RSD'S found in flesh were in the range of 1.9% -9.7% ,and values of recovery were in the ranges of 80% -118%; values of RSD' S found in soil were in the range of 4. 0% - 13. 5% ,and values of recovery were in the ranges of 82% - 120%. [ Conclusion] The method could be used to detect the tebuconazole in banana and soil, which showed good separating result, high sensitivity, good reproducibility and so on.%[目的]建立戊-唑醇在香蕉中的GC-MS分析方法.[方法]试样经乙腈提取,固相萃取柱净化,选择离子监测/全扫描(SIM/SCAN)采集气相色谱-质谱法(GC-MS)对香蕉及土壤中戊唑醇残留量进行定性和定量分析.[结果]方法检出限为0.005 mg/kg,戊唑醇在香蕉全蕉中的添加水平回收率为80%~ 120%,相对标准偏差为2.4% ~11.0%;在香蕉蕉肉中的添加水平回收率为80%~118%,相对标准偏差为1.9%~9.7%;在土壤中的添加水平回收率为82% ~ 120%,相对标准偏差为4 0%~13.5%.[结论]该方法具有分离效果好、灵敏度高、重现性好等特点,可用于测定香蕉及土壤中的戊唑醇残留量.

  10. 香菜挥发油GC/MS测定%Determination of Volatile Oil of Coriandrum Sativum L.by GC/MS

    Institute of Scientific and Technical Information of China (English)

    孙小媛; 马玉芳; 李铁纯; 辛广

    2002-01-01

    对香菜茎叶及根经水蒸汽蒸馏--萃取得到的挥发油进行气相色谱/质谱(GC/MS)分析.其中香菜茎叶中主要成分有:壬烷、癸烷、癸醛、十一醛、环癸烷、十二醛、2-十一烯醛、2-癸烯-1-醇、十三醛、十四醛等,香菜根挥发油中主要成分有:壬烷、辛醛、癸醛、环癸烷、十-醛、十二醛、十四醛等.

  11. Analysis of fatty acids in 12 Mediterranean fish species: advantages and limitations of a new GC-FID/GC-MS based technique.

    Science.gov (United States)

    Nevigato, Teresina; Masci, Maurizio; Orban, Elena; Di Lena, Gabriella; Casini, Irene; Caproni, Roberto

    2012-07-01

    When fatty acids in fish are analyzed, results in percentage form (profile analysis) are mostly reported. However, the much more useful results expressed as mg/100 g (absolute analysis) is the main information required. Absolute methods based on calibration curves are of good accuracy but with a high degree of complexity if applied to a great number of analytes. Procedures based on the sequence profile analysis-total FA determination-absolute analysis may be suitable for routine use, but suffer from a number of uncertainties that have never been really resolved. These uncertainties are mainly related to the profile analysis. In fact, most profile analyses reported in the literature disagree about the number and type of fatty acids monitored as well as about the total percentage to assign to their sum so leading to possible inaccuracies; in addition the instrumental response factor for all FAME (fatty acid methyl esters) is often considered as a constant, but this is not exactly true. In this work, a set of 24 fatty acids was selected and studied on 12 fish species in the Mediterranean area (variable in lipid content and month of sampling): in our results, and in these species, this set constitutes, on average, 90 ± 3 % of the total fatty acid content. Moreover the error derived from the assumption of a unique response factor was investigated. Two different detection techniques (GC-FID and GC-MS) together with two capillary columns (different in length and polarity) were used in order to acquire complementary data on the same sample. With the protocol here proposed absolute analyses on the 12 cited species are easily achievable by the total FA determination procedure. The accuracy of this approach is good in general, but in some cases (DHA for example) is lower than the accuracy of calibration-based methods. The differences were evaluated on a case by case basis.

  12. SPME/GC-MS鉴别地沟油新方法(Ⅱ)%A Novel Method for the Identification of Gutter Oils Using SPME/GC - MS ( Ⅱ )

    Institute of Scientific and Technical Information of China (English)

    吴惠勤; 黄晓兰; 林晓珊; 陈江韩; 朱志鑫; 黄芳; 马叶芬; 罗辉泰; 邓欣

    2012-01-01

    The trace impurities of gutter oils were investigated by gas chromatography -mass spec-trometry( GC - MS) with solid-phase microextraction( SPME). By comparison of the trace endogenous substances of various pure vegetable oil and the exogenous impurities of the gutter oils from different areas, together with the analysis of the source of exogenous impurities, the characteristic components of the gutter oils from Guangzhou, Guizhou, Shenzhen and Beijing were acquired, which can be used as indicated components for the distinguishment of gutter oils. With high sensitivity and characteristic , this method was recruited in the blind samples evaluation organized by the Ministry of Public Health and the accuracy on positive samples was as high as 95. 5% .%采用固相微萃取/气相色谱-质谱(SPME/GC- MS)方法测定地沟油中的微量杂质成分,通过对各种纯正植物油中的内源性微量成分与不同地区地沟油中的外源性杂质成分的对比分析,以及对地沟油中杂质成分来源的分析,确定了广州、贵州、深圳、北京等地区地沟油的特征成分,并作为鉴别指示成分.该方法灵敏度高、特征性强,在卫生部组织的地沟油检测盲样考核中,对阳性样品判断的准确率高达95.5%.

  13. GC-CI-MS-SIM方法诊断新生儿苯丙酮尿症%Newborn Screening of Phenylketonuria by GC-CI-MS-SIM

    Institute of Scientific and Technical Information of China (English)

    邓春晖; 胡耀铭; 胡克季; 张雅芬; 顾学范

    2001-01-01

    The application of MS in newborn screening is one of the most important branches of MS′s current clinical application.In this paper we first reported a new method of newborn screening for Phenylketonuria (PKU) by GC-CI-MS-SIM,which was relatively cheap,fast,sensitive and accurate.In this method Phenylalanine (Phe) and Tyrosine (Tyr) were extracted from dry blood spots with 0.1% mol/L HCl-methanol.The protein in the extraction was gotten rid of by centrifugor.Phe and Tyr were reacted with 3.0 mol/L HCl-butanol,then the products Phe and Tyr butyl esters were reacted with trifluoroacetic anhydride.The final derivations from Phe and Tyr,alanine,3-phenyl-N(trifluoroacetyl)-,butyl este and L-tyrosine,N(trifluoroacetyl)-,butyl ester,trifl were analyzed by GCCI-MS-SIM.The contents of the two amino acids in blood samples were determined by calculating the areas of their final derivations with exterior standard.Finally,the molar ratios of Phe to Tyr in blood sample were calculated as the basis of PKU diagnosis.Because chemical ionization and selective ion measurement were used in this method,the limits of detection for Phe and Tyr were low and the sensitivity was excellent.About 30 blood samples were analyzed by this method,and the results prove that this method could successfully discriminate between normal infants and PKU positive ones.The price of instrument GC-MS is cheaper than that of MS-MS.Therefore it was capable for large-scale screening in developing countries.

  14. Determination of trace tin in textiles by DLLME-GC-MS method%DLLME-GC-MS法测定纺织品中的痕量锡

    Institute of Scientific and Technical Information of China (English)

    于文佳; 卫碧文; 郑翊; 杨荣静

    2014-01-01

    基于纺织品水迁移相中有机锡离子首先与四乙基硼化钠生成有机锡化合物,再以四氯乙烯为萃取剂,乙腈为分散剂,建立了分散液液微萃取(DLLME)结合气相色谱-质谱(GC-MS)测定十种有机锡含量的新方法.对影响DLLME萃取效率的因素进行优化试验,萃取条件为:50 μL四氯乙烯为萃取剂,0.5mL乙腈为分散剂,超声萃取0.5 min,以3 000 r/min离心3min,取萃取溶液1.0 μL直接进行GC-MS分析.该方法线性范围为0.005~1 mg/L,线性相关系数(R2)为0.992 6 ~0.999 5,检出限为0.1~0.5μg/L,平均回收率为82.6% ~113.5%,相对标准偏差为5.45% ~ 13.56%,平均富集倍数达到140.

  15. 金银花叶挥发油的GC-MS分析%Study on Essential Oil from Leaf of Lonicera japonic by GC-MS

    Institute of Scientific and Technical Information of China (English)

    肖敏; 谭红军; 李晓华; 康活泼

    2013-01-01

    [Objective] To analyze chemical constituents in the volatile oil from leaves of Lonicera japonic, provide instruction for comprehensive utilization of Lonicera japonic. [Method] The leaves of Lonicera japonic were collected and dried, their volatile oil were extracted by steam distillation method. Then the chemical constituents of volatile oil was analyzed by GC-MS. [Result] There are 29 compounds were detected, among which, 26 compounds were confirmed, which are mainly organic acid and organic acid esters. Some chemical consituents were found similarly in the leaves volatile oil and the flowers volatile oil. These compounds are the materialfoundation for similar functions. [Conclusion] The leaves volatile oil of Lonicera japonic has the latent value of application.%[目的]对金银花叶挥发油的化学成分进行分析,为金银花的综合利用提供指导.[方法]采集金银花叶,干燥,粉碎,采取水蒸气蒸馏法提取其挥发油,GC-MS分析其化学成分.[结果]在金银花叶挥发油中检测出29个化合物,确认26个化合物.这些化合物多为有机酸和有机酸酯.金银花叶挥发油与金银花挥发油有许多相同的化学成分.这些化合物可能是它们具有相似功能的物质基础.[结论]金银花叶挥发油具有潜在的应用价值.

  16. Analysis of Chemical Constituents of Essential Oils from Magnolia coco by GC-MS%夜合花挥发油化学成分的GC-MS分析

    Institute of Scientific and Technical Information of China (English)

    朱小勇; 邵敏敏; 张宏建; 卢汝梅

    2011-01-01

    Objective:To study the chemical constituents of the essential oils from Magnolia coco. Method:The essential oils were extracted by steam distillation(SD) and supercritical carbon dioxide extraction(SFE) , and then the constituents were separated and identified by GC-MS. Result: Fifty six compounds were isolated and identified by SD that composed about 87.46% of the total essential oils; and 25 compounds were isolated and identified by SFE that composed about 95.86% of the total essential oils. Conclusion: The principal constituents of essential oils in M. coco from Guangxi are α-pinene, nerolidol, caryophyllene, germacrene D, bicyclogermacrene,which are very different from the other origin.%目的:研究夜合花挥发油的化学成分.方法:利用水蒸气蒸馏法及超临界CO2萃取法提取桂产夜合花挥发油,用GC-MS联用技术对其化学成分进行分离鉴定,用面积归一化法确定各成分的相对含量.结果:水蒸气蒸馏法提取的挥发油鉴定56个化合物,占挥发油总量的87.46%,超临界CO2萃取法提取的挥发油鉴定25个化合物,占总量的95.86%.结论:桂产夜合花挥发油主要成分是α-蒎烯、橙花叔醇、石竹烯、吉玛烯D、双环吉玛烯,与文献报道其他产地的夜合花挥发油成分有明显差异.

  17. GC-MS of Volatile Chemical Constituents of Liquidamobar orientalis%苏合香挥发性化学成分的GC-MS研究

    Institute of Scientific and Technical Information of China (English)

    王世宇; 彭颖; 夏厚林; 周颖; 王建; 曾南

    2012-01-01

    目的:研究苏合香的挥发性化学成分.方法:通过固相微萃取技术提取苏合香的挥发性成分,采用气相色谱-质谱联用技术进行分析鉴定.结果:共鉴定出苏合香28种成分,占总色谱峰面积的90.72%,其中α-蒎烯(15.97%)、莰烯(13.28%)和β-蒎烯(12.82%)的含量较高.结论:本方法简便、高效,可为芳香辛味含挥发性成分药物的成分研究提供参考.%OBJECTIVE: To investigate the volatile chemical constituents of Liquidamobar orientalis. METHODS: HS-SPME was used to extract the volatile chemical constituents and GC-MS was used to analyze the volatile chemical constituents. RESULTS: 28 compounds were identified, which accounts for 90.72% of the total GC peak area, of which the amounts of the volatile chemical constituents a-pinene( 15.97%),camphene( 13.28%) and ^-pinene (12.82%) had taken a larger part. CONCLUSION: The method employed in the study is convenient and efficient, and the study can serve as a reference to researches on aromatic and pungent Pharmaceuticals with volatile constituents.

  18. Analysis of Volatile oil from Flos Chrysanthemi by GC-MS%菊花挥发油成分的GC-MS分析

    Institute of Scientific and Technical Information of China (English)

    郭昌洪; 黄爱华; 许汉香

    2012-01-01

    目的:对菊花的挥发油成分进行分析,为菊花的综合利用提供指导.方法:采用水蒸气蒸馏法提取菊花挥发油,经乙酸乙酯萃取处理,以GC-MS法分析其化学成分.结果:在菊花的挥发油中检测出74个化合物,确认了其中24个.结论:菊花挥发油中主要成分中,1-甲基-5-亚甲基-8-异丙基-1,6-环癸二烯(15.777%)含量最高,有7个化合物为以往文献中未曾报道.%Objective; To analyze the constituents of volatile oil from Chrysanthemum to provide guidance for comprehensive utilization of Chrysanthemum. Method: The volatile oil from Chrysanthemum was extracted by steam distillation followed by ethyl acetate extraction. The chemical compositions were analyzed by GC-MS method. Result: Seventy-four compounds of volatile oil from Chrysanthemum were detected, among them, 24 ones were confirmed. Conclusion; Among the constituents in volatile oil from Chrysanthemum, l-methyl-methylene-8-isopropyl-l ,6-ring-5-decadiene (15.777% ) is the main component, and 7 other compounds have not bepn reported in the literature before.

  19. 空气及非金属材料脱气中苯的GC/MS-SIM分析方法%GC/MS- SIM Analysis Method for Benzene in Ambient Air and Offgas of Nonmetal Material

    Institute of Scientific and Technical Information of China (English)

    于芳; 何正杰; 姜洁; 何新

    2001-01-01

    We have built GC/MS - SIM analysis method for benzene in ambient air and offgas of nonmetal material and determined the concentration of benzene in the offgas of a kind of nonmetal material with external standard quantity method.

  20. Multiresidue pesticide analysis of ginseng powders using acetonitrile- or acetone-based extraction, solid-phase extraction cleanup, and gas chromatography-mass spectrometry/selective ion monitoring (GC-MS/SIM) or -tandem mass spectrometry (GC-MS/MS).

    Science.gov (United States)

    Wong, Jon W; Zhang, Kai; Tech, Katherine; Hayward, Douglas G; Krynitsky, Alexander J; Cassias, Irene; Schenck, Frank J; Banerjee, Kaushik; Dasgupta, Soma; Brown, Don

    2010-05-26

    A multiresidue method for the analysis of 168 pesticides in dried powdered ginseng has been developed using acetonitrile or acetone mixture (acetone/cyclohexane/ethyl acetate, 2:1:1 v/v/v) extraction, solid-phase extraction (SPE) cleanup with octyl-bonded silica (C(8)), graphitized carbon black/primary-secondary amine (GCB/PSA) sorbents and toluene, and capillary gas chromatography-mass spectrometry/selective ion monitoring (GC-MS/SIM) or -tandem mass spectrometry (GC-MS/MS). The geometric mean limits of quantitation (LOQs) were 53 and 6 microg/kg for the acetonitrile extraction and 48 and 7 microg/kg for the acetone-based extraction for GC-MS/SIM and GC-MS/MS, respectively. Mean percent recoveries and standard deviations from the ginseng fortified at 25, 100, and 500 microg/kg using GC-MS/SIM were 87 +/- 10, 88 +/- 8, and 86 +/- 10% from acetonitrile extracts and 88 +/- 13, 88 +/- 12, and 88 +/- 14% from acetone mixture extracts, respectively. The mean percent recoveries from the ginseng at the 25, 100, and 500 microg/kg levels using GC-MS/MS were 83 +/- 19, 90 +/- 13, and 89 +/- 11% from acetonitrile extracts and 98 +/- 20, 91 +/- 13, and 88 +/- 14% from acetone extracts, respectively. Twelve dried ginseng products were found to contain one or more of the following pesticides and their metabolites: BHCs (benzene hexachlorides, alpha-, beta-, gamma-, and delta-), chlorothalonil, chlorpyrifos, DDT (dichlorodiphenyl trichloroethane), dacthal, diazinon, iprodione, quintozene, and procymidone ranging from 4000 microg/kg. No significant differences were found between the two extraction solvents, and GC-MS/MS was found to be more specific and sensitive than GC-MS/SIM. The procedures described were shown to be effective in screening, identifying, confirming, and quantitating pesticides in commercial ginseng products.