WorldWideScience

Sample records for cromatografia gasosa gc

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

    Directory of Open Access Journals (Sweden)

    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.

  2. Determinação de compostos nitrogenados aromáticos em alcatrão de carvão através da cromatografia gasosa bidimensional abrangente acoplada à espectrometria de massas

    OpenAIRE

    Juliana Macedo da Silva

    2014-01-01

    A cromatografia gasosa bidimensional abrangente (GC×GC) é uma excelente técnica analítica para a determinação de diversos compostos em matrizes complexas, como é o caso do alcatrão de carvão, objeto deste estudo. O alcatrão foi obtido através do processo de pirólise e submetido à análise por GC×GC visando a especiação de compostos nitrogenados aromáticos. A GC×GC acoplada à espectrometria de massas com analisadores do tipo quadrupolar (qMS) e por tempo de voo (TOFMS) foram utilizados para a d...

  3. (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

    Directory of Open Access Journals (Sweden)

    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

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

    Directory of Open Access Journals (Sweden)

    Marina Venzon Antunes

    2008-01-01

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

  5. 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

    Directory of Open Access Journals (Sweden)

    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

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

    Directory of Open Access Journals (Sweden)

    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

  7. 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

    Directory of Open Access Journals (Sweden)

    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.

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

    Directory of Open Access Journals (Sweden)

    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.

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

    Directory of Open Access Journals (Sweden)

    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.

  10. 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

    Directory of Open Access Journals (Sweden)

    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

  11. 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

    Directory of Open Access Journals (Sweden)

    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%.

  12. 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

    Directory of Open Access Journals (Sweden)

    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.

  13. 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)

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

    Directory of Open Access Journals (Sweden)

    Izabela Miranda de Castro

    2008-01-01

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

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

    Directory of Open Access Journals (Sweden)

    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.

  16. 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

    Directory of Open Access Journals (Sweden)

    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.

  17. 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

    Directory of Open Access Journals (Sweden)

    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

  18. 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

    Directory of Open Access Journals (Sweden)

    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.

  19. 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

    Directory of Open Access Journals (Sweden)

    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.

  20. 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

    Directory of Open Access Journals (Sweden)

    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.

  1. 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.

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

    Directory of Open Access Journals (Sweden)

    José Carlos P. Penteado

    2008-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Trevizan Luiz Roberto Pimentel

    2000-01-01

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

  4. INFLUÊNCIA DE DIFERENTES TIPOS DE EMBALAGENS NAS CARACTERÍSTICAS FÍSICO-QUÍMICAS E COMPOSIÇÃO GASOSA DE BRÓCOLIS (Brassica oleracea L. var Itálica ORGÂNICOS MINIMAMENTE PROCESSADOS E ARMAZENADOS SOB REFRIGERAÇÃO

    Directory of Open Access Journals (Sweden)

    M. L. PADULA

    2009-01-01

    Full Text Available

    Este trabalho teve como objetivo avaliar os efeitos dos diferentes tipos de embalagens na vida útil de brócolis (Brassica oleracea orgânicos minimamente processados e armazenados sob refrigeração. As amostras foram selecionadas e higienizadas, centrifugadas e acondicionados em embalagens de polipropileno (PP, câmara de acrílico hermeticamente selada e com canais abertos à 10ºC por doze dias. Para avaliar a vida útil do produto foram realizadas análises físico-químicas a cada três dias e de composição gasosa, em função de O2 e CO2, diariamente durante dez dias, por cromatografia gasosa. Os resultados mostraram que a umidade das amostras não foi afetada significativamente pelo período de armazenamento. O pH, acidez total titulável e o conteúdo de sólidos solúveis aumentaram ao longo do período de armazenamento. A perda de massa durante o armazenamento foi inferior a 1% em todas as amostras analisadas. A embalagem que melhor preservou a textura dos brócolis ao longo do período de armazenamento foi a de acrílico selado. A degradação das clorofilas a e b, e a síntese de carotenóides foram mais acentuadas nas flores das amostras acondicionadas em acrílico com canais abertos. A composição gasosa apresentou comportamento similar ao observado na literatura. Os dados experimentais de concentração apresentaram bom ajuste aos dados da literatura.

  5. 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

  6. 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.

  7. Implementação e validação de um método de avaliação do perfil de ácidos gordos e do teor de gordura em alimentos por cromatografia gasosa

    OpenAIRE

    Sousa, Laura Cristina Oliveira

    2011-01-01

    Nos dias de hoje é necessário criar hábitos de vida mais saudáveis que contribuam para o bem-estar da população. Adoptar medidas e práticas de modo regular e disciplinado, pode diminuir o risco do aparecimento de determinadas doenças, como a obesidade, as doenças cardiovasculares, a hipertensão, a diabetes, alguns tipos de cancro e tantas outras. É também importante salientar que, uma alimentação cuidada dá saúde e aumenta a esperança média de vida. Em Portugal, nos últimos anos, os costumes ...

  8. 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.

  9. 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.

  10. 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.

  11. Determinación de aminas aromaticas por cromatografia liquida de alta resolución.

    OpenAIRE

    Gutiérrez Bouzán, Mª Carmen; Crespi Rosell, Martí

    1989-01-01

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

  12. A GC Instrument Simulator

    Science.gov (United States)

    Armitage, D. Bruce

    1999-02-01

    the difference between the boiling point of the component and the temperature of the column. The polarity difference between the column packing and the component is also used to modify the retention time. The retention time decreases as the difference between the boiling point of the component and the temperature of the column increases, and retention time increases as the polarity of the component approaches the polarity of the column. If the temperature of the column is too low, a warning message is given and the chromatogram does not show that component. There is no "carry-over" to the next chromatogram, as might be the case for an actual instrument. Carrier-gas flow rate is fixed and is not part of the retention-time calculation. Because of this latter condition and the method used to determine retention time, this simulator is not useful for gas chromatography method development and is not intended for such use. The purpose of the simulator is to give a beginning student experience in what happens as column temperature is varied, why one might need temperature programming, why an autosampler might be useful, and the pitfalls of "smart" integrators. When students make mistakes in instrument setup with the simulator the consequences are not damaging to the simulator but might cause serious problems with a real instrument. Hardware and Software Requirements Hardware and software requirements for A GC Instrument Simulator are shown in Table 1. right> right> Shown (right to left) are the main instrument control window and the manual injection window from A GC Instrument Simulator.

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

    Directory of Open Access Journals (Sweden)

    Aldemir da Silva

    2016-06-01

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

  14. Theoretical study of GC+/GC base pair derivatives

    International Nuclear Information System (INIS)

    Meng Fancui; Wang Huanjie; Xu Weiren; Liu Chengbu

    2005-01-01

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

  15. 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.

  16. Solvents orgànics en electroforesi capil·lar i cromatografia de líquids

    OpenAIRE

    Subirats i Vila, Xavier

    2007-01-01

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

  17. Hidrólise do óleo de Azadirachta indica em água subcrítica e determinação da composição dos triacilglicerídeos e ácidos graxos por cromatografia gasosa de alta resolução a alta temperatura e cromatografia gasosa de alta resolução acoplada à espectrometria de massas Hydrolysis of Azadirachta indica oil using subcritical water and determination of triacylglycerides and fat acids by HT-HRGC-FID and HRGC-MS

    Directory of Open Access Journals (Sweden)

    Jair Sebastião da Silva Pinto

    2010-01-01

    Full Text Available The development of modern analytical tools plays an important role in quality control. The main purpose of this study was to explore the use of subcritical water as a versatile analytical tool, employed simultaneously as a reagent and solvent, as well as the application of high temperature-high resolution gas chromatography (HT-HRGC to develop a procedure for the analysis of triacylglycerides and fatty acids in Azadirachta indica A. Juss. (Neem oil without the need for solvents, chemical reagents, or catalytic agents. The developed method presented satisfactory results and is in agreement with the concepts of Green Analytical Chemistry (GAC.

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

    Science.gov (United States)

    Kubwabo, C; Rollmann, B; Tilquin, B

    1993-04-01

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

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

    OpenAIRE

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

    2001-01-01

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

  20. Salvia officinalis (Lamiaceae) Lin. : caracterização química, atividade citotóxica e apoptótica em células de mamíferos

    OpenAIRE

    Garcia, Charlene Silvestrin Celi

    2014-01-01

    Salvia officinalis (Lamiaceae), conhecida popularmente como sálvia, tem sido muito utilizada no sul do Brasil como condimento nos alimentos, tintura hidroalcoólica e chá para o tratamento de vários distúrbios de saúde. As propriedades dessa planta são estudadas por apontar possíveis mecanismos de ação antioxidante e antitumoral. Neste trabalho, o extrato hidroalcoólico e aquoso de sálvia foram analisados quimicamente por meio de cromatografia gasosa acoplada a espectrômetro de massas (GC-MS) ...

  1. 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.

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

    Directory of Open Access Journals (Sweden)

    Flaviana G. da Silva

    2015-10-01

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

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

    Science.gov (United States)

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

    2003-01-01

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

  4. 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...

  5. 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.

  6. 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

  7. Admission levels of serum Gc-globulin

    DEFF Research Database (Denmark)

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

    1996-01-01

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

  8. Estudo de nitro-hidrocarbonetos policíclicos aromáticos em partículas atmosféricas ultrafinas associadas a técnicas analíticas de cromatografia gasosa com detecção por captura de elétrons e sensoriamento remoto

    OpenAIRE

    Karine Oliveira Garcia

    2013-01-01

    Os nitro-hidrocarbonetos policíclicos aromáticos (NPAHs – nitro-polycyclic aromatic hydrocarbons) são compostos orgânicos constituídos de dois ou mais anéis benzênicos ligados ao grupo nitro (NO2). Tais compostos são amplamente distribuídos no meio ambiente e associados a partículas atmosféricas. O objetivo do presente estudo foi identificar os grupos funcionais dos NPAHs associados ao PM1.0 por espectroscopia de infravermelho termal com transformada de Fourier (FTIR – Fourier Transform Infra...

  9. 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.

  10. 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.

  11. Quality Control Of Selected Pesticides With GC

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-07-15

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

  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

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

    Directory of Open Access Journals (Sweden)

    José Lucínio de Oliveira Freire

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

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

    OpenAIRE

    GONÇALVES, Darlene

    2010-01-01

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

  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. GC ‘Multi-Analyte’ Detection Method

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-07-15

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

  17. 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

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

    Directory of Open Access Journals (Sweden)

    David de Holanda Campelo

    2015-10-01

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

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

    OpenAIRE

    Nakovich, Laura

    2003-01-01

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

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

    OpenAIRE

    Diogo Capelin

    2016-01-01

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

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

    OpenAIRE

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

    2008-01-01

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

  2. Cromatografia unificada Unified chromatography

    Directory of Open Access Journals (Sweden)

    Carin von Mühlen

    2004-10-01

    Full Text Available The scope of this study encompasses an overview of the principles of unified chromatography as well as the principles of chromatographic techniques as applied to unified systems, which include gas chromatography, liquid chromatography, supercritical fluid chromatography, high temperature and high pressure liquid chromatography, micro-liquid chromatography, enhanced fluidity chromatography, and solvating gas chromatography. Theoretical considerations and individual instrumental parameters such as mobile phase, sample introduction system, columns, and detection system are also discussed. Future applications of this separation approach are discussed.

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

    OpenAIRE

    Glaucia Maria Ferreira Pinto

    2002-01-01

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

  4. Modern methods of sample preparation for GC analysis

    NARCIS (Netherlands)

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

    2009-01-01

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

  5. 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

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

    DEFF Research Database (Denmark)

    Pihl, Tina Holberg

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

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

    NARCIS (Netherlands)

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

    2006-01-01

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

  8. Determination of selected organophosphorus pesticides using GC ...

    African Journals Online (AJOL)

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

  9. DETERMINAÇÃO DE POPS E AGROTÓXICOS EM LEITE MATERNO EMPREGANDO CROMATOGRAFIA A GÁS ACOPLADA À ESPECTROMETRIA DE MASSAS COM IONIZAÇÃO QUÍMICA NEGATIVA (GC-NCI-MS)

    OpenAIRE

    Mariela de Souza Viera

    2016-01-01

    A Convenção de Estocolmo foi a primeira atitude mundial a tentar preservar a saúde humana e o ambiente do uso indiscriminado de agrotóxicos, especialmente os poluentes orgânicos persistentes (POPs), que se caracterizam por serem lipofílicos podendo bioacumular nos tecidos adiposos e também no leite materno. Porém, os POPs constituem apenas uma parte dos produtos químicos com potencial de contaminação ambiental e humana uma vez que novas substâncias estão constantemente sendo desenvolvidas e l...

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

    Science.gov (United States)

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

    2002-01-01

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

  11. 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.

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

    DEFF Research Database (Denmark)

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

    2010-01-01

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

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

    OpenAIRE

    Yamamoto, Nobuto; Suyama, Hirofumi; Yamamoto, Nobuyuki

    2008-01-01

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

  14. 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.

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

    Science.gov (United States)

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

    2013-02-05

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

  16. 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

  17. 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

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

    Science.gov (United States)

    2012-01-01

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

  19. 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

  20. 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

  1. 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

  2. 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.

  3. 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

  4. High GC content causes orphan proteins to be intrinsically disordered.

    Directory of Open Access Journals (Sweden)

    Walter Basile

    2017-03-01

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

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

    Directory of Open Access Journals (Sweden)

    Zhitao Niu

    2017-11-01

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

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

    Science.gov (United States)

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

    2017-01-01

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

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

    African Journals Online (AJOL)

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

  8. 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

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

    Directory of Open Access Journals (Sweden)

    Isabela da Costa César

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

  10. A Monolithically-Integrated μGC Chemical Sensor System

    Directory of Open Access Journals (Sweden)

    Davor Copic

    2011-06-01

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

  11. 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.

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

    Science.gov (United States)

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

    2005-09-09

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

  13. 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...

  14. Group separation of organohalogenated contaminants by GCxGC

    Energy Technology Data Exchange (ETDEWEB)

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

    2004-09-15

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

  15. Environmental trace analysis by means of supersensitive GC-IMS

    International Nuclear Information System (INIS)

    Leonhardt, J.W.

    1997-01-01

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

  16. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

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

  18. 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.

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

    Science.gov (United States)

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

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

    Science.gov (United States)

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

    2011-07-01

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

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

    Science.gov (United States)

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

    2005-02-01

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

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

    International Nuclear Information System (INIS)

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

    2004-01-01

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

  3. GC – MS Characterization of Degutted White Grubs' Fatty Acids ...

    African Journals Online (AJOL)

    Fatty acids composition of white grubs examined by GC- MS identified 19 different fatty acids; 11 saturated, 7 monoene and a cyclopropaneoctanoate. The identified ones are Methyl tetradecanoate (C14:0), Methyl dodecanoate (C12:0), Methyl cis – 9 - octadecenote (C18:1), Methyl(7E) – 7 – hexadecenoate (C16:1), Methyl ...

  4. Performance of the future MOMA GC-ITMS instrument

    Science.gov (United States)

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

    2016-10-01

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

  5. GC-Content Normalization for RNA-Seq Data

    Science.gov (United States)

    2011-01-01

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

  6. Middle distillates hydrogen content via GC×GC-FID.

    Science.gov (United States)

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

    2018-08-15

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

  7. 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

  8. 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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2004-04-01

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

  10. G+C content dominates intrinsic nucleosome occupancy

    Directory of Open Access Journals (Sweden)

    Hughes Timothy R

    2009-12-01

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

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

    Science.gov (United States)

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

    2012-06-01

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

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

    Science.gov (United States)

    Ruggiero, Marco; Reinwald, Heinz; Pacini, Stefania

    2016-09-01

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

  13. Analysis of residual solvents in PET radiopharmaceuticals by GC

    International Nuclear Information System (INIS)

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

    2013-01-01

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

  14. Amino acid analysis in biological fluids by GC-MS

    OpenAIRE

    Kaspar, Hannelore

    2009-01-01

    Amino acids are intermediates in cellular metabolism and their quantitative analysis plays an important role in disease diagnostics. A gas chromatography-mass spectrometry (GC-MS) based method was developed for the quantitative analysis of free amino acids as their propyl chloroformate derivatives in biological fluids. Derivatization with propyl chloroformate could be carried out directly in the biological samples without prior protein precipitation or solid-phase extraction of the amino acid...

  15. 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

    Directory of Open Access Journals (Sweden)

    Michella de Albuquerque Lima

    2010-12-01

    Full Text Available 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/Ce. O experimento foi conduzido entre setembro de 2006 e agosto de 2007, na estação experimental da Embrapa Agroindústria Tropical, localizada no município de Paraipaba, Ceará. As variáveis A, g s, E e Ci/Ce foram afetadas apenas em função da época do ano e dos tipos de folhas. A maior influência nos fatores fisiológicos analisados ocorreu devido às condições em que as folhas estavam submetidas (sol ou sombra e aos fatores meteorológicos e não à supressão da irrigação. Isto, possivelmente porque os resultados aqui obtido estejam mais bem relacionados com as fases fenológicas da cultura do que com os tratamentos, demonstrando assim o conspícuo efeito fisiológico da força dos drenos e da irradiância nessas plantas.In this experiment we analyzed the seasonal variations in gas exchange rates of dwarf cashew (Anacardium occidentale L. when exposed to irrigated and rainfed conditions. Full sun and shaded of clones CCP 76 and BRS 189 were monthly assessed for determination of stomatal conductance (g s, transpiration rate (E and photosynthesis (A, internal and external CO2 (Ci/Ce and leaf temperature. The experiment was carried out between September 2006 and August 2007, at the experimental station of Embrapa Agroindústria Tropical, located at Paraipaba County, state of Ceará, Brazil. In general, the variables A, g s, E and Ci/Ce were affected only in terms of time of year and types of leaves. Light influenced the

  16. Gas exchange alteration caused by water deficit during the bean reproductive stage Alterações das trocas gasosas na fase reprodutiva e produtividade do feijão sob déficit hídrico

    Directory of Open Access Journals (Sweden)

    Lauricio Endres

    2010-01-01

    Full Text Available The purpose of the present study was to analyze gas exchanges in leaves and the parameters of productivity of beans (Phaseolus vulgaris, L. submitted to two water deficiency periods during which three water regimes were employed: W1 (1,0 ETo during the entire plant cycle; W2 (1,0 ETo up to the flowering period and irrigation interruption from the 37 to the 51st day following sowing, and W3 (in addition to the reproductive phase, water deficit was also applied during the vegetative stage. Photosynthesis was one of the main physiological factors affected by water deficit. This was not only caused by the stomata closure, but also by carboxilation reduction due to metabolic damage. This effect was, however, offset 24 h after rehydration. During flowering, the water deficit caused crop productivity to drop significantly, reducing the number of pods and the number of seeds per pod, independently of the water deficit during the vegetative stage. The weight of 100 seeds however, was the same regardless of treatment. These results suggest that the water deficit caused the reduction of photo-assimilates, which affected grain productivity. Nevertheless, once properly formed, seeds developed totally; a strategy of the plant to produce less seeds under stress, but viable to perpetuate the species.Neste trabalho, se analisaram as trocas gasosas das folhas e parâmetros de produtividade de feijão (Phaseolus vulgaris, L. submetido a dois períodos de deficiência hídrica e se empregaram três regimes hídricos, a saber: W1 (1,0 ETo durante todo o ciclo da cultura; W2 (1,0 ETo até a floração e suspensão da irrigação do 37 ao 51º dia após a semeadura (DAS, correspondendo à fase de floração e W3 (além da fase reprodutiva também se aplicou um déficit hídrico durante a fase vegetativa. A fotossíntese foi um dos principais fatores fisiológicos afetados pelo déficit hídrico devido não só ao fechamento estomático, mas, também, à redução da

  17. 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

  18. Photosynthetic CO2 fixation in guard cells (GC)

    International Nuclear Information System (INIS)

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

    1987-01-01

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

  19. Clinical experience of integrative cancer immunotherapy with GcMAF.

    Science.gov (United States)

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

    2013-07-01

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

  20. 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%.

  1. 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.

  2. 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.

  3. [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.

  4. 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.

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

    Science.gov (United States)

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

    2007-08-01

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

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

    OpenAIRE

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

    2016-01-01

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

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

    Science.gov (United States)

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

    2016-01-29

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

  8. GC/MS determination of monosaccharides in yogurt products

    Energy Technology Data Exchange (ETDEWEB)

    Nam, Sang Kyu; Cheong, Won Jo [Inha Univ., Incheon (Korea, Republic of)

    2000-02-01

    Yogurt products are known to be effective for enhancing health and preventing diseases such as cancers. Such effects are generally believed to be due to actions of polysaccharides in yogurt products. In this study we have determined compositions of monosaccharides in hydrolysates of commercial yogurt products as the first step of understanding structures of polysaccharides. The yogurt products were ultracentrifuged, filtered, hydrolyzed in 1M sulfuric acid and neutralized. A porting of the solution was taken and evaporated to dryness, derivatized with TMSI (trimethyl- silylimidazole) and analyzed by GC/MS. We found that the monosaccharides were fructose, glucose, and galactose. Their compositions were variant among several yogurt products.

  9. GC/MS determination of monosaccharides in yogurt products

    International Nuclear Information System (INIS)

    Nam, Sang Kyu; Cheong, Won Jo

    2000-01-01

    Yogurt products are known to be effective for enhancing health and preventing diseases such as cancers. Such effects are generally believed to be due to actions of polysaccharides in yogurt products. In this study we have determined compositions of monosaccharides in hydrolysates of commercial yogurt products as the first step of understanding structures of polysaccharides. The yogurt products were ultracentrifuged, filtered, hydrolyzed in 1M sulfuric acid and neutralized. A porting of the solution was taken and evaporated to dryness, derivatized with TMSI (trimethyl- silylimidazole) and analyzed by GC/MS. We found that the monosaccharides were fructose, glucose, and galactose. Their compositions were variant among several yogurt products

  10. Economics of LNG and pipeline gas export from GC C

    International Nuclear Information System (INIS)

    White, N.

    1995-01-01

    This paper briefly reviews the economic and non-economic considerations underlying gas exports from the GC C and the Arabian Peninsula in general. It addresses four themes: policy issues, political risks, technical risks and economics. It examines the distance between the regional resource areas and the major gas markets in the Far East and Europe, and examines the implications for moving gas to those markets in liquid form or by pipeline, in terms of number of LNG vessels required, and capital costs. (Author)

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

    Science.gov (United States)

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

    2010-04-01

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

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

    NARCIS (Netherlands)

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

    1997-01-01

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

  13. 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...

  14. 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.

  15. 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

  16. 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.

  17. GC Analyses of Salvia Seeds as Valuable Essential Oil Source

    Directory of Open Access Journals (Sweden)

    Mouna Ben Taârit

    2014-01-01

    Full Text Available The essential oils of seeds of Salvia verbenaca, Salvia officinalis, and Salvia sclarea were obtained by hydrodistillation and analyzed by gas chromatography (GC and GC-mass spectrometry. The oil yields (w/w were 0.050, 0.047, and 0.045% in S. verbenaca, S. sclarea, and S. officinalis, respectively. Seventy-five compounds were identified. The essential oil composition of S. verbenaca seeds showed that over 57% of the detected compounds were oxygenated monoterpenes followed by sesquiterpenes (24.04% and labdane type diterpenes (5.61%. The main essential oil constituents were camphor (38.94%, caryophyllene oxide (7.28%, and 13-epi-manool (5.61%, while those of essential oil of S. officinalis were α-thujone (14.77%, camphor (13.08%, and 1,8-cineole (6.66%. In samples of S. sclarea, essential oil consists mainly of linalool (24.25%, α-thujene (7.48%, linalyl acetate (6.90%, germacrene-D (5.88%, bicyclogermacrene (4.29%, and α-copaene (4.08%. This variability leads to a large range of naturally occurring volatile compounds with valuable industrial and pharmaceutical outlets.

  18. 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. 

  19. 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.

  20. 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.

  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. Trocas gasosas em plantas de girassol submetidas à deficiência hídrica em diferentes estádios fenológicos Gas exchange in sunflower plants subjected to water deficit at different stages of growth

    Directory of Open Access Journals (Sweden)

    Alexandre Reuber Almeida da Silva

    2013-03-01

    Full Text Available Este estudo avaliou as respostas das trocas gasosas do girassol quando submetido à regimes de déficit hídrico em seus diferentes estádios fenológicos. O experimento foi conduzido em Pentecoste, CE, sob delineamento experimental em blocos casualizados, em esquema de parcelas subdivididas no tempo, com oito parcelas, três subparcelas e quatro blocos. Nas parcelas, foram avaliadas as épocas de indução do déficit hídrico nos diferentes estádios fenológicos (vegetativo, floração e formação da produção, correspondendo à ocorrência de déficit hídrico em um, dois ou três estádios, e nas subparcelas, as épocas de avaliação das características fisiológicas, que corresponderam ao término de cada fase (52; 68 e 110 dias após a semeadura - DAS. A cultura foi irrigada com uma lâmina equivalente a 100% da evapotranspiração de referência (ETo e o déficit hídrico foi imposto com metade da lâmina que foi aplicada no tratamento controle. As épocas de avaliação influenciaram a maioria das variáveis analisadas, com exceção da eficiência intrínseca de uso da água. Os resultados de temperatura foliar e taxas de fotossíntese, transpiração, condutância estomática, concentração interna de CO2 e as eficiências instantâneas e intrínsecas do uso da água, não mostraram efeitos em relação ao nível de déficit hídrico avaliado, independentemente da época em que os mesmos foram aplicados. A fotossíntese e a transpiração decresceram com o estádio de desenvolvimento da cultura, causando reduções na eficiência instantânea de uso da água. Portanto, conclui-se que a cultura pode ser irrigada com 50% da ETo, durante todo o ciclo sem danos no processo fotossintético.This study evaluated gas-exchange responses of the sunflower when subjected to water deficit at different stages of growth. The experiment was carried out at Pentecost, in the state of Ceara, in a randomized-block design of time-split plots

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

    Directory of Open Access Journals (Sweden)

    Maayan Amit

    2012-05-01

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

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

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

    Science.gov (United States)

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

    2016-01-01

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

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

    Science.gov (United States)

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

    2016-01-01

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

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

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

    Science.gov (United States)

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

    2015-01-01

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

  9. 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.

  10. Sterol Profile for Natural Juices Authentification by GC-MS

    Science.gov (United States)

    Culea, M.

    2007-04-01

    A GC-MS analytical method is described for some natural juices analysis. The fingerprint of sterols was used to characterize the natural juice. A rapid liquid-liquid extraction method was used. The sterols were separated on a Rtx-5MS capillary column, 15m×0.25mm, 0.25μm film thickness, in a temperature program from 50°C for 1 min, then ramped at 15°C/min to 300°C and held for 15 min. Identification of sterols and their patterns were used for juice characterization. The sterol profile is a useful approach for confirming the presence of juices of orange, grapefruit, pineapple and passion fruit in compounded beverages and for detecting of adulteration of fruit juices.

  11. Sterol Profile for Natural Juices Authentification by GC-MS

    International Nuclear Information System (INIS)

    Culea, M.

    2007-01-01

    A GC-MS analytical method is described for some natural juices analysis. The fingerprint of sterols was used to characterize the natural juice. A rapid liquid-liquid extraction method was used. The sterols were separated on a Rtx-5MS capillary column, 15mx0.25mm, 0.25μm film thickness, in a temperature program from 50 deg. C for 1 min, then ramped at 15 deg. C/min to 300 deg. C and held for 15 min. Identification of sterols and their patterns were used for juice characterization. The sterol profile is a useful approach for confirming the presence of juices of orange, grapefruit, pineapple and passion fruit in compounded beverages and for detecting of adulteration of fruit juices

  12. GC/MS confirmatory method for etorphine in horse urine

    Energy Technology Data Exchange (ETDEWEB)

    Bonnaire, Y.; Plou, P. (Laboratoire de la Federation Nationale des Societes de Courses, Chatenay-Malabry (France)); Pages, N.; Boudene, C. (Universite de Paris XI (France)); Jouany, J.M. (Universite de Rouen (France))

    A highly sensitive procedure for GC/MS determine of etorphine in horse urine is described. This assay provides both specificity and reliability and is particularly well suited for the confirmation of radioimmunoassay screening procedures usually used for etorphine. After solvent extraction and purifications, the etorphine is characterized as a pentafluoroacetic derivative (PFAA) by using mass fragmentography. The detection limit is O.1 ng/mLin urine; the coefficient of variation of the estimations is 10.9%. The procedure has been validated after on-field administration of 5 to 90 {mu}g of etorphine to five thoroughbred horses of 5 to 90 {mu}g of etorphine to five thoroughbred horses (10 to 180 ng/kg).

  13. GC/MS confirmatory method for etorphine in horse urine

    International Nuclear Information System (INIS)

    Bonnaire, Y.; Plou, P.; Pages, N.; Boudene, C.; Jouany, J.M.

    1989-01-01

    A highly sensitive procedure for GC/MS determine of etorphine in horse urine is described. This assay provides both specificity and reliability and is particularly well suited for the confirmation of radioimmunoassay screening procedures usually used for etorphine. After solvent extraction and purifications, the etorphine is characterized as a pentafluoroacetic derivative (PFAA) by using mass fragmentography. The detection limit is O.1 ng/mLin urine; the coefficient of variation of the estimations is 10.9%. The procedure has been validated after on-field administration of 5 to 90 μg of etorphine to five thoroughbred horses of 5 to 90 μg of etorphine to five thoroughbred horses (10 to 180 ng/kg)

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

    OpenAIRE

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

    2016-01-01

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

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

    International Nuclear Information System (INIS)

    Uto, Yoshihiro; Hori, Hitoshi

    2013-01-01

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

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

    OpenAIRE

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

    2016-01-01

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

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-09-03

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-03-15

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

  20. 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

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

    Science.gov (United States)

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

    2017-11-01

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

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

    Science.gov (United States)

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

    2018-02-01

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

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

    Science.gov (United States)

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

    2001-01-01

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

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

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

    NARCIS (Netherlands)

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

    1996-01-01

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

  8. 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.

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

    Science.gov (United States)

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

    2013-03-01

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

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

    DEFF Research Database (Denmark)

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

    2010-01-01

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

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

    DEFF Research Database (Denmark)

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

    2010-01-01

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

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

    Science.gov (United States)

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

    2015-09-03

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

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

    NARCIS (Netherlands)

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

    1988-01-01

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

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

    Science.gov (United States)

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

    2015-08-01

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

  15. 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.

  16. Quantitative determination of phenobarbital derivatives by GC-MS

    International Nuclear Information System (INIS)

    Gal, J.; Hodshon, B.J.; Cho, A.K.

    1975-01-01

    Analytical methods based on stable isotope labeling in conjunction with gas chromatography-mass spectrometry have been developed for the new anticonvulsant 1,3-bis(methoxymethyl)phenobarbital and two of its metabolites, 1-methoxymethylphenobarbital and phenobarbital. Deuterium-labeled analogs of the three compounds were synthesized for use as internal standards in measuring the concentration of the unlabeled drug and its metabolites in biological fluids. The compounds were extracted from the acidified biological fluid, and the parent drug was separated from its two metabolites. The latter were methylated with diazomethane before GC-MS analysis. Selected ions in the spectra of the three compounds and their respective internal standards were monitored using a quadrupole mass spectrometer controlled by a digital selected ion monitor. The sensitivity of the assay was 50 pmoles/ml for each compound. The method was applied to the study of the plasma and brain levels of the three compounds in the rat after intravenous administration of the parent drug (6 mg/kg). Rapid formation of the two metabolites was observed, and accumulation of phenobarbital in the rat brain was found. The plasma levels of the three compounds were also measured in man after oral doses. It was concluded that a significant aspect of the anticonvulsant action of 1,3-bis(methoxymethyl) phenobarbital is its rapidconversion in vivo to phenobarbital

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

    International Nuclear Information System (INIS)

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

    1986-01-01

    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 3 H-piperidino- 14 C-cyano-PCC (synthesized in the lab and recrystallized twice, m.p. 67 0 C) and burned under conditions which simulated smoking. Mainstream smoke was passed through glass wool filters and H 2 SO 4 and NaOH traps. Tritium and 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 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%)

  18. 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.

  19. Microembolia gasosa em operação cardíaca com uso de circulação extracorpórea: emprego de shunt venoarterial como método preventivo Gaseous microemboli in cardiac surgery with cardiopulmonary bypass: the use of veno-arterial shunt as a preventive method

    Directory of Open Access Journals (Sweden)

    Edison Emidio dos Reis

    2012-09-01

    Full Text Available As complicações neurológicas representam importante causa de morbidade no período pós-operatório de cirurgia cardíaca e sua incidência alcança até 75% dos pacientes. Uma importante causa desses eventos é a formação de microbolhas na corrente sanguínea durante a circulação extracorpórea. Realizou-se revisão integrativa sobre microembolia gasosa na circulação extracorpórea. Esse trabalho analisou estudos com abordagens metodológicas diferentes, mas que contemplam o tema. O resultado sugere que a desnitrogenação do sangue causada pela hiperoxia dissolve microbolhas formadas no sangue e o shunt venoarterial pode equilibrar os parâmetros respiratórios alterados pela hiperoxia.Neurological complications are an important cause of morbidity in the postoperative period of cardiac surgery and its incidence reaches up to 75% of patients. An important cause of these events is the formation of microbubbles in the bloodstream during cardiopulmonary bypass. Integrative review was carried out on gaseous microemboli in cardiopulmonary bypass. This study analyzed studies with different methodological approaches, but that address the issue. The result suggests the denitrogenation of blood by hyperoxia dissolved microbubbles in the blood and venoarterial shunt can balance the respiratory parameters changed with hyperoxia.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2004-02-01

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

  1. 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.

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

    Directory of Open Access Journals (Sweden)

    Marie-Claude Marsolier-Kergoat

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

  3. A new ppb-gas analyzer by means of GC-ion mobility spectrometry (GC-IMS)

    International Nuclear Information System (INIS)

    Leonhardt, J.W.

    2003-01-01

    IMS-detectors are using beta-sources like tritium or nickel-63. This detection principle uses fast ion-molecular reactions between air cluster ions, produced by beta ionization and the analyte. The system works at normal pressure, the very high sensitivity and selectivity is used widely in industry, research, medicine and environmental control. In the last few years especially, small tritium sources were reduced to a level of some 50 MBq, which is 20 times less than the exemption levels for these sources. One of the handicaps of that technology is the problem of cross sensitivities. To overcome these problems a special GC-column of 1 m length has been included into the gas inlet and mixtures of compounds get separated by their retention times before entering the drift sensor. By means of that method a new analytical quality of IMS is arrived. The application of these analytical devices got a spin off in the last year. The main applications being discussed are as follows: (1) anti terror systems in buildings and facilities, (2) working place monitoring in chemical industry, (3) microelectronics: HF, HCl, Cl 2 , NMP, NH 3 , NO 2 , SO 2 , (4) environment: NH 3 , HCN, HCl, CH 2 O, organic compounds, SO 2 , NO 2 , (5) gas and petrol: gas-carottage, H 2 S, mercaptans, (6) household, furniture: solvents, clue, organic vapour from furniture, and (7) health care: diagnostics of various diseases. (author)

  4. 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

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

    Science.gov (United States)

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

    2016-09-06

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

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

    Science.gov (United States)

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

    2017-01-01

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

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

    Science.gov (United States)

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

    2016-07-01

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

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

    Science.gov (United States)

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

    2013-07-01

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

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

    Science.gov (United States)

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

    2013-07-01

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

  10. 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.

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

    Science.gov (United States)

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

    2000-05-01

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

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

    Science.gov (United States)

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

    2015-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Jie Yu Chen

    2009-08-01

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

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

    Science.gov (United States)

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

    2018-02-01

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

  15. 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

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

    OpenAIRE

    Andrea Scabora Boix Caro

    2002-01-01

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

  17. 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

  18. Gc/ms analysis of coal tar composition produced from coal

    African Journals Online (AJOL)

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

  19. VOLATILE ORGANO-METALLOIDS IN BIO-SOLID MATERIALS: ANALYSIS BY VACUUM DISTILLATION-GC/MS

    Science.gov (United States)

    An analytical method based on vacuum distillation-gas chromatography-mass spectrometry (VD-GC-MS)was developed for determining volatile organo-metalloid contaminants in bio-solid materials. Methodperformance was evaluated for dimethylselenide (DMSe), dimethyldisel...

  20. 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

  1. Crescimento, trocas gasosas e potencial osmótico da bananeira-'Prata', submetida a diferentes doses de sódio e cálcio em solução nutritiva Growth, gaseous exchange and osmotic potential of banana 'Prata' plants, exposed to different concentrations of sodium and calcium in nutritive solution

    Directory of Open Access Journals (Sweden)

    LUDMILA LAFETÁ DE MELO NEVES

    2002-08-01

    Full Text Available O cálcio vem sendo utilizado com o intuito de incrementar tolerância a sais nas plantas, pois sabe-se que a salinidade restringe o crescimento e a produtividade de muitas culturas. Este estudo teve por objetivo avaliar os efeitos da aplicação de sódio e cálcio sobre o crescimento inicial, trocas gasosas e potencial osmótico da bananeira (Musa spp. 'Prata' (AAB. Foi utilizado o delineamento experimental em blocos casualizados, com arranjo fatorial 4 x 4 [ 4 doses de sódio ( 0; 5; 10; 15 mmol L-1 e 4 de cálcio ( 2; 4; 8; 12 mmol L-1] e 3 repetições. A emissão total de folhas e o potencial osmótico das plantas não foram influenciados pelos tratamentos. O aumento dos níveis de sódio na solução promoveu redução significativa na massa fresca da parte aérea, altura, área foliar, diâmetro do pseudocaule e massa seca das plantas. A presença de 5 mmol L-1 de Na na solução favoreceu as trocas gasosas. O aumento dos níveis de cálcio na solução promoveu a redução da massa fresca da parte aérea, altura e área foliar da bananeira-'Prata'.The Calcium has been used to increase salt tolerance in plants since salinity restricts growth and productivity in many crops. This study was conducted with the objective of evaluating the effects of sodium and calcium application on the initial growth, gaseous exchange and osmotic potential of banana (Musa spp. 'Prata' plants (AAB. The experimental layout was a 4 x 4 factorial with three replicates in a randomized complete block design. The factors tested were concentrations of sodium (0; 5; 10; 15 mmol L-1 and calcium (2; 4; 8; 12 mmol L-1. The total emition of leaves and the osmotic potential of the plants were not influenced by the treatments. However, the increase in concentrations of sodium in the nutritive solution resulted in significant reduction of the fresh weight of aerial plant parts, height and leaf area of the plants, diameter of the pseudostem, and dry weight of the plants. The

  2. Assessment of organochlorine pesticides and atrazine residues in Maize Produced in Ghana using GC-ECD/ GC-MS

    International Nuclear Information System (INIS)

    Miensah, E.D.

    2015-07-01

    Maize is consumed by over 95% of the Ghanaian populace and the practice of using atrazine, lindane and other organochlorine pesticides in its production has raised concerns about potential adverse effects on human health and the environment. A field survey was conducted in this study to assess farmers’ knowledge of safe handling and use of these chemicals as well as toxicity awareness and symptoms among farmers and traders. Residues of the pesticides in maize samples as well as the potential health risk associated with exposure to them were also evaluated. Data obtained from the field survey indicate that a large proportion of farmers are at risk of pesticide poisoning through occupational exposure. Over 80 % of applicators do not apply safety precautions during pesticide mixing and application; resulting in considerable prevalence of pesticide related illnesses in the study area. Residues of lindane and atrazine were below detection limits of 0.005 mg/kg and 0.010 mg/kg respectively of the GC-ECD/MS used for the analysis; except in the Ashanti region where atrazine was 0.05 mg/kg which is within the EU-MRL of 0.1 mg/kg. However, minute concentrations of other organochlorines (endrin- 0.007 mg/kg; heptachlor- 0.023 mg/kg; alpha-endosulfan- 0.013 mg/kg) were found in maize samples from Brong Ahafo, Eastern, Central and Upper west regions. Though endrin and alpha-endosulfan were below the EU-MRL of 0.01 mg/kg and 0.10 mg/kg respectively, heptachlor was slightly above the EU-MRL of 0.01 mg/kg. The estimated doses for all these other organochlorines pesticides do not pose direct hazard to human health because their estimated dose values were lower than toxic thresholds and reference doses. However, due to the unsafe application practices by applicators, there exists a potential risk for systemic and carcinogenic health effects by these chemicals in the study area. (au)

  3. 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.

  4. 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.

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

    International Nuclear Information System (INIS)

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

    1984-01-01

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

  6. 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 .

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

    Science.gov (United States)

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

    2007-01-01

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

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

    Science.gov (United States)

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

    2018-05-01

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

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

    Science.gov (United States)

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

    2017-01-01

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

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

    Science.gov (United States)

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

    2017-11-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1999-06-01

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

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

    Directory of Open Access Journals (Sweden)

    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

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

    Science.gov (United States)

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

    2002-09-04

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

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

    Science.gov (United States)

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

    2003-10-01

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

  16. A review on g-C3N4-based photocatalysts

    International Nuclear Information System (INIS)

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

    2017-01-01

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

  17. 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.

  18. 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.

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

    Science.gov (United States)

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

    2011-08-01

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

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

    Science.gov (United States)

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

    2018-05-20

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

  1. 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

  2. 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

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

    Science.gov (United States)

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

    2013-05-01

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

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

    Science.gov (United States)

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

    2008-01-15

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

  5. 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

    Directory of Open Access Journals (Sweden)

    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.

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

    Science.gov (United States)

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

    2015-11-03

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2002-11-01

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

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

    Science.gov (United States)

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

    2014-08-01

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

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

    Science.gov (United States)

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

    2018-04-01

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

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

    International Nuclear Information System (INIS)

    Farheen, R.; Mahmood, I.

    2016-01-01

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

  12. 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.

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Gülin Renda

    2016-01-01

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

  15. 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.

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

    Science.gov (United States)

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

    1994-01-01

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

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

    Science.gov (United States)

    Nikokavoura, Aspasia; Trapalis, Christos

    2018-02-01

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

  18. 1000 human genomes carry widespread signatures of GC biased gene conversion.

    Science.gov (United States)

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

    2018-04-16

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

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

    Science.gov (United States)

    Borges, Chad R; Rehder, Douglas S

    2016-09-15

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

  20. 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.

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

    International Nuclear Information System (INIS)

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

    1993-01-01

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

  2. The GC computer code for flow sheet simulation of pyrochemical processing of spent nuclear fuels

    International Nuclear Information System (INIS)

    Ahluwalia, R.K.; Geyer, H.K.

    1996-01-01

    The GC computer code has been developed for flow sheet simulation of pyrochemical processing of spent nuclear fuel. It utilizes a robust algorithm SLG for analyzing simultaneous chemical reactions between species distributed across many phases. Models have been developed for analysis of the oxide fuel reduction process, salt recovery by electrochemical decomposition of lithium oxide, uranium separation from the reduced fuel by electrorefining, and extraction of fission products into liquid cadmium. The versatility of GC is demonstrated by applying the code to a flow sheet of current interest

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

    Science.gov (United States)

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

    2003-10-22

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

  4. 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.

  5. HS-SPME-GC-MS Analysis of onion (Allium cepa L. and shallot (Allium ascalonicum L.

    Directory of Open Access Journals (Sweden)

    D’Auria, M.

    2017-06-01

    Full Text Available The volatile organic compounds of onion and shallot were determined via HS-SPME-GC-MS. The main components were dipropyldisulphide and allylpropyldisulphide. Thiopropanal S-oxide were detected only in onion volatiles. In shallot is interesting the presence of 2-methyl-2-pentenal, a compound with an intense fruity aroma, that can characterize the different aroma between onion and shallot. The SPME-GC-MS analysis of shallot after absorption on the SPME fiber at 50°C showed the presence of new compounds, whose structures have been discussed.

  6. 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.

  7. Active and realistic passive marijuana exposure tested by three immunoassays and GC/MS in urine

    International Nuclear Information System (INIS)

    Mule, S.J.; Lomax, P.; Gross, S.J.

    1988-01-01

    Human urine samples obtained before and after active and passive exposure to marijuana were analyzed by immune kits (Roche, Amersham, and Syva) and gas chromatography/mass spectrometry (GC/MS). Seven of eight subjects were positive for the entire five-day test period with one immune kit. The latter correlated with GC/MS in 98% of the samples. Passive inhalation experiments under conditions likely to reflect realistic exposure resulted consistently in less than 10 ng/mL of cannabinoids. The 10-100-ng/mL cannabinoid concentration range essential for detection of occasional and moderate marijuana users is thus unaffected by realistic passive inhalation

  8. 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.

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

    OpenAIRE

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

    2013-01-01

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

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

    Science.gov (United States)

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

    2018-04-18

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

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

    Science.gov (United States)

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

    2018-02-01

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

  12. 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.

  13. 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

  14. GC/MS analysis of coal tar composition produced from coal pyrolysis

    African Journals Online (AJOL)

    Coal tar is a significant product generated from coal pyrolysis. A detailed analytical study on its composition and chemical structure will be of great advantage to its further processing and utilization. Using a combined method of planigraphy-gas chromatograph/mass spectroscopy (GC/MS), this work presents a composition ...

  15. Influence of Interleukin-6 (174G/C Gene Polymorphism on Obesity in Egyptian Children

    Directory of Open Access Journals (Sweden)

    Ola M. Ibrahim

    2017-10-01

    CONCLUSION: Our study showed that carriers of the C allele for the IL-6 (174G/C polymorphism have higher BMI. As the G174C polymorphism is likely to affect IL-6 expression and its physiological regulation; consequently this polymorphism may affect adiposity.

  16. 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...

  17. Acid-activated structural reorganization of the Rift Valley fever virus Gc fusion protein

    NARCIS (Netherlands)

    Boer, de S.M.; Kortekaas, J.A.; Spel, L.; Rottier, P.J.M.; Moormann, R.J.M.; Bosch, B.J.

    2012-01-01

    Entry of the enveloped Rift Valley fever virus (RVFV) into its host cell is mediated by the viral glycoproteins Gn and Gc. We investigated the RVFV entry process and its pH-dependent activation mechanism in particular using our recently developed nonspreading RVFV particle system. Entry of the virus

  18. Development of a GC-MS-SPME Method for the Determination of Amines in Meteorites

    Science.gov (United States)

    Hilts, R. W.; Skelhorne, A. W.; Simkus, D.; Herd, C. D. K.

    2016-08-01

    A GC-MS-SPME analytical method for the direct determination of amines in aqueous solution has been developed. The key step in the procedure is the conversion of the amines into their non-volatile ammonium salts by protonation with HCl.

  19. Gas chromatography-mass spectrometry (GC-MS) analysis of extractives of naturally durable wood

    Science.gov (United States)

    G.T. Kirker; A.B. Blodgett; S.T. Lebow; C.A. Clausen

    2011-01-01

    A preliminary study to evaluate naturally durable wood species in an above ground field trial using Gas Chromatography-Mass Spectrometry (GC-MS) detected differences in fatty acid extractives between species and within the same species over time. Fatty acids were extracted with chloroform: methanol mixture then methylated with sodium methoxide and fractionated using...

  20. Determination of methylmercury in cryptogams by means of GC-AFS using enzymatic hydrolysis

    Czech Academy of Sciences Publication Activity Database

    Coufalík, Pavel; Meszarosová, N.; Coufalíková, K.; Zvěřina, O.; Komárek, J.

    2018-01-01

    Roč. 140 (2018), s. 8-13 ISSN 0026-265X Institutional support: RVO:68081715 Keywords : methylmercury * cryptogam * GC-AFS Subject RIV: CB - Analytical Chemistry, Separation OBOR OECD: Analytical chemistry Impact factor: 3.034, year: 2016

  1. 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...

  2. Gene evolutionary trajectories and GC patterns driven by recombination in Zea mays

    Science.gov (United States)

    Recombination occurring during meiosis is critical for creating genetic variation and plays an essential role in plant evolution. In addition to creating novel gene combinations, recombination can affect genome structure through altering GC patterns. In maize (Zea mays) and other grasses, another in...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2005-03-01

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

  4. High-throughput investigation of polymerization kinetics by online monitoring of GPC and GC

    NARCIS (Netherlands)

    Hoogenboom, R.; Fijten, M.W.M.; Abeln, C.H.; Schubert, U.S.

    2004-01-01

    Gel permeation chromatography (GPC) and gas chromatography (GC) were successfully introduced into a high-throughput workflow. The feasibility and limitations of online GPC with a high-speed column was evaluated by measuring polystyrene standards and comparison of the results with regular offline GPC

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

    African Journals Online (AJOL)

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

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

    Directory of Open Access Journals (Sweden)

    Yong-Gang Xia

    2018-05-01

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

  7. GC/MS for profiling volatile constituents of red wine and their changes during radiation processing

    International Nuclear Information System (INIS)

    Gupta, Sumit; Variyar, Prasad S.; Sharma, Arun

    2013-01-01

    The aim of present study was therefore to investigate the effect of radiation processing of grape berries on the quality of Shiraz wines. In order to obtain this objective, wines prepared from control and irradiated grapes were analyzed for total antioxidant potential, total phenolic contents and aroma analysis by HS-SPME and GC/MS

  8. GC-MS Analysis of Insecticidal Essential Oil of Aerial Parts of ...

    African Journals Online (AJOL)

    Methods: Steam distillation of the aerial parts of P. scandens was carried out using Clavenger apparatus in order to obtain the volatile oils. Gas chromatography/mass spectrometric (GC/MS) analyses (HP-5MS column) of the essential oil were performed and its composition determined. Insecticidal activity of the essential oil ...

  9. Using Py-GC/MS to fingerprint additives associated with paper mill effluent toxicity episodes

    CSIR Research Space (South Africa)

    Sithole, Bruce

    2012-10-01

    Full Text Available techniques applicable to mill effluents such as gas chromatography. Py-GC/MS is a powerful analytical technique that can be used to fingerprint these additives. The presence of the additives is confirmed by fingerprint pyrograms of the additives (or...

  10. 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...

  11. 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…

  12. 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.

    H and temperature (air and water). Moreover, GC-MS analysis of methanolic extract of E. bangtawaensis showed major constituents of fatty acids such as myristic acid, oleic acid, stearic acid, arachidic acid, etc. The presence of such bioactive compounds (identified...

  13. Field Portable GC-MS Unit for Semi-Volatile Compound Analysis in Groundwater

    Science.gov (United States)

    2011-06-01

    the size and power consumption compared to standard GC systems. These modifications to the instrument design all serve to decrease the size and...Environment Mass Spectrometry (HEMS) Conference, September 2007, Cocoa Beach, FL. USEPA. 1998. USEPA Superfund Record of Decision, Milan Army

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

    International Nuclear Information System (INIS)

    Guidotti, M.; Ravaioli, G.

    1999-01-01

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

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

    Science.gov (United States)

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

    2010-06-01

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

  16. Development of an interface for directly coupled solid-phase extraction and GC-MS analysis

    NARCIS (Netherlands)

    Öllers, M.J.H.; van Lieshout, H.P.M.; Janssen, J.G.M.; Cramers, C.A.M.G.

    Solid-phase extraction (SPE) is widely used as a sample preparation technique in numerous application areas of chromatography. Large-volume injection is an attractive technique for coupling SPE to gas chromatography (GC) because it provides improved detection limits and circumvents the need for

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

    Science.gov (United States)

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

    2015-01-01

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

  18. Improvenments in environmental trace analysis by GC-IR and LC-IR.

    NARCIS (Netherlands)

    Visser, T.; Vredenbregt, M.J.; Jong, A.P.J.M.; Somsen, G.W.; Hankemeier, T.; Velthorst, N.H.; Gooijer, C.; Brinkman, U.A.T.

    1997-01-01

    Research has been carried out to enlarge the potential of infrared (IR) spectrometry as a detector in gas and liquid chromatography (GC and LC). The study has been directed to applications in environmental analysis. Examples of recently obtained results are presented. The analyte detectability of

  19. 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...

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

    African Journals Online (AJOL)

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

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

    International Nuclear Information System (INIS)

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

    2017-01-01

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

  2. 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.

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

  4. 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.

  5. 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.

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

    Science.gov (United States)

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

    2018-03-01

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

  7. 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.

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

    International Nuclear Information System (INIS)

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

    2002-01-01

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

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

  10. Inhibition of the Hantavirus Fusion Process by Predicted Domain III and Stem Peptides from Glycoprotein Gc.

    Science.gov (United States)

    Barriga, Gonzalo P; Villalón-Letelier, Fernando; Márquez, Chantal L; Bignon, Eduardo A; Acuña, Rodrigo; Ross, Breyan H; Monasterio, Octavio; Mardones, Gonzalo A; Vidal, Simon E; Tischler, Nicole D

    2016-07-01

    Hantaviruses can cause hantavirus pulmonary syndrome or hemorrhagic fever with renal syndrome in humans. To enter cells, hantaviruses fuse their envelope membrane with host cell membranes. Previously, we have shown that the Gc envelope glycoprotein is the viral fusion protein sharing characteristics with class II fusion proteins. The ectodomain of class II fusion proteins is composed of three domains connected by a stem region to a transmembrane anchor in the viral envelope. These fusion proteins can be inhibited through exogenous fusion protein fragments spanning domain III (DIII) and the stem region. Such fragments are thought to interact with the core of the fusion protein trimer during the transition from its pre-fusion to its post-fusion conformation. Based on our previous homology model structure for Gc from Andes hantavirus (ANDV), here we predicted and generated recombinant DIII and stem peptides to test whether these fragments inhibit hantavirus membrane fusion and cell entry. Recombinant ANDV DIII was soluble, presented disulfide bridges and beta-sheet secondary structure, supporting the in silico model. Using DIII and the C-terminal part of the stem region, the infection of cells by ANDV was blocked up to 60% when fusion of ANDV occurred within the endosomal route, and up to 95% when fusion occurred with the plasma membrane. Furthermore, the fragments impaired ANDV glycoprotein-mediated cell-cell fusion, and cross-inhibited the fusion mediated by the glycoproteins from Puumala virus (PUUV). The Gc fragments interfered in ANDV cell entry by preventing membrane hemifusion and pore formation, retaining Gc in a non-resistant homotrimer stage, as described for DIII and stem peptide inhibitors of class II fusion proteins. Collectively, our results demonstrate that hantavirus Gc shares not only structural, but also mechanistic similarity with class II viral fusion proteins, and will hopefully help in developing novel therapeutic strategies against hantaviruses.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2004-01-01

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

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

    Science.gov (United States)

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

    2016-11-01

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

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

    Directory of Open Access Journals (Sweden)

    Rolf Jorde

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

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

    Science.gov (United States)

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

    2018-04-01

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

  15. A fast and simple GC MS method for lignan profiling in Anthriscus sylvestris and biosynthetically related plant species

    NARCIS (Netherlands)

    Koulman, A; Bos, R; Medarde, M; Pras, N; Quax, WJ

    2001-01-01

    A new GC-MS method for monitoring lignans was developed to study the variation in plants and elucidate the biosynthetic steps. A simple and fast extraction procedure for lyophilised plant material was developed, giving a lignan-rich extract. A GC-MS method was set up using an apolar WCOT fused

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

    Science.gov (United States)

    Khrustalev, Vladislav Victorovich

    2009-01-01

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

  17. 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...

  18. 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.

  19. 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.

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

    International Nuclear Information System (INIS)

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

    1996-01-01

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

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

    International Nuclear Information System (INIS)

    Shibata, Yasuyuki

    2003-01-01

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

  2. 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

  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

    Directory of Open Access Journals (Sweden)

    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. Determination of pesticides in fruits and vegetables using acetonitrile extraction and GC/MS technique

    International Nuclear Information System (INIS)

    Hussain, Z.

    2010-01-01

    A selection of oranges, guava and spinach were purchased from the local markets of Lahore, Pakistan. Extraction of the samples was carried out using an acetonitrile/toluene extraction procedure to determine the residual concentration of pesticides which may have been used during seasonal growth. Gas chromatography/mass spectrometry (GC/MS) was used for quantitative and confirmatory analysis of GC-amenable pesticides. The data obtained was compared with that of a referenced pesticide by matching molecular weight to a library of known pesticides. For comparison the same non-sprayed fruits/vegetable were extracted as a control reference. Factors studied were retention time, elution time, relative abundance and molecular weight. The results showed that low molecular weight pesticides were eluted before the high molecular weight pesticides. Pesticides identified included crotoxyphos, fenoxycarb and methoxyfenozide. (author)

  5. 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.

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

    Science.gov (United States)

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

    2017-08-01

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

  7. Postirradiation examination data report for gap conductance test series. Test GC 2-1

    International Nuclear Information System (INIS)

    Murdock, B.A.

    1978-02-01

    The results of the postirradiation examination of four boiling water reactor type, zircaloy-clad, UO 2 -fueled rods tested in the Power Burst Facility are discussed. These rods were employed in Gap Conductance Test GC 2-1 which was performed to obtain experimental data from which test fuel rod gap conductance values could be determined by both the steady state ∫kdT and the power oscillation methods. The postirradiation examination results provided in the document will aid in interpreting the experimental data obtained during Test GC 2-1 and in evaluating the effect of fuel behavior on the fuel rod thermal response and interpreted gap conductances. Fuel rod fill gas composition and pressure are discussed. Measurements of fuel pellet-cladding gap and fuel crack areas are presented. The fuel structure is analyzed. Test rod instrumentation and power profiles are examined to better evaluate the test conditions

  8. 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.

  9. Measurement of HDO Products Using GC-TCD: Towards Obtaining Reliable Analytical Data

    Directory of Open Access Journals (Sweden)

    Zuas Oman

    2018-03-01

    Full Text Available This paper reported the method development and validation of a gas chromatography with thermal conductivity detector (GC-TCD method for the measurement of the gaseous products of hydrodeoxygenation (HDO. The method validation parameters include selectivity, precision (repeatability and reproducibility, accuracy, linearity, limit of detection (LoD, limit of quantitation (LoQ, and robustness. The results showed that the developed method was able to separate the target components (H2, CO2, CH4 and CO from their mixtures without any special sample treatment. The validated method was selective, precise, accurate, and robust. Application of the developed and validated GC-TCD method to the measurement of by-product components of HDO of bio-oil revealed a good performance with relative standard deviation (RSD less than 1.0% for all target components, implying that the process of method development and validation provides a trustworthy way of obtaining reliable analytical data.

  10. 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.

  11. [GC-MS analysis of volatile constituents from five different kinds of Chinese eaglewood].

    Science.gov (United States)

    Mei, Wen-Li; Zeng, Yan-Bo; Liu, Jun; Dai, Hao-Fu

    2007-05-01

    Volatile oils of five different kinds of Chinese eaglewood were extracted with aether at room temperature. The chemical constituents and relative contents of the volatile oils were analysed by GC-MS. It showed that all the five volatile oils were mainly composed of sesquiterpenes, aromatic constituents and fatty acids. Several sesquiterpenes, such as hinesol, nootkatone, valerenic acid, velleral, guaiol, gamma-gurjunene, gamma-selinene, viridiflorol, isoaromadendrene epoxide, valencene, alpha-costol et. al., together with several aromatic constituents, 2,4-di-tert-butylphenol,4-methyl-2,6-di-tert-butylphenol, phenylpropionic acid, 1-(benzyloxy)-8-naphthol, anisylacetone, et. al. were found in the volatile oils of Chinese eaglewood for the first time. The samilarities and differences of the volatile oils from the five kinds of Chinese eaglewood were compared. It suggested that the quality of Chinese eaglewood could be evaluated by GC-MS analyse of the volatile oil.

  12. 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

  13. 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

  14. Determination of Sesquiterpenes in Wines by HS-SPME Coupled with GC-MS

    OpenAIRE

    Cincotta, Fabrizio; Verzera, Antonella; Tripodi, Gianluca; Condurso, Concetta

    2015-01-01

    The sesquiterpene compounds present in red wines were characterized and quantified by Headspace Solid-Phase Microextraction in combination with Gas Chromatography–Mass Spectrometry (HS-SPME-GC-MS). Sixteen sesquiterpenes were identified, mainly hydrocarbons but also derived oxygenated compounds. Sesquiterpenes were acyclic, monocyclic, byciclic and tryciclic. Sesquiterpenes were detected in SIM (selected ion monitoring) mode using their characteristics ions. All the sesquiterpenes were identi...

  15. GC-MS analysis of off-odor volatiles from irradiated pork

    International Nuclear Information System (INIS)

    Lin Ruotai; Geng Shengrong; Zhang Jinmu; Chen Yuxia; Liu Yangmin; Wang Liping; Wang Hong; Xu Ying; Yao Side

    2007-01-01

    The main compounds of off-odor volatiles from irradiated refrigerated vacuum-packaged pork were analyzed by gas chromatograph/mass spectrometer (GC-MS). The analytical results showed that the main compounds of off-odor volatiles were dimethyl disulfide, dimethyl sulfide, dimethyl trisulfide, S-methyl thioacetate, and methanethiol. It was proved that the off-odor volatile came from irradiated S-containing amino acid and thiamin. (authors)

  16. NO-sGC Pathway Modulates Ca2+ Release and Muscle Contraction in Zebrafish Skeletal Muscle.

    Science.gov (United States)

    Xiyuan, Zhou; Fink, Rainer H A; Mosqueira, Matias

    2017-01-01

    Vertebrate skeletal muscle contraction and relaxation is a complex process that depends on Ca 2+ ions to promote the interaction of actin and myosin. This process can be modulated by nitric oxide (NO), a gas molecule synthesized endogenously by (nitric oxide synthase) NOS isoforms. At nanomolar concentrations NO activates soluble guanylate cyclase (sGC), which in turn activates protein kinase G via conversion of GTP into cyclic GMP. Alternatively, NO post-translationally modifies proteins via S-nitrosylation of the thiol group of cysteine. However, the mechanisms of action of NO on Ca 2+ homeostasis during muscle contraction are not fully understood and we hypothesize that NO exerts its effects on Ca 2+ homeostasis in skeletal muscles mainly through negative modulation of Ca 2+ release and Ca 2+ uptake via the NO-sGC-PKG pathway. To address this, we used 5-7 days-post fecundation-larvae of zebrafish, a well-established animal model for physiological and pathophysiological muscle activity. We evaluated the response of muscle contraction and Ca 2+ transients in presence of SNAP, a NO-donor, or L-NAME, an unspecific NOS blocker in combination with specific blockers of key proteins of Ca 2+ homeostasis. We also evaluate the expression of NOS in combination with dihydropteridine receptor, ryanodine receptor and sarco/endoplasmic reticulum Ca 2+ ATPase. We concluded that endogenous NO reduced force production through negative modulation of Ca 2+ transients via the NO-sGC pathway. This effect could be reversed using an unspecific NOS blocker or sGC blocker.

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

    International Nuclear Information System (INIS)

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

    2017-01-01

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

  18. Laser assisted ratio analysis - An alternative to GC/IRMS for CO2

    International Nuclear Information System (INIS)

    Murnick, D.E.

    2001-01-01

    A new technique for laser based analysis of carbon isotope ratios, with the acronym LARA, based on large isotope shifts in molecular spectra, the use of fixed frequency isotopic lasers, and sensitive detection via the laser optogalvanic effect is reviewed and compared with GC/IRMS for carbon dioxide in specific applications. The possibility for development of new classes of isotope ratio measurement systems with LARA is explored. (author)

  19. 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.

  20. Fast Pyrolysis of Four Lignins from Different Isolation Processes Using Py-GC/MS

    OpenAIRE

    Lin, Xiaona; Sui, Shujuan; Tan, Shun; Pittman, Charles; Sun, Jianping; Zhang, Zhijun

    2015-01-01

    Pyrolysis is a promising approach that is being investigated to convert lignin into higher value products including biofuels and phenolic chemicals. In this study, fast pyrolysis of four types of lignin, including milled Amur linden wood lignin (MWL), enzymatic hydrolysis corn stover lignin (EHL), wheat straw alkali lignin (AL) and wheat straw sulfonate lignin (SL), were performed using pyrolysis gas-chromatography/mass spectrometry (Py-GC/MS). Thermogravimetric analysis (TGA) showed that the...

  1. Speciation of organotin compounds in environmental samples by GC-ICPMS

    International Nuclear Information System (INIS)

    Vahcic, M.; Milacic, R.; Scancar, J.

    2009-01-01

    Full text: Analytical procedure using 15 m GC column was applied for simultaneous speciation of OTCs in various environmental samples. Methyl-, butyl-, phenyl- and octyl- tin species were quantitatively determined. different extraction reagents and conditions were studied. OTCs species were derivatized by NaBEt 4 and extracted into isooctane or hexane. The applied analytical procedure considerably shortened analytical time and enabled simultaneous determination of 12 OTCs in environmental samples. (author)

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

    Directory of Open Access Journals (Sweden)

    Cedric R Uytingco

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

  3. Promising role for Gc-MAF in cancer immunotherapy: from bench to bedside

    OpenAIRE

    Saburi, Ehsan; Saburi, Amin; Ghanei, Mostafa

    2017-01-01

    Immunotherapy has been used for years in many types of cancer therapy. Recently, cancer immunotherapy has focused on mechanisms which can enhance the development of cell-mediated immunity. Anticancer medications are administered to inhibit immunosuppressive factors such as nagalase enzyme, which is produced by neoplastic cells and destroys macrophage activating factor (Gc-MAF). Anti-neoplastics medications can also enhance immune-cell activity against tumors. Such medications show great poten...

  4. 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.

  5. Miniature GC-Minicell Ion Mobility Spectrometer (IMS) for In Situ Measurements in Astrobiology Planetary Missions

    Science.gov (United States)

    Kojiro, Daniel R.; Stimac, Robert M.; Kaye, William J.; Holland, Paul M.; Takeuchi, Norishige

    2006-01-01

    Astrobiology flight experiments require highly sensitive instrumentation for in situ analysis of volatile chemical species and minerals present in the atmospheres and surfaces of planets, moons, and asteroids. The complex mixtures encountered place a heavy burden on the analytical instrumentation to detect and identify all species present. The use of land rovers and balloon aero-rovers place additional emphasis on miniaturization of the analytical instrumentation. In addition, smaller instruments, using tiny amounts of consumables, allow the use of more instrumentation and/or ionger mission life for stationary landers/laboratories. The miniCometary Ice and Dust Experiment (miniCIDEX), which combined Gas Chromatography (GC) with helium Ion Mobility Spectrometry (IMS), was capable of providing the wide range of analytical information required for Astrobiology missions. The IMS used here was based on the PCP model 111 IMS. A similar system, the Titan Ice and Dust Experiment (TIDE), was proposed as part of the Titan Orbiter Aerorover Mission (TOAM). Newer GC systems employing Micro Electro- Mechanical System (MEMS) based technology have greatly reduced both the size and resource requirements for space GCs. These smaller GCs, as well as the continuing miniaturization of Astrobiology analytical instruments in general, has highlighted the need for smaller, dry helium IMS systems. We describe here the development of a miniature, MEMS GC-IMS system (MEMS GC developed by Thorleaf Research Inc.), employing the MiniCell Ion Mobility Spectrometer (IMS), from Ion Applications Inc., developed through NASA's Astrobiology Science and Technology Instrument Development (ASTID) Program and NASA s Small Business Innovative Research (SBIR) Program.

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

    International Nuclear Information System (INIS)

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

    1990-01-01

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

  7. 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.

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

    Science.gov (United States)

    Reifenberger, Jeffrey; Dorfman, Kevin; Cao, Han

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

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

    International Nuclear Information System (INIS)

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

    1999-01-01

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

  10. A novel assay of DGAT activity based on high temperature GC/MS of triacylglycerol.

    Science.gov (United States)

    Greer, Michael S; Zhou, Ting; Weselake, Randall J

    2014-08-01

    Diacylglycerol acyltransferase (DGAT) catalyzes the final step in the acyl-CoA-dependent biosynthesis of triacylglycerol (TAG), a high-energy compound composed of three fatty acids esterified to a glycerol backbone. In vitro DGAT assays, which are usually conducted with radiolabeled substrate using microsomal fractions, have been useful in identifying compounds and genetic modifications that affect DGAT activity. Here, we describe a high-temperature gas chromatography (GC)/mass spectrometry (MS)-based method for monitoring molecular species of TAG produced by the catalytic action of microsomal DGAT. This method circumvents the need for radiolabeled or modified substrates, and only requires a simple lipid extraction prior to GC. The utility of the method is demonstrated using a recombinant type-1 Brassica napus DGAT produced in a strain of Saccharomyces cerevisae that is deficient in TAG synthesis. The GC/MS-based assay of DGAT activity was strongly correlated with the typical in vitro assay of the enzyme using [1-(14)C] acyl-CoA as an acyl donor. In addition to determining DGAT activity, the method is also useful for determining substrate specificity and selectivity properties of the enzyme.

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

    Science.gov (United States)

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

    2007-07-01

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

  12. 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.

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

    Science.gov (United States)

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

    2018-02-05

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

  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. GC determination of N-nitrosamines by supersonic molecular beam MS equipped with triple quadrupole analyzer, GC/SMB/QQQ/MS

    International Nuclear Information System (INIS)

    Anna, Voloshenko; Rimma, Shelkov; Lev, Ovadia; Jenny, Gun

    2011-01-01

    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.

  16. 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

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

    Science.gov (United States)

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

    2017-03-01

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

  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. 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

    Directory of Open Access Journals (Sweden)

    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.

  20. Improving Student Understanding of Qualitative and Quantitative Analysis via GC/MS Using a Rapid SPME-Based Method for Determination of Trihalomethanes in Drinking Water

    Science.gov (United States)

    Huang, Shu Rong; Palmer, Peter T.

    2017-01-01

    This paper describes a method for determination of trihalomethanes (THMs) in drinking water via solid-phase microextraction (SPME) GC/MS as a means to develop and improve student understanding of the use of GC/MS for qualitative and quantitative analysis. In the classroom, students are introduced to SPME, GC/MS instrumentation, and the use of MS…

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

    Directory of Open Access Journals (Sweden)

    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.

  2. 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

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

    KAUST Repository

    Li, Shu-Long

    2017-10-27

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

  4. Using GC-combustion isotope ratio mass spectrometry for confirming steroid administration from urinary metabolites in humans and animals

    International Nuclear Information System (INIS)

    Phillips, A.; Churchman, D.; Davis, S.

    2000-01-01

    Gas chromatography-combustion-isotope ratio mass spectrometry (GC-C-IRMS) was used to study the incorporation of exogenous testosterone enanthate into excreted urinary 5α- and 5β-androstane-3α, 17β-diols

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

    KAUST Repository

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

    2017-01-01

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

  6. Educational Program Improvement in Chemistry Through the Acquisition of GC/MS And FT-NMR Instruments

    National Research Council Canada - National Science Library

    Anderson, Gloria

    1997-01-01

    ...), Department of Defense. The purpose of this grant was to enable the department to acquire instrumentation necessary for incorporating the theory and practice of Gas Chromatography/Mass Spectrometry (GC/MS...

  7. Comparison of LC-ESI-MS and GC-MS for the Analysis of a Synthetic Tabun Sample

    National Research Council Canada - National Science Library

    D'Agostino, Paul

    2003-01-01

    Packed capillary LC-ESI-MS and capillary column GC-MS were compared for the analysis of a synthetic tabun sample as each method has advantages for the analysis of samples containing chemical warfare...

  8. Field-portable Gas Chromatograph Mass Spectrometer (GC-MS) Unit for Semi-volatile Compound Analysis in Groundwater

    Science.gov (United States)

    2011-09-01

    the need for a convective oven, greatly reducing the size and power consumption compared to standard GC systems. These modifications to the...spectrometer. In Harsh Environment Mass Spectrometry (HEMS) Conference; September 2007; Cocoa Beach, FL. Science Applications International Corporation

  9. 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.

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

    Science.gov (United States)

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

    2014-01-01

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

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

    Science.gov (United States)

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

    2014-01-01

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

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

    Science.gov (United States)

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

    1997-01-01

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

  13. Detection Characteristics of Gamma-Irradiated Seeds by using PSL, TL, ESR and GC/MS

    International Nuclear Information System (INIS)

    Kim, K.H.; Shon, J.H.; Kang, Y.J.; Jo, T.Y.; Park, H.Y.; Kwak, J.Y.; Lee, J.H.; Park, Y.C.; Kim, J.I.; Lee, H.J.; Lee, S.J.; Han, S.B.

    2013-01-01

    In this study, we investigated the applicability of the photostimulated luminescence (PSL), thermoluminescence (TL), electron spin resonance (ESR) and gas chromatography/mass spectrometry (GC/MS) methods for 5 seeds which are not allowed to be irradiated in Korea. All 5 seeds including evening primrose seed, safflower seed, rape seed, sunflower seed and flax seed were analyzed. Samples were irradiated at 1~10 kGy using a 60 Co gamma-ray irradiator. In PSL study, the photon counts of all the unirradiated samples showed negative (lower than 700). The photon counts of irradiated (1, 5, 10 kGy) samples showed positive (higher than 5,000). In TL analysis, results showed that it is possible to apply TL method to all foods containing minerals. In ESR measurements, the ESR signal (single-line) intensity of irradiated foods was higher than non-irradiated foods. The hydrocarbons 1,7-hexadecadiene (C 16:2 ) and 8-heptadecene (C 17:1 ) from oleic acid were detected only in the irradiated samples before and after the treatment at doses ≥ 1 kGy, but they were not detected in non-irradiated samples before and after treatment. These two hydrocarbons could be used as markers to identify irradiated safflower seed, rape seed, Sunflower seed and flax seed. And then, the hydrocarbons 1,7,10-hexadecatriene (C 16:3 ) and 6,9-heptadecadiene (C 17:2 ) from linoleic acid were detected in the evening primrose seed, safflower seed and sunflower seed. According to the results, PSL, TL and GC/ MS methods were successfully applied to detect the irradiated foods. It is concluded that PSL, TL and GC/MS methods are suitable for detection of irradiated samples and a combined method is recommendable for enhancing the reliability of detection results. (author)

  14. Switches in Genomic GC Content Drive Shifts of Optimal Codons under Sustained Selection on Synonymous Sites

    Science.gov (United States)

    Sun, Yu; Tamarit, Daniel

    2017-01-01

    Abstract The major codon preference model suggests that codons read by tRNAs in high concentrations are preferentially utilized in highly expressed genes. However, the identity of the optimal codons differs between species although the forces driving such changes are poorly understood. We suggest that these questions can be tackled by placing codon usage studies in a phylogenetic framework and that bacterial genomes with extreme nucleotide composition biases provide informative model systems. Switches in the background substitution biases from GC to AT have occurred in Gardnerella vaginalis (GC = 32%), and from AT to GC in Lactobacillus delbrueckii (GC = 62%) and Lactobacillus fermentum (GC = 63%). We show that despite the large effects on codon usage patterns by these switches, all three species evolve under selection on synonymous sites. In G. vaginalis, the dramatic codon frequency changes coincide with shifts of optimal codons. In contrast, the optimal codons have not shifted in the two Lactobacillus genomes despite an increased fraction of GC-ending codons. We suggest that all three species are in different phases of an on-going shift of optimal codons, and attribute the difference to a stronger background substitution bias and/or longer time since the switch in G. vaginalis. We show that comparative and correlative methods for optimal codon identification yield conflicting results for genomes in flux and discuss possible reasons for the mispredictions. We conclude that switches in the direction of the background substitution biases can drive major shifts in codon preference patterns even under sustained selection on synonymous codon sites. PMID:27540085

  15. Cell Monitoring and Manipulation Systems (CMMSs based on Glass Cell-Culture Chips (GC3s

    Directory of Open Access Journals (Sweden)

    Sebastian M. Buehler

    2016-06-01

    Full Text Available We developed different types of glass cell-culture chips (GC3s for culturing cells for microscopic observation in open media-containing troughs or in microfluidic structures. Platinum sensor and manipulation structures were used to monitor physiological parameters and to allocate and permeabilize cells. Electro-thermal micro pumps distributed chemical compounds in the microfluidic systems. The integrated temperature sensors showed a linear, Pt1000-like behavior. Cell adhesion and proliferation were monitored using interdigitated electrode structures (IDESs. The cell-doubling times of primary murine embryonic neuronal cells (PNCs were determined based on the IDES capacitance-peak shifts. The electrical activity of PNC networks was detected using multi-electrode arrays (MEAs. During seeding, the cells were dielectrophoretically allocated to individual MEAs to improve network structures. MEA pads with diameters of 15, 20, 25, and 35 µm were tested. After 3 weeks, the magnitudes of the determined action potentials were highest for pads of 25 µm in diameter and did not differ when the inter-pad distances were 100 or 170 µm. Using 25-µm diameter circular oxygen electrodes, the signal currents in the cell-culture media were found to range from approximately −0.08 nA (0% O2 to −2.35 nA (21% O2. It was observed that 60-nm thick silicon nitride-sensor layers were stable potentiometric pH sensors under cell-culture conditions for periods of days. Their sensitivity between pH 5 and 9 was as high as 45 mV per pH step. We concluded that sensorized GC3s are potential animal replacement systems for purposes such as toxicity pre-screening. For example, the effect of mefloquine, a medication used to treat malaria, on the electrical activity of neuronal cells was determined in this study using a GC3 system.

  16. Identification of natural indigo in historical textiles by GC-MS.

    Science.gov (United States)

    Degani, Laura; Riedo, Chiara; Chiantore, Oscar

    2015-02-01

    The possibility of successfully applying a common GC-MS procedure for identification in one step of all types of dyes from plants of unknown origin and from historical objects is particularly attractive due to the high separation efficiency of the capillary columns, the MS detection sensitivity and the reproducibility of results. In this work, GC-MS analysis, previously and successfully used for the characterization of anthraquinones, flavonoids and tannins from plant extracts and historical samples, has been tested on indigoid dyestuffs. An analytical procedure based on the silylating agent N,O-bis-(trimethylsilyl)trifluoroacetamide (BSTFA) with 1% trimethylchlorosilane (TMCS) was applied to pure molecules of indigotin and indirubin and to plant extracts of Indigofera tinctoria L. and Isatis tinctoria L. Preliminary tests have been done to establish the chromatographic conditions and the derivatization amounts most suitable for the simultaneous detection of indigoid molecules and of the other natural compounds, such as fatty acids, carboxylic acids and sugars, contained within the plant extracts. In order to assess the capacity and the sensitivity of the analytical procedure in typical archaeometric applications, wool samples dyed in the laboratory with indigo were analysed by mimicking the sample amounts typically available with historical objects. The electron ionization (EI) spectra of the main silylated derivatives of indigoid molecules obtained in this way constitute the necessary data set for the characterization of natural extracts and historical works of art. Subsequently, the procedure has been applied to historical samples for the detection of indigo and of other dyestuffs eventually contained in samples. Additional information, useful for restoration and preservation of works of art, could be also obtained on the nature of stains and smudges present on the sampled textile material. The GC-MS method turns out to be an efficient and fast analytical tool

  17. Implementation of AICAR analysis by GC-C-IRMS for anti-doping purposes.

    Science.gov (United States)

    Buisson, C; Frelat, C; Mongongu, C; Martinat, N; Audran, M

    2017-11-01

    AICAR (5-aminoimidazole-4-carboxamide-1-β-D-ribofuranoside), is a naturally occurring substance which is part to the World Anti-Doping Agency (WADA) Prohibited List. It is claimed to improve physical performance when administered as a supplement. As for other endogenous compounds such as steroids, the gas chromatography-combustion-isotope ratio mass spectrometry (GC-C-IRMS) analysis remains an efficient tool to differentiate endogenous substances from exogenous ones. A protocol was described in the literature for the analysis of AICAR by GC-C-IRMS. The aim of the present study was to implement this protocol in our laboratory and to propose solutions to avoid the difficulties encountered. The first point discussed in this study is the derivatization step. Due to the structure of the AICAR molecule, conventional derivatization for GC-C-IRMS such as acetylation could not be applied and silylation was preferred. The improvement of the derivatives stability was achieved thanks to several derivatization conditions tested. This adjustment led to a reproducible derivatization pattern with the 3-TMS form as major derivative product. The second point discussed in this study is the diminution of extracts' background noise. Indeed, the implementation of the published protocol was not easy due to high performance liquid chromatography (HPLC) problems encountered when concentrated urine was injected into our system. Also, too many interferences in the endogenous reference compound fractions were observed. The addition of both a wash step before the HPLC purification and a HPLC purification step for the endogenous reference compound (ERC) fraction allowed us to increase the robustness of the method. This study presents the modified protocol compared to the original protocol as well as the evaluation of the whole method performances. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

  18. Determination of patulin in fruit juices using HPLC-DAD and GC-MSD techniques.

    Science.gov (United States)

    Moukas, Athanasios; Panagiotopoulou, Vasiliki; Markaki, Panagiota

    2008-08-15

    A high performance liquid chromatography with a diode-array detector (HPLC-DAD) and a gas chromatography with a mass spectrometer (GC-MSD) are described for the determination of patulin (PAT) in apple juice. The limits of detection (DL) and quantification (QL) for the HPLC-DAD and GC-MSD method were found to be (DL=0.23μgkg(-1) QL=1.2μgkg(-1)) and (DL=5.8μgkg(-1) and QL=13.8μgkg(-1)), respectively. The recovery factors for HPLC-DAD and GC-MSD were found to be 99.5% (RSD%=0.73) and 41% (RSD%=10.03), respectively. The HPLC-DAD method was used to determine the occurrence of PAT in 90 samples of fruit juices. Results revealed the presence of PAT in 100% of the samples examined. The mean values of PAT in concentrated fruit juices and in the commercial fruit juices collected from the Greek market were found to be 10.54μg PAT kg(-1) and 5.57μg PAT kg(-1) juice, respectively. The most contaminated samples were four concentrated juices ranging from 18.10μg PAT kg(-1) to 36.8μg PAT kg(-1) juice. The daily exposure to patulin for the consumers of all ages in Greece, is ranging from 0.008μg PAT kg(-1) bw to 0.1μg PAT kg(-1) bw if the daily intake of fruit juices is from 0.1 to 0.5kg. With the exception to the most contaminated sample, the daily exposure due to the samples examined, is below the provisional maximum tolerable daily intake for PAT (0.4μg PAT kg(-1) bw). Copyright © 2008 Elsevier Ltd. All rights reserved.

  19. Dereplication of pentacyclic triterpenoids in plants by GC-EI/MS.

    Science.gov (United States)

    Gu, Jian-Qiao; Wang, Yuehong; Franzblau, Scott G; Montenegro, Gloria; Timmermann, Barbara N

    2006-01-01

    Three common plant-derived pentacyclic triterpenoids, oleanolic acid (1), betulinic acid (2) and ursolic acid (3), have been found to exhibit moderate anti-tubercular activity in a microplate alamar blue assay. In order to facilitate the discovery of novel anti-tubercular leads with diverse chemical structures, a new and rapid GC-EI/MS method was developed simultaneously and unambiguously to dereplicate 1-3 as their methyl esters with limits of detection of 25.6, 26.9 and 26.8 ng, respectively.

  20. Nearest neighbor affects G:C to A:T transitions induced by alkylating agents.

    OpenAIRE

    Glickman, B W; Horsfall, M J; Gordon, A J; Burns, P A

    1987-01-01

    The influence of local DNA sequence on the distribution of G:C to A:T transitions induced in the lacI gene of E. coli by a series of alkylating agents has been analyzed. In the case of nitrosoguanidine, two nitrosoureas and a nitrosamine, a strong preference for mutation at sites proceeded 5' by a purine base was noted. This preference was observed with both methyl and ethyl donors where the predicted common ultimate alkylating species is the alkyl diazonium ion. In contrast, this preference ...

  1. Study of organohalogen contaminants in yogurt by NAA and GC-ECD

    International Nuclear Information System (INIS)

    Zhang, H.; Chai, Z.F.; Shenzen Univ.; Sun, H.B.; Zhang, J.L.; Ouyang, H.; Xin, L.; Chuai, Y.D.

    2007-01-01

    The concentrations and distributions of total halogen (TX), extractable organohalogen (EOX) and extractable persistent organohalogen (EPOX) were determined in 20 kinds of yogurt specimens collected from Chinese supermarkets using neutron activation analysis (NAA) and gas chromatography equipped with a 63 Ni electron capture detector (GC-ECD). The results indicated that the halogens in yogurt mainly existed as non-extractable organohalogen compounds. About 25-30% of EOX was EPOX. EOCl and EPOCl were the main organohalogen species in yogurt. The average concentration of the identified organochlorine, such as organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs), was below 4% of EPOCl. (author)

  2. Preliminary study of urine metabolism in type two diabetic patients based on GC-MS

    OpenAIRE

    Zhang, Ning; Geng, Fang; Hu, Zhong-Hua; Liu, Bin; Wang, Ye-Qiu; Liu, Jun-Cen; Qi, Yong-Hua; Li, Li-Jing

    2016-01-01

    Objective: Comparative study of type 2 diabetes and healthy controls by metabolomics methods to explore the pathogenesis of Type II diabetes. Methods: Gas chromatography - mass spectrometry (GC-MS) with a variety of multivariate statistical analysis methods to the healthy control group 58 cases, 68 cases of Type II diabetes group were analyzed. Chromatographic conditions: DB-5MS column; the carrier gas He; flow rate of 1 mL·min-1, the injection volume 1 uL; split ratio is 100: 1. MS condition...

  3. On-line coupled LC-LC-GC for irradiation detection in complex lipid matrices

    International Nuclear Information System (INIS)

    Schulzki, G.; Spiegelberg, A.; Helle, N.; Boegl, K.W.; Schreiber, G.A.

    1993-01-01

    Since sample preparation with HPLC coupled on-line to the GC has been performed for only a few weeks in our laboratory, the results presented give a first look at what can be done by means of this technique. Even difficult samples as the described fish species, where an unequivocal identification regarding an irradiation treatment seemed to become a hopeless enterprise, could be managed. Because of the greater variety of fatty acids in fish ''new'' radiation-induced hydrocarbons were available. According to the theory of Nawar in addition to 16:2 and 17:2 hydrocarbons we have looked for in irradiated meat, further alkadienes appeared in irradiated fish, which were 14:2, 18:2 and 20:2. Analysis of the alkadiene-fraction, transferred to the GC after a two step LC clean up, resulted in an unequivocal identification of all fish samples as well as the fruits and sponge cake. For fruits and sponge cake the detection limit seems to be clearly below 0.5 kGy. It can further be lowered by increasing the amount of lipid whereas the upper limit for a certain LC column has to be determined. In contrast to these samples only qualitative results were obtained for fish. In the case of sponge cake for the first time irradiation of a component of a heat treated food was detected. Further investigations regarding reproducibility, dose dependence and detection limit have to be done. On-line coupled (LC-)LC-GC was proved to be a highly efficient method for analysis of complex samples. In contrast to off-line Florisil column chromatography only a small part of the initial lipid material is needed because the complete hydrocarbon fraction is transferred on-line to the GC. This offers the possibility to analyze even foods with a low fat content like various seafoods. Classification of the hydrocarbon fraction by a two step LC may facilitate the identification of the radiolytic products also if no mass spectrometric detection system is available. (orig./vhe)

  4. Amino Acid Usage Is Asymmetrically Biased in AT- and GC-Rich Microbial Genomes

    DEFF Research Database (Denmark)

    Bohlin, Jon; Brynildsrud, Ola Brønstad; Vesth, Tammi Camilla

    2013-01-01

    frequencies were distributed in over 2000 microbial genomes and how these distributions were affected by base compositional changes. In addition, we wanted to know how genome-wide amino acid usage was biased in the different genomes and how changes to base composition and mutations affected this bias...... purifying selection than genomes with higher AAUB. Conclusion: Genomic base composition has a substantial effect on both amino acid- and codon frequencies in bacterial genomes. While phylogeny influenced amino acid usage more in GC-rich genomes, AT-content was driving amino acid usage in AT-rich genomes. We...

  5. [Analysis of essential oil extracted from Lactuca sativa seeds growing in Xinjiang by GC-MS].

    Science.gov (United States)

    Xu, Fang; Wang, Qiang; Haji, Akber Aisa

    2011-12-01

    To analyze the components of essential oil from Lactuca sativa seeds growing in Xinjiang. The components of essential oil from Lactuca sativa seeds were analyzed by gas chromatography-mass spectrometry (GC-MS). 62 components were identified from 71 separated peaks,amounting to total mass fraction 95.07%. The dominant compounds were n-Hexanol (36.31%), n-Hexanal (13.71%), trans-2-Octen-l-ol (8.09%) and 2-n-Pentylfuran (4.41%). The research provides a theoretical basis for the exploitation and use of Lactuca sativa seeds resource.

  6. Analysis of flavor-related compounds from tabacco using SPME-GC-MS

    Energy Technology Data Exchange (ETDEWEB)

    Park, G.B.; Lee, S.G. [Korea Research Institute of Chemical Technology, Taejeon (Korea)

    2001-04-01

    The flavor-related compounds contained in tobacco were analyzed by selected ion monitoring (SIM) method using headspace SPME gas chromatography-mass spectrometry (GC-MS). Flavor-related compounds were estragole, pulegone, trans-anethole, safrole, piperonal, eugenol, methyleugenol, coumarin, trans-isoeugenol, trans-methyleugenol and myristicin More than one of the flavor-related compounds were detected in the range of 0.001-1.3 {mu}g/g from all brands of tobacco studied. The recovery was ranged from 89.1 to 102.9% and relative standard deviation was ranged from 2.6 to 25.2%. (author). 19 refs., 4 tabs., 2 figs.

  7. Chemical characterization of neonicotinoids in surface waters by high performance liquid chromatography with Tandem Mass Spectrometry (HPLC MS/MS); Caracterização química dos neonicotinóides em águas superficiais via cromatografia liquída de alta eficiência acoplada a Espectrometria de Massas em Tandem (HPLC-MS/MS)

    Energy Technology Data Exchange (ETDEWEB)

    Amaral, Priscila Oliveira

    2017-07-01

    The present study aimed to develop a method for the determination and validation of a method for the identification and quantification of Neonicotinoids in surface waters collected in the Bauru region, in the state of São Paulo. The analytical techniques studied for the development of this method were the high performance liquid chromatography with tandem mass spectrometry (HPLC - MS / MS), gas chromatography with mass spectrometry (GC / MS) and gas chromatography with electron capture detector (GC / ECD). The class of pesticides Neonicotinoids was chosen for this work because it is related to a sudden disappearance of bees in colonies around the world. This phenomenon is known as Colony Collapse Disorder (CCD) and it is characterized by a rapid loss in the population of adult bees. The Neonicotinoids used in this study were the compounds Clothianidin, Imidacloprid and Thiamethoxam which were banned in their use as pesticides in Europe by Implementing Regulation No. 540/2011. The samples were concentrated using solid phase extraction (SPE) and liquid liquid extraction (LLE) techniques and injected into HPLC-MS / MS, GC / MS and GC / ECD. The GC / ECD and GC / MS techniques were not satisfactory for determination in the water matrix because the detection limit (10 mg L{sup -1}) is above the maximum allowed by the US Environmental Protection Agency (0.6 μg L{sup -1}). The HPLC - MS / MS technique using the multiple reaction monitoring (MRM) proved to be adequate for this study because it obtained quantification limits between 5.89 and 8.06 μg L{sup -1} and a linearity between 0.9963 and 0.9999 for the three compounds. (author)

  8. Analysis of acrylamide by LC-MS/MS and GC-MS in processed Japanese foods.

    Science.gov (United States)

    Ono, H; Chuda, Y; Ohnishi-Kameyama, M; Yada, H; Ishizaka, M; Kobayashi, H; Yoshida, M

    2003-03-01

    Acrylamide concentrations in processed foods (63 samples covering 31 product types) from Japan were analysed by LC-MS/MS and GC-MS methods. The limit of detection and limit of quantification of acrylamide were 0.2 ng x ml(-1) (6 fmol) and 0.8 ng x ml(-1) (22 fmol), respectively, by LC-MS/MS, and those of 2,3-dibromopropionamide derived from acrylamide were 12 ng x ml(-1) (52 fmol) and 40 ng x ml(-1) (170 fmol), respectively, by GC-MS. Repeatability given as RSD was 1000 microg x kg(-1). The concentrations in non-whole potato-based snacks, rice crackers processed by grilling or frying, and candied sweet potatoes were lower compared with those in the potato crisps and the whole potato-based fried snacks. One of the whole potato-based fried snacks, however, showed low acrylamide concentration (instant precooked noodles and won-tons were <100 microg x kg(-1) with only one exception. Roasted barley grains for 'Mugi-cha' tea contained 200-600 microg x kg(-1) acrylamide.

  9. Detection of irradiated mushrooms by GC/MS analysis of lipid-derived hydrocarbons

    International Nuclear Information System (INIS)

    Delincee, H.; Koller, W.D.

    1993-01-01

    A number of methods has been developed for the detection of irradiated foods in recent years, and in the case of mushrooms several methods have been proposed, of which the thermoluminescence (TL) measurements seem to be the most valuable. However, in several cases mineral contamination of fresh mushrooms is so extremely low that not enough minerals can be isolated for TL analysis. In that case an alternative method is needed to detect the radiation treatment of mushrooms. Several methods including TTC (2,3,5-triphenyl-tetrazolium-chloride) staining, kinetin treatment, dropping out of spores and mirco-gel electrophoresis of spores, were tested, but the most promising method was the GC/MS analysis of radiation-induced lipid-derived hydrocarbons in spite of the low fat content - around 0.2-0.3% - of mushrooms. Successful results were achieved by GC/MS analysis of the radiolytic hydrocarbons. Although mushrooms have a low fat content, by extracting a large quantity, in this case 500 g of mushrooms, about 1.2-1.5 g of fat could be obtained. The main fatty acids of mushroom fat and some of their expected cleavage products on irradiation - the c n-1 hydrocarbon which has one C atom less than the parent fatty acid and the C n-2:1 hydrocarbon, which has two C atoms less and an additional double bond in position 1 - are given. (orig./Vhe)

  10. Surface modification of GC and HOPG with diazonium, amine, azide, and olefin derivatives.

    Science.gov (United States)

    Tanaka, Mutsuo; Sawaguchi, Takahiro; Sato, Yukari; Yoshioka, Kyoko; Niwa, Osamu

    2011-01-04

    Surface modification of glassy carbon (GC) and highly oriented pyrolytic graphite (HOPG) was carried out with diazonium, amine, azide, and olefin derivatives bearing ferrocene as an electroactive moiety. Features of the modified surfaces were evaluated by surface concentrations of immobilized molecule, blocking effect of the modified surface against redox reaction, and surface observation using cyclic voltammetry and electrochemical scanning tunneling microscope (EC-STM). The measurement of surface concentrations of immobilized molecule revealed the following three aspects: (i) Diazonium and olefin derivatives could modify substrates with the dense-monolayer concentration. (ii) The surface concentration of immobilized amine derivative did not reach to the dense-monolayer concentration reflecting their low reactivity. (iii) The surface modification with the dense-monolayer concentration was also possible with azide derivative, but the modified surface contained some oligomers produced by the photoreaction of azides. Besides, the blocking effect against redox reaction was observed for GC modified with diazonium derivative and for HOPG modified with diazonium and azide derivatives, suggesting fabrication of a densely modified surface. Finally, the surface observation for HOPG modified with diazonium derivative by EC-STM showed a typical monolayer structure, in which the ferrocene moieties were packed densely at random. On the basis of those results, it was demonstrated that surface modification of carbon substrates with diazonium could afford a dense monolayer similar to the self-assembled monolayer (SAM) formation.

  11. Hydrogen Isotope Measurements of Organic Acids and Alcohols by Pyrolysis-GC-MS-TC-IRMS

    Science.gov (United States)

    Socki, Richard A.; Fu, Qi; Niles, Paul B.

    2011-01-01

    One possible process responsible for methane generation on Mars is abiotic formation by Fischer-Tropsch-type (FTT) synthesis during serpentinization reactions. Measurement of carbon and hydrogen isotopes of intermediary organic compounds can help constrain the origin of this methane by tracing the geochemical pathway during formation. Of particular interest within the context of this work is the isotopic composition of organic intermediaries produced on the surfaces of mineral catalysts (i.e. magnetite) during hydrothermal experiments, and the ability to make meaningful and reproducible hydrogen isotope measurements. Reported here are results of experiments to characterize the hydrogen isotope composition of low molecular weight organic acids and alcohols. The presence of these organic compounds has been suggested by others as intermeadiary products made during mineral surface catalyzed reactions. This work compliments our previous study characterizing the carbon isotope composition of similar low molecular weight intermediary organic compounds (Socki, et al, American Geophysical Union Fall meeting, Abstr. #V51B-2189, Dec., 2010). Our hydrogen isotope measurements utilize a unique analytical technique combining Pyrolysis-Gas Chromatograph-Mass Spectrometry-High Temperature Conversion-Isotope Ratio Mass Spectrometry (Py-GC-MS-TC-IRMS). Our technique is unique in that it carries a split of the pyrolyzed GC-separated product to a Thermo DSQ-II? quadrupole mass spectrometer as a means of making qualitative and semi-quantitative compositional measurements of separated organic compounds, therefore both chemical and isotopic measurements can be carried out simultaneously on the same sample.

  12. Modeling compositional dynamics based on GC and purine contents of protein-coding sequences

    KAUST Repository

    Zhang, Zhang; Yu, Jun

    2010-01-01

    Background: Understanding the compositional dynamics of genomes and their coding sequences is of great significance in gaining clues into molecular evolution and a large number of publically-available genome sequences have allowed us to quantitatively predict deviations of empirical data from their theoretical counterparts. However, the quantification of theoretical compositional variations for a wide diversity of genomes remains a major challenge.Results: To model the compositional dynamics of protein-coding sequences, we propose two simple models that take into account both mutation and selection effects, which act differently at the three codon positions, and use both GC and purine contents as compositional parameters. The two models concern the theoretical composition of nucleotides, codons, and amino acids, with no prerequisite of homologous sequences or their alignments. We evaluated the two models by quantifying theoretical compositions of a large collection of protein-coding sequences (including 46 of Archaea, 686 of Bacteria, and 826 of Eukarya), yielding consistent theoretical compositions across all the collected sequences.Conclusions: We show that the compositions of nucleotides, codons, and amino acids are largely determined by both GC and purine contents and suggest that deviations of the observed from the expected compositions may reflect compositional signatures that arise from a complex interplay between mutation and selection via DNA replication and repair mechanisms.Reviewers: This article was reviewed by Zhaolei Zhang (nominated by Mark Gerstein), Guruprasad Ananda (nominated by Kateryna Makova), and Daniel Haft. 2010 Zhang and Yu; licensee BioMed Central Ltd.

  13. Urease Inhibition of Fixed Oils and Fractions of Caralluma tuberculata: Component Identification by GC-MS

    International Nuclear Information System (INIS)

    Khan, M. A.; Khan, H.; Saeed, M.; Rauf, A.; Basharat, T.; Khan, A.

    2015-01-01

    The in vitro urease inhibitory activity of fixed oil and various organic fractions of Caralluma tuberculata followed by GC-MS analysis of the fixed oil are described in this research article. The fixed oil caused marked attenuation of jack bean urease with half-maximal inhibitory concentration (IC50) of 2.97 mg/ml. The similar urease inhibitory profile was observed for chloroform and ethyl acetate fractions with IC50 values of 3.36 and 4.90 mg/ml, respectively. GC-MS analysis led to the identification of 20 different constituents of the fixed oil by their m/z ratio and retention time in comparison with the standard compounds. The major constituents were methyl linoleate (30.97%) followed by methyl octadecadienoate (19.16%), ethyl linolenate (13.70 %), and methyl palmitate (9.86 %). The fixed oil and organic fractions of C. tuberculata exhibited marked urease inhibition and thus provide scientific background for use of the plant as antiulcer agent. (author)

  14. HS-GC-MS-O analysis and sensory acceptance of passion fruit during maturation.

    Science.gov (United States)

    Janzantti, Natália S; Monteiro, Magali

    2017-07-01

    The odor-active compounds of the conventional yellow passion fruit influence the aroma during ripeness and the acceptance of the juice. HS-GC-MS and GC-OSME analysis and sensory acceptance of the conventional passion fruit from different stages of ripeness were studied to characterize the aroma of the fruit and, aroma and flavor of the juice. Ethyl butanoate, ethyl hexanoate and propyl acetate showed high odoriferous importance in the passion fruit from the 1/3 yellow skin color. C is -3-hexen-1-ol and diethyl carbonate plus the odor-active compounds from the 1/3 yellow skin color showed high odoriferous importance in the 2/3 yellow skin color, and butyl acetate and alpha-terpineol plus the same odor-active compounds from 2/3 were the most important for the 3/3 yellow skin color. There was difference in the aroma and flavor of the juices, with higher acceptance means for the passion fruit from the 3/3 yellow skin color. The passion fruit volatile compounds peak area, odoriferous intensity and sensory acceptance of the juices increased during ripeness, indicating that the conventional passion fruit characteristic aroma is completely expressed when the fruit reaches the whole maturation, at the 3/3 yellow skin color.

  15. SPME-GC-MS analysis of commercial henna samples (Lawsonia inermis L.).

    Science.gov (United States)

    Mengoni, Tamara; Peregrina, Dolores Vargas; Censi, Roberta; Cortese, Manuela; Ricciutelli, Massimo; Maggi, Filippo; Di Martino, Piera

    2016-01-01

    The aim of this work was to provide a characterisation of volatile constituents from different commercial batches of henna (Lawsonia inermis) leaves of different geographic origin. Headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS) was used for the purpose. A total of 72 components were identified by GC-MS in the headspace of different henna samples which proved to differ considerably from each other, because they were characterised by different classes of components, mainly aliphatic compounds (9.0-64.7%), terpenoids (5.8-45.5%) and aromatics (7.9-45.2%), with alkanes (0.9-18.5%), aldehydes (2.1-18.8%) and carboxylic acids (3.1-29.3%), monoterpenes (3.4-30.0%) and sesquiterpenes (0.8-23.7%) and phenyl propanoids (0.6-43.1%), being the most abundant, respectively. Major representatives of these groups were n-hexadecane (0.5-4.7%), (2E)-hexenal (0.5-11.7%) and acetic acid (2.8-24.5%), limonene (0.8-14.7%), carvol (3.8-7.1%), geranyl acetone (1.4-7.9%) and (E)-caryophyllene (3.3-8.4%), and (E)-anethole (0.6-35.0%), respectively. We assume that factors such as the manufacturing process, the storage conditions and the different geographic origin of the samples may contribute to such variability.

  16. Optimization of Biochemical Screening Methods for Volatile and Unstable Sesquiterpenoids Using HS-SPME-GC-MS

    Directory of Open Access Journals (Sweden)

    Trine Bundgaard Andersen

    2015-06-01

    Full Text Available HS-SPME-GC-MS has been suggested as a fast and robust analytical platform for the product characterization of sesquiterpene synthases. The choice of fiber and injection temperature can have a significant effect on the observed product profile, due to the chemical rearrangements that can occur on the fiber material. Here we present a systematic study on the effects of fiber choice and injection port temperature on the observed sesquiterpenoid profile of four sesquiterpene synthases expressed in Nicotiana benthamiana. We found that the absorbent material PDMS was much less likely to support acid-induced rearrangement of sesquiterpenoids when compared to the adsorbent materials PDMS/DVB, PDMS/CAR, and PDMS/CAR/DVB. Furthermore, utilizing an injection port temperature at 160 °C almost eliminated the inherent thermal instability of germacrene sesquiterpenoids. Thus, for fast screening of sesquiterpene synthases, the results suggest that PDMS fibers and an injection temperature of 160 °C provide a fast and reproducible HS-SPME GC-MS method when using H2 as carrier gas.

  17. SPME GC/MS determination of organochlorine pesticides in water samples

    Directory of Open Access Journals (Sweden)

    Yerbolat Sailaukhanuly

    2013-05-01

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

  18. PY-GC-MS applied to the identification of synthetic resins in Brazilian painting

    International Nuclear Information System (INIS)

    Redigolo, Marcelo M.; Amaral, Priscila O.; Leao, Claudio; Crepaldi, Caike; Munita, Casimiro S.; Bustillos, Oscar V.; Russo, Tatiana; Mendonca, Valeria de

    2015-01-01

    Works of art are appreciated for their material and immaterial value. Restoring objects of art is a delicate procedure, mostly due to the irreversibility of the interventions. Hence, it is recommended to study the chemical composition of the object to avoid errors. The premise for restoring or conserving these objects is their physical preservation, i.e., it is advisable to avoid sampling and, when necessary, samples must be minute. The analytical techniques that fulfill these requirements are limited. Mass spectrometry (MS) is a versatile technique due to its hyphenation possibilities. Recently, it has being employed in the identification of natural and synthetic resins in works of art. Electron ionization (EI) is a powerful method of molecular fragmentation employed in the detection of volatile organic compounds by mass spectrometry. In this work, two micrograms (μg) of sample from a Brazilian contemporary painting were analyzed by pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) technique. A microfurnace-type pyrolyzer was coupled to a gas chromatograph, using a non-polar capillary column. The electron ionization was achieved applying 70 eV electron energy. This technique is suitable for the analysis of material from objects of art, being specific, accurate and requiring minimal sampling. The synthetic resin diallyl phthalate (DAP) was identified by the Py-GC/MS technique. (author)

  19. Determination of the Fatty Acid Content of Biological Membranes: A Highly Versatile GC-MS Experiment

    Science.gov (United States)

    Schultz, Emeric; Pugh, Michael Eugene

    2001-07-01

    The experiment involves the GC-MS of fatty acid methyl esters (FAMEs) obtained from bacterial membranes. It takes about 2 h, from cell harvest to injection. This experiment is done in a lab course for non-science majors and in biochemistry. For non-science majors the focus is on GC-MS as a technique for fingerprinting and on the underlying basis of that fingerprinting. In biochemistry the focus is on the composition of membranes and how this changes with temperature--specifically how the ratio of saturated to unsaturated fatty acids changes to maintain constant cell fluidity. Combined with a parallel DNA experiment, the two major types of intermolecular forces important for the structure and function of biomolecules are compared. How this versatile experiment could be adapted in other chemistry courses is presented. The experiment has obvious appeal to biology majors, can be used to develop several important chemistry concepts, involves teamwork, and employs an important instrument. It could be used in the laboratory portion of a course other than biochemistry to fulfill the new ACS biochemistry requirement.

  20. Determination of benzene in different food matrices by distillation and isotope dilution HS-GC/MS

    International Nuclear Information System (INIS)

    Medeiros Vinci, Raquel; Canfyn, Michael; De Meulenaer, Bruno; Schaetzen, Thibault de; Van Overmeire, Ilse; De Beer, Jacques; Van Loco, Joris

    2010-01-01

    Benzene is classified by the IARC as carcinogenic to humans. Several sources may contribute for the occurrence of benzene in foods, such as, environmental contamination and the reaction of benzoate salts with ascorbic acid (naturally present or added as food additives). Matrix effect on benzene recovery (e.g. in fatty foods) and artefactual benzene formation from benzoate during analysis in the presence of ascorbate are some of the challenges presented when determining benzene in a wide range of foodstuffs. Design of experiment (DOE) was used to determine the most important variables in benzene recovery from headspace GC/MS. Based on the results of the DOE, a versatile method for the extraction of benzene from all kind of food commodities was developed. The method which consisted of distillation and isotope dilution HS-GC/MS was in-house validated. Artefactual benzene was prevented by addition of a borate buffer solution (pH 11) under distillation conditions. The method presented in this study allows the use of a matrix-independent calibration with detection limits below the legal limit established by the European Council for benzene in drinking water (1 μg L -1 ).

  1. Modeling compositional dynamics based on GC and purine contents of protein-coding sequences

    KAUST Repository

    Zhang, Zhang

    2010-11-08

    Background: Understanding the compositional dynamics of genomes and their coding sequences is of great significance in gaining clues into molecular evolution and a large number of publically-available genome sequences have allowed us to quantitatively predict deviations of empirical data from their theoretical counterparts. However, the quantification of theoretical compositional variations for a wide diversity of genomes remains a major challenge.Results: To model the compositional dynamics of protein-coding sequences, we propose two simple models that take into account both mutation and selection effects, which act differently at the three codon positions, and use both GC and purine contents as compositional parameters. The two models concern the theoretical composition of nucleotides, codons, and amino acids, with no prerequisite of homologous sequences or their alignments. We evaluated the two models by quantifying theoretical compositions of a large collection of protein-coding sequences (including 46 of Archaea, 686 of Bacteria, and 826 of Eukarya), yielding consistent theoretical compositions across all the collected sequences.Conclusions: We show that the compositions of nucleotides, codons, and amino acids are largely determined by both GC and purine contents and suggest that deviations of the observed from the expected compositions may reflect compositional signatures that arise from a complex interplay between mutation and selection via DNA replication and repair mechanisms.Reviewers: This article was reviewed by Zhaolei Zhang (nominated by Mark Gerstein), Guruprasad Ananda (nominated by Kateryna Makova), and Daniel Haft. 2010 Zhang and Yu; licensee BioMed Central Ltd.

  2. Analysis of odorous gases with simultaneous GC-MS and sensory determination

    Energy Technology Data Exchange (ETDEWEB)

    Orko, I.; Lehtomaeki, J.; Sandell, E.; Arnold, M. [VTT Chemical Technology, Espoo (Finland). Environmental Technology

    1995-12-31

    Industrial odorous off-gases can consist of hundreds of different compounds giving cause to odour annoyance in the vicinity of the odour-emitting plant. For the identification of the odorous components in the gas, traditional analytical methods are not always sufficient since the odour threshold values cannot often be found in literature. This report describes the development of a GC-MS sniffing port method for identifying odorous compounds in off-gases. In the method the sample is injected into a gas chromatograph and divided into two flows. The compounds in these sample flows are separated in two identical columns and detected simultaneously in a mass spectrometer and by sensory means. The olfactory detections are marked in the iongram and the odorous compounds are identified. Tenax TA adsorbent is generally used for collecting the odorous sample for analysis. The compounds are released from the adsorbent for analysis by thermal desorption. The report also describes a case study where the GC-MS sniffing port method was applied to a gaseous emission from a food factory. Over ten odorous compounds could be identified. (author)

  3. Validation of rapid dioxin screening by GC-FID in fish products

    Energy Technology Data Exchange (ETDEWEB)

    Bassompierre, M.; Munck, L.; Bro, R.; Tomasi, G.; Engelsen, S.B. [Royal Veterinary and Agricultural Univ., Copenhagen (Denmark). Food Technology, Institute of Food Science, Centre for Advanced Food Studies

    2004-09-15

    A novel, cost- and time-effective dioxin screening method was developed and validated for fish product. The method is based on multivariate covariance between fatty acid composition monitored by GC-FID and dioxin content as teq WHO pg/ g fat. A dioxin range varying from 1.1 to 47.1 pg TEQ-WHO/ g fat using 65 fish meal samples was accessible for model calibration. An optimal multivariate dioxin prediction model was developed based on automatic peak integration, thereby enabling extraction of the area of 140 peaks from the gas chromatogramms. Models were produced employing partial least squares regression (PLS) based upon the duplicate GC-FID run and 46 specific peaks, selected after variable selection from the 140 investigated. The best results were yielded by local pls modelling employing three latent variables based upon the 12 nearest neighbors. For each prediction sample, the neighbors, yielding the 12 smallest sum of squares of differences to the test sample using the 140 peaks, were extracted from the whole calibration set and a local model built using these 12 chromatograms and related dioxin content. Prediction performance was thereafter validated for 10 fully independent samples. The performance of this model, yielded a correlation of 0.85 (r{sup 2}) and a root mean square error of prediction of 2.3 pg PCDD/F TEQWHO/ g fat.

  4. Steroids from Poison Hemlock (Conium maculatum L.: A GC-MS analysis

    Directory of Open Access Journals (Sweden)

    Radulović Niko S.

    2011-01-01

    Full Text Available The steroid content of Conium maculatum L. (Poison Hemlock, Apiaceae, a well-known weed plant species, was studied herein for the first time. This was achieved by detailed GC-MS analyses of twenty two samples (dichloromethane extracts of different plant organs of C. maculatum at three or four different stages of phenological development, collected from three locations. In total, twenty four different steroids were identified. Six steroids had an ergostane nucleus while the other ones possessed a stigmastane carbon framework. The identity of these compounds was determined by spectral means (MS fragmentation, GC co-injections with authentic standards and chemical transformation (silylation. Steroid compounds were noted to be the main chemical constituents of root extracts (up to 70 % of this plant species in the last phase of development. The predominant ones were stigmasta-5,22- dien-3β-ol (stigmasterol and stigmasta-5-en-3β-ol (β-sitosterol. In an attempt to classify the samples, principal component analysis (PCA and agglomerative hierarchical clustering (AHC were performed using steroid percentages as variables.

  5. Determination of benzene in different food matrices by distillation and isotope dilution HS-GC/MS

    Energy Technology Data Exchange (ETDEWEB)

    Medeiros Vinci, Raquel [Department of Food Safety and Food Quality, Faculty of Bioscience Engineering, Ghent University, Coupure Links 653, B-9000 Ghent (Belgium); Canfyn, Michael [Food, Medicines and Consumer Safety, Scientific Institute of Public Health, Rue Juliette Wytsmanstraat 14, 1050 Brussels (Belgium); De Meulenaer, Bruno [Department of Food Safety and Food Quality, Faculty of Bioscience Engineering, Ghent University, Coupure Links 653, B-9000 Ghent (Belgium); Schaetzen, Thibault de; Van Overmeire, Ilse; De Beer, Jacques [Food, Medicines and Consumer Safety, Scientific Institute of Public Health, Rue Juliette Wytsmanstraat 14, 1050 Brussels (Belgium); Van Loco, Joris, E-mail: Joris.VanLoco@iph.fgov.BE [Food, Medicines and Consumer Safety, Scientific Institute of Public Health, Rue Juliette Wytsmanstraat 14, 1050 Brussels (Belgium)

    2010-07-05

    Benzene is classified by the IARC as carcinogenic to humans. Several sources may contribute for the occurrence of benzene in foods, such as, environmental contamination and the reaction of benzoate salts with ascorbic acid (naturally present or added as food additives). Matrix effect on benzene recovery (e.g. in fatty foods) and artefactual benzene formation from benzoate during analysis in the presence of ascorbate are some of the challenges presented when determining benzene in a wide range of foodstuffs. Design of experiment (DOE) was used to determine the most important variables in benzene recovery from headspace GC/MS. Based on the results of the DOE, a versatile method for the extraction of benzene from all kind of food commodities was developed. The method which consisted of distillation and isotope dilution HS-GC/MS was in-house validated. Artefactual benzene was prevented by addition of a borate buffer solution (pH 11) under distillation conditions. The method presented in this study allows the use of a matrix-independent calibration with detection limits below the legal limit established by the European Council for benzene in drinking water (1 {mu}g L{sup -1}).

  6. GC-MS analysis of chemical compounds from acetone extract of Echium amoenum Fisch.

    Directory of Open Access Journals (Sweden)

    M.J. Chaichi

    2017-11-01

    Full Text Available Background and objectives: Plants play a significant role in the prevention and treatment of diseases and can even prevent and reduce the adverse effects of conventional treatments.  Echium amoenum Fisch is one of the most commonly used medicinal plants, and has long been used as a traditional herbal medicine for many diseases in Iran. Gas chromatography-mass spectrometry (GC-MS method can be an interesting tool for testing the amount of some active principles in herbs used in cosmetic, drugs, pharmaceutical or food industries. Methods: The flowers of Echium amoenum Fisch were collected, washed, shade dried, powdered and extracted with acetone using Soxhlet apparatus. The extract were concentrated and analyzed by GC-MS for the identification of chemical compounds present in the flowers of Echium amoenum. Results: The major compounds were pentacosane, tricosan, 2-pentanone-4-hydroxy-4-methyl and 3-hexene-2-one. Conclusion: Identification of these compounds in the plant serves as the basis in determining the possible health benefits of the plant leading to further biologic and pharmacologic studies.

  7. Quantification of Polyfunctional Thiols in Wine by HS-SPME-GC-MS Following Extractive Alkylation.

    Science.gov (United States)

    Musumeci, Lauren E; Ryona, Imelda; Pan, Bruce S; Loscos, Natalia; Feng, Hui; Cleary, Michael T; Sacks, Gavin L

    2015-07-06

    Analyses of key odorous polyfunctional volatile thiols in wines (3-mercaptohexanol (3-MH), 3-mercaptohexylacetate (3-MHA), and 4-mercapto-4-methyl-2-pentanone (4-MMP)) are challenging due to their high reactivity and ultra-trace concentrations, especially when using conventional gas-chromatography electron impact mass spectrometry (GC-EI-MS). We describe a method in which thiols are converted to pentafluorobenzyl (PFB) derivatives by extractive alkylation and the organic layer is evaporated prior to headspace solid phase microextraction (HS-SPME) and GC-EI-MS analysis. Optimal parameters were determined by response surface area modeling. The addition of NaCl solution to the dried SPME vials prior to extraction resulted in up to less than fivefold improvement in detection limits. Using 40 mL wine samples, limits of detection for 4-MMP, 3-MH, and 3-MHA were 0.9 ng/L, 1 ng/L, and 17 ng/L, respectively. Good recovery (90%-109%) and precision (5%-11% RSD) were achieved in wine matrices. The new method was used to survey polyfunctional thiol concentrations in 61 commercial California and New York State wines produced from V. vinifera (Riesling, Gewürztraminer, Cabernet Sauvignon, Sauvignon blanc and non-varietal rosé wines), V. labruscana (Niagara), and Vitis spp. (Cayuga White). Mean 4-MMP concentrations in New York Niagara (17 ng/L) were not significantly different from concentrations in Sauvignon blanc, but were significantly higher than 4-MMP in other varietal wines.

  8. Development of a sensitive GC-C-IRMS method for the analysis of androgens.

    Science.gov (United States)

    Polet, Michael; Van Gansbeke, Wim; Deventer, Koen; Van Eenoo, Peter

    2013-02-01

    The administration of anabolic steroids is one of the most important issues in doping control and is detectable through a change in the carbon isotopic composition of testosterone and/or its metabolites. Gas chromatography-combustion-isotope ratio mass spectrometry (GC-C-IRMS), however, remains a very laborious and expensive technique and substantial amounts of urine are needed to meet the sensitivity requirements of the IRMS. This can be problematic because only a limited amount of urine is available for anti-doping analysis on a broad spectrum of substances. In this work we introduce a new type of injection that increases the sensitivity of GC-C-IRMS by a factor of 13 and reduces the limit of detection, simply by using solvent vent injections instead of splitless injection. This drastically reduces the amount of urine required. On top of that, by only changing the injection technique, the detection parameters of the IRMS are not affected and there is no loss in linearity. Copyright © 2012 John Wiley & Sons, Ltd.

  9. EH-GC: An Efficient and Secure Architecture of Energy Harvesting Green Cloud Infrastructure

    Directory of Open Access Journals (Sweden)

    Saurabh Singh

    2017-04-01

    Full Text Available Nowadays, the high power consumption of data centers is the biggest challenge to making cloud computing greener. Many researchers are still seeking effective solutions to reduce or harvest the energy produced at data centers. To address this challenge, we propose a green cloud infrastructure which provides security and efficiency based on energy harvesting (EH-GC. The EH-GC is basically focused on harvesting the heat energy produced by data centers in the Infrastructure-as-a-Service (IaaS infrastructure. A pyroelectric material is used to generate the electric current from heat using the Olsen cycle. In order to achieve efficient green cloud computing, the architecture utilizes a genetic algorithm for proper virtual machine allocation, taking into consideration less Service Level Agreement (SLA violations. The architecture utilizes Multivariate Correlation Analysis (MCA correlation analysis based on a triangular map area generation to detect Denial of Service (DoS attacks in the data center layer of the IaaS. Finally, the experimental analysis is explained based on the energy parameter, which proves that our model is efficient and secure, and that it efficiently reuses the energy emitted from the data center.

  10. Identification of additives in poly(vinylacetate) artist's paints using PY-GC-MS.

    Science.gov (United States)

    Silva, Miguel F; Doménech-Carbó, Maria Teresa; Fuster-López, Laura; Mecklenburg, Marion F; Martin-Rey, Susana

    2010-05-01

    Commercial poly(vinyl acetate) (PVAc) paint formulations for artists include a number of compounds in addition to the PVAc polymer and pigments to improve the physical and chemical properties of the resulting product. Among the most common additives are surfactants, coalescing agents, defoamers, freeze-thaw agents and thickeners. These products significantly influence the behaviour of the dried film. Nevertheless, they are usually difficult to detect with conventional analytical methods given their low concentration. In order to identify these additives, present in the dried film as minor components, an analytical method based on in situ thermally assisted pyrolysis-silylation gas chromatography-mass spectrometry (GC-MS) using hexamethyldisilazane as a derivatisation reagent is proposed. This method improves the conventional GC-MS analysis performed by direct pyrolysis and enables the simultaneous identification of the PVAc binding medium and the additives included by the manufacturer in the commercial paint. Five different commercial PVAc paints have been analysed, namely, armour green, burnt umber, oriental red, raw umber and white from Flashe. Internal plasticiser VeoVa consisting of C(10) fatty acids with highly branched chains has been recognised from the MS spectra. On the other hand, the differences found in the additive content of the studied paints, in particular the poly(ethylene glycol)-type surfactant, are in good agreement with their mechanical properties.

  11. Dioxin analysis by gas chromatography-Fourier transform ion cyclotron resonance mass spectrometry (GC-FTICRMS).

    Science.gov (United States)

    Taguchi, Vince Y; Nieckarz, Robert J; Clement, Ray E; Krolik, Stefan; Williams, Robert

    2010-11-01

    The feasibility of utilizing a gas chromatograph-tandem quadrupole-Fourier transform ion cyclotron resonance mass spectrometer (GC-MS/MS-FTICRMS) to analyze chlorinated-dioxins/furans (CDDs/CDFs) and mixed halogenated dioxins/furans (HDDs/HDFs) was investigated by operating the system in the GC-FTICRMS mode. CDDs/CDFs and mixed HDDs/HDFs could be analyzed at 50,000 to 100,000 resolving power (RP) on the capillary gas chromatographic time scale. Initial experiments demonstrated that 1 pg of 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD) and 5 pg of 2-bromo-3,7,8-trichlorodibenzo-p-dioxin (BTrCDD) could be detected. The feasibility of utilizing an FTICRMS for screening of CDDs/CDFs, HDDs/HDFs and related compounds was also investigated by analyzing an extract from vegetation exposed to fall-out from an industrial fire. CDDs/CDFs, chlorinated pyrenes and chlorinated tetracenes could be detected from a Kendrick plot analysis of the ultrahigh resolution mass spectra. Mass accuracies were of the order of 0.5 ppm on standards with external mass calibration and 1 ppm on a sample with internal mass calibration. Copyright © 2010 American Society for Mass Spectrometry. Published by Elsevier Inc. All rights reserved.

  12. The optimization of phthalate analysis from plastic matrices by using GC/MS related techniques

    Science.gov (United States)

    Pusfitasari, Eka Dian; Hendarsyah, Hendris; Athaillah, Zatil Afrah

    2017-11-01

    Indication of malicious acts conducted by food vendors has been reported in many places in Indonesia and has been worrying the population. One of the issues is the indication that frying oil used by the vendors has been added with food packaging plastic to impart more crispy texture of the fried foods. One of the challenges for the monitoring process is to find suitable analytical method to identify this type of food adulteration. Because some food packaging, particularly from polyethylene group, contains plasticizer diethylhexylphthalate (DEHP), we intended to investigate the adulteration by detecting the phthalate compound. In this preliminary study, we focused on the optimization of GC equipment as well as the optimization of plastic extraction process with various types of solvents (hexane, dichloromethane, and acetonitrile) and extraction time (24, 48, and 72 hours). For 72-hour duration, treatment with solvent refreshment was also conducted to minimize solvent saturation effect. Our findings suggested that LOD and LOQ of the GC/MS instrument used for the DEHP analysis were 19.6 ng and 65.5 ng, respectively. In addition, it could be concluded that the process of plastic extraction through sonication for five minutes with n-hexane as a solvent resulted in the optimal value.

  13. GC-MS studies of the chemical composition of two inedible mushrooms of the genus Agaricus

    Directory of Open Access Journals (Sweden)

    Gjosheva Melania

    2007-12-01

    Full Text Available Abstract Background Mushrooms in the genus Agaricus have worldwide distribution and include the economically important species A. bisporus. Some Agaricus species are inedible, including A. placomyces and A. pseudopratensis, which are similar in appearance to certain edible species, yet are known to possess unpleasant odours and induce gastrointestinal problems if consumed. We have studied the chemical composition of these mushrooms using GC-MS. Results Our GC-MS studies on the volatile fractions and butanol extracts resulted in the identification of 44 and 34 compounds for A. placomyces and A. pseudopratensis, respectively, including fatty acids and their esters, amino acids, and sugar alcohols. The most abundant constituent in the volatiles and butanol were phenol and urea respectively. We also identified the presence of ergosterol and two Δ7-sterols. In addition, 5α,8α-Epidioxi-24(ξ-methylcholesta-6,22-diene-3β-ol was isolated for the first time from both mushrooms. Our study is therefore the first report on the chemical composition of these two species. Conclusion The results obtained contribute to the knowledge of the chemical composition of mushrooms belonging to the Agaricus genus, and provide some explanation for the reported mild toxicity of A. placomyces and A. pseudopratensis, a phenonomenon that can be explained by a high phenol content, similar to that found in other Xanthodermatei species.

  14. PY-GC-MS applied to the identification of synthetic resins in Brazilian painting

    Energy Technology Data Exchange (ETDEWEB)

    Redigolo, Marcelo M.; Amaral, Priscila O.; Leao, Claudio; Crepaldi, Caike; Munita, Casimiro S.; Bustillos, Oscar V., E-mail: marcelo.redigolo@usp.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Russo, Tatiana; Mendonca, Valeria de [Pinacoteca do Estado de Sao Paulo, SP (Brazil)

    2015-07-01

    Works of art are appreciated for their material and immaterial value. Restoring objects of art is a delicate procedure, mostly due to the irreversibility of the interventions. Hence, it is recommended to study the chemical composition of the object to avoid errors. The premise for restoring or conserving these objects is their physical preservation, i.e., it is advisable to avoid sampling and, when necessary, samples must be minute. The analytical techniques that fulfill these requirements are limited. Mass spectrometry (MS) is a versatile technique due to its hyphenation possibilities. Recently, it has being employed in the identification of natural and synthetic resins in works of art. Electron ionization (EI) is a powerful method of molecular fragmentation employed in the detection of volatile organic compounds by mass spectrometry. In this work, two micrograms (μg) of sample from a Brazilian contemporary painting were analyzed by pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) technique. A microfurnace-type pyrolyzer was coupled to a gas chromatograph, using a non-polar capillary column. The electron ionization was achieved applying 70 eV electron energy. This technique is suitable for the analysis of material from objects of art, being specific, accurate and requiring minimal sampling. The synthetic resin diallyl phthalate (DAP) was identified by the Py-GC/MS technique. (author)

  15. Carbon and Hydrogen Isotope Measurements of Alcohols and Organic Acids by Online Pyroprobe-GC-IRMS

    Science.gov (United States)

    Socki, Richard A.; Fu, Qi; Niles, Paul B.; Gibson, Everett K., Jr.

    2012-01-01

    The detection of methane in the atmosphere of Mars, combined with evidence showing widespread water-rock interaction during martian history, suggests that the production of methane on Mars may be the result of mineral surface-catalyzed CO2 and or CO reduction during Fisher-Tropsch Type (FTT) reactions. A better understanding of these reaction pathways and corresponding C and H isotope fractionations is critical to deciphering the synthesis of organic compounds produced under abiotic hydrothermal conditions. Described here is a technique for the extraction and analysis of both C and H isotopes from alcohols (C1-C4) and organic acids (C1-C6). This work is meant to provide a "proof of concept" for making meaningful isotope measurements on complex mixtures of solid-phase hydrocarbons and other intermediary products produced during high-temperature and high-pressure synthesis on mineral-catalyzed surfaces. These analyses are conducted entirely "on-line" utilizing a CDS model 5000 Pyroprobe connected to a Thermo Trace GC Ultra that is interfaced with a Thermo MAT 253 isotope ratio mass spectrometer operating in continuous flow mode. Also, this technique is designed to carry a split of the GC-separated product to a DSQ II quadrupole mass spectrometer as a means of making semi-quantitative compositional measurements. Therefore, both chemical and isotopic measurements can be carried out on the same sample.

  16. Analysis of Endocrine Disrupting Pesticides by Capillary GC with Mass Spectrometric Detection

    Directory of Open Access Journals (Sweden)

    Svetlana Hrouzková

    2012-09-01

    Full Text Available Endocrine disrupting chemicals, among them many pesticides, alter the normal functioning of the endocrine system of both wildlife and humans at very low concentration levels. Therefore, the importance of method development for their analysis in food and the environment is increasing. This also covers contributions in the field of ultra-trace analysis of multicomponent mixtures of organic pollutants in complex matrices. With this fact conventional capillary gas chromatography (CGC and fast CGC with mass spectrometric detection (MS has acquired a real importance in the analysis of endocrine disrupting pesticide (EDP residues. This paper provides an overview of GC methods, including sample preparation steps, for analysis of EDPs in a variety of matrices at ultra-trace concentration levels. Emphasis is put on separation method, mode of MS detection and ionization and obtained limits of detection and quantification. Analysis time is one of the most important aspects that should be considered in the choice of analytical methods for routine analysis. Therefore, the benefits of developed fast GC methods are important.

  17. Potential Health Benefits and Metabolomics of Camel Milk by GC-MS and ICP-MS.

    Science.gov (United States)

    Ahamad, Syed Rizwan; Raish, Mohammad; Ahmad, Ajaz; Shakeel, Faiyaz

    2017-02-01

    None of the research reports reveals the metabolomics and elemental studies on camel milk. Recent studies showed that camel milk possesses anticancer and anti-inflammatory activity. Metabolomics and elemental studies were carried out in camel milk which showed us the pathways and composition that are responsible for the key biological role of camel milk. Camel milk was dissolved in methanol and chloroform fraction and then vortexed and centrifuged. Both the fractions were derivatized by N,O-bis-(trimethylsilyl)trifluoroacetamide (BSTFA) and TMCS after nitrogen purging and analyzed by GC-MS. Camel milk was also analyzed by ICP-MS after microwave digestion. We found that higher alkanes and fatty acids are present in the chloroform fraction and amino acids, sugars and fatty acid derivatives are present in aqueous fractions. All the heavy metals like As, Pb, Cd, Co, Cu, and Ni were in the safe limits in terms of maximum daily intake of these elements. Na, K, Mg, and Ca were also present in the safe limits in terms of maximum daily intake of these elements. These results suggested that the camel milk drinking is safe and there is no health hazard. The present data of GC-MS and ICP-MS correlate the activities related to camel milk.

  18. Desulfurization of petroleum by Co-60 gamma irradiation and analysis of products using GC-MS

    International Nuclear Information System (INIS)

    Mathuthu, M.; Tshivhase, V.M.; Olobatoke, R.Y.; Gaxela, N.N.

    2014-01-01

    Sulfur is an undesirable hetero-atom that has negative on motor engines if present in quantities between 50 and 180.000 ppm. Research has shown that sour petroleum can be 'sweetened' by gamma irradiation to de-sulfurize the crude oil. In this research we will report experimental results of desulfurizing petroleum locally procured. The objective is to improve the quality of product delivered to the motor market and also reduce the environmental pollution due to SO 2 emissions from engines. The gamma irradiated (de-sulfurized petroleum was chemically analyzed using GC-MS. The preliminary results show that the petroleum is polymerized by gamma radiation to higher molecular mass. The un-irradiated petroleum had a sulfur concentration of 3.24% and 0.020% wt after gamma irradiation. The sulfur content was reduced by a factor of about 160 when dose was increased from zero to 50 kGys. GC-MS Chromatographs are presented for the identified hydrocarbons after gamma irradiation. (authors)

  19. Automated GC-MS analysis of free amino acids in biological fluids.

    Science.gov (United States)

    Kaspar, Hannelore; Dettmer, Katja; Gronwald, Wolfram; Oefner, Peter J

    2008-07-15

    A gas chromatography-mass spectrometry (GC-MS) method was developed for the quantitative analysis of free amino acids as their propyl chloroformate derivatives in biological fluids. Derivatization with propyl chloroformate is carried out directly in the biological samples without prior protein precipitation or solid-phase extraction of the amino acids, thereby allowing automation of the entire procedure, including addition of reagents, extraction and injection into the GC-MS. The total analysis time was 30 min and 30 amino acids could be reliably quantified using 19 stable isotope-labeled amino acids as internal standards. Limits of detection (LOD) and lower limits of quantification (LLOQ) were in the range of 0.03-12 microM and 0.3-30 microM, respectively. The method was validated using a certified amino acid standard and reference plasma, and its applicability to different biological fluids was shown. Intra-day precision for the analysis of human urine, blood plasma, and cell culture medium was 2.0-8.8%, 0.9-8.3%, and 2.0-14.3%, respectively, while the inter-day precision for human urine was 1.5-14.1%.

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

    Science.gov (United States)

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

    2016-01-01

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

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

    Science.gov (United States)

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

    2008-02-01

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

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

    Directory of Open Access Journals (Sweden)

    Pablo Guardado-Calvo

    2016-10-01

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

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

    Science.gov (United States)

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

    2003-04-23

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

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

    Science.gov (United States)

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

    2015-09-01

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

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

    Science.gov (United States)

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

    2002-05-01

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

  6. 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

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

    International Nuclear Information System (INIS)

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

    2016-01-01

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

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

    Science.gov (United States)

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

    2015-01-01

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

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

    CSIR Research Space (South Africa)

    Opoku, F

    2018-01-01

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

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

    Science.gov (United States)

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

    2010-03-01

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

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

    Science.gov (United States)

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

    2018-02-01

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

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

    Science.gov (United States)

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

    2008-01-01

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

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

    Science.gov (United States)

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

    2017-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Cécile Philippe

    2018-01-01

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

  15. Matrix interference evaluation employing GC and LC coupled to triple quadrupole tandem mass spectrometry.

    Science.gov (United States)

    Uclés, S; Lozano, A; Sosa, A; Parrilla Vázquez, P; Valverde, A; Fernández-Alba, A R

    2017-11-01

    Gas and liquid chromatography coupled to triple quadrupole tandem mass spectrometry are currently the most powerful tools employed for the routine analysis of pesticide residues in food control laboratories. However, whatever the multiresidue extraction method, there will be a residual matrix effect making it difficult to identify/quantify some specific compounds in certain cases. Two main effects stand out: (i) co-elution with isobaric matrix interferents, which can be a major drawback for unequivocal identification, and therefore false negative detections, and (ii) signal suppression/enhancement, commonly called the "matrix effect", which may cause serious problems including inaccurate quantitation, low analyte detectability and increased method uncertainty. The aim of this analytical study is to provide a framework for evaluating the maximum expected errors associated with the matrix effects. The worst-case study contrived to give an estimation of the extreme errors caused by matrix effects when extraction/determination protocols are applied in routine multiresidue analysis. Twenty-five different blank matrices extracted with the four most common extraction methods used in routine analysis (citrate QuEChERS with/without PSA clean-up, ethyl acetate and the Dutch mini-Luke "NL" methods) were evaluated by both GC-QqQ-MS/MS and LC-QqQ-MS/MS. The results showed that the presence of matrix compounds with isobaric transitions to target pesticides was higher in GC than under LC in the experimental conditions tested. In a second study, the number of "potential" false negatives was evaluated. For that, ten matrices with higher percentages of natural interfering components were checked. Additionally, the results showed that for more than 90% of the cases, pesticide quantification was not affected by matrix-matched standard calibration when an interferent was kept constant along the calibration curve. The error in quantification depended on the concentration level. In a

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

    Institute of Scientific and Technical Information of China (English)

    Joselin Joseph; Solomon Jeeva

    2016-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Joselin Joseph

    2016-05-01

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

  18. PHYTOCHEMICAL ASSESSMENT ON N-HEXANE EXTRACT AND FRACTIONS OF Marsilea crenata Presl. LEAVES THROUGH GC-MS

    Directory of Open Access Journals (Sweden)

    Burhan Ma'arif

    2016-08-01

    Full Text Available Estrogen deficiency causes various health problems in postmenopausal women, including osteoporosis. Phytoestrogen emerged as a potential alternative of estrogen with minimum side effects. Green clover (Marsilea crenata Presl. is a typical plant in East Java which suspected contains estrogen-like substances. The aim of this research was to report the phytochemical properties of M. crenata using GC-MS as a preliminary study. M. crenata leaves were dried and extracted with n-hexane, then separated using vacuum column chromatography to get four fractions, after that the n-hexane extract and four fractions were identified with GC-MS. The results of GC-MS analysis showed some compounds contained in M. crenata leaves like monoterpenoid, diterpenoid, fatty acid compounds, and other unknown compounds. The results obtained in this research indicated a promising potential of M. crenata as medicinal plants, especially as antiosteoporotic agent.

  19. Detection limits in the chromatographic element trace analysis - quantitative TLC, HPLC and GC with the example of beryllium acetylacetonate

    International Nuclear Information System (INIS)

    Schwedt, G.

    1981-01-01

    Chromatographic analyses of beryllium acetylacetonate are carried out in synthetic solutions within the nano- and picogram range of beryllium. For thin-layer chromatography (TLC) normal and silanized silica gel is used, for high-performance liquid chromatography (HPLC) silica gel of 7 μm particles, for gas chromatography (GC) silicone SE-30 as stationary phase. Visual evaluation and remission measurements in TLC, UV-254 nm absorption measurements in HPLC and measurements with a FID in GC are employed for the determination of the calibration curves. A calibration curve through the origin and a detection limit of 150 pg Be determinable form are received by HPLC only. For trace analyses by GC a new definition of a detection limit for the evaluation of substance peaks on a solvent tailing is suggested. (orig.) [de

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

    Directory of Open Access Journals (Sweden)

    Praveen K. Yadav

    2017-12-01

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

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

    International Nuclear Information System (INIS)

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

    1991-01-01

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

  2. Improved solar light stimulated charge separation of g-C3N4 through self-altering acidic treatment

    Science.gov (United States)

    Leong, Kah Hon; Lim, Ping Feng; Sim, Lan Ching; Punia, Varun; Pichiah, Saravanan

    2018-02-01

    Herein, we report the use of acid treatment to treat g-C3N4 nanostructured by a direct and facile synthesis route. The adopted treatment enhanced photoactivity of g-C3N4 and reflected in the removal of recalcitrant organic pollutant, Bisphenol A under direct sunlight. A complete removal of Bisphenol A was attained in a short duration (225 min) as compared to pure g-C3N4. The analysis clearly substantiated the robustness of acid exfoliation that promoted a blue shift, extended the conjugated length of its respective conduction and valance band. It also drastically prolonged the recombination rate of charge carriers, by producing excess of unpaired electrons in the conduction band for active radicals' generation. Thus, this new findings could offer a new sight of self-alteration in improving the photoactivity of complex organic pollutants for sustainable environmental remediation.

  3. Fate of iprovalicarb, indoxacarb, and boscalid residues in grapes and wine by GC-ITMS analysis.

    Science.gov (United States)

    Angioni, Alberto; Dedola, Fabrizio; Garau, Vincenzo Luigi; Schirra, Mario; Caboni, Pierluigi

    2011-06-22

    The behavior in field and the transfer from grapes to wine during winemaking of iprovalicarb, indoxacarb, and boscalid was studied. The residue levels found in grapes were far below the MRLs set for grapes in EU, accounting at harvest time 0.81, 0.43, and 4.23 mg/kg for iprovalicarb, indoxacarb, and boscalid, respectively. The residue levels in the samples treated with boscalid may have residual problems (due to an accumulation effect) if repeated field treatments will be performed. Winemaking experiments showed a complete transfer of all pesticide from grapes to the must, while in wine the residues were low or negligible due to the adsorbing effect of lees and pomace. The clarification experiments showed a good removal of pesticide residues from the wine media, for all pesticides. The GC-ITMS method showed good performance with adequate recoveries ranging from 75 to 115%, and good method limits of quantitation (LOQs) and of determination (LODs) far below MRLs.

  4. Methylation effect on the ohmic resistance of a poly-GC DNA-like chain

    Energy Technology Data Exchange (ETDEWEB)

    Moura, F.A.B.F. de, E-mail: fidelis@fis.ufal.br [Instituto de Física, Universidade Federal de Alagoas, Maceió AL 57072-970 (Brazil); Lyra, M.L. [Instituto de Física, Universidade Federal de Alagoas, Maceió AL 57072-970 (Brazil); Almeida, M.L. de; Ourique, G.S.; Fulco, U.L.; Albuquerque, E.L. [Departamento de Biofísica e Farmacologia, Universidade Federal do Rio Grande do Norte, 59072-970, Natal-RN (Brazil)

    2016-10-14

    We determine, by using a tight-binding model Hamiltonian, the characteristic current–voltage (IxV) curves of a 5-methylated cytosine single strand poly-GC DNA-like finite segment, considering the methyl groups attached laterally to a random fraction of the cytosine basis. Striking, we found that the methylation significantly impacts the ohmic resistance (R) of the DNA-like segments, indicating that measurements of R can be used as a biosensor tool to probe the presence of anomalous methylation. - Highlights: • Ohmic resistance of finite segments of poly-CG DNA-like segments. • Possibility for the development of biosensor devices. • Methylation effect and electronic transport in DNA-like segments.

  5. Rapid Quantification of Abscisic Acid by GC-MS/MS for Studies of Abiotic Stress Response.

    Science.gov (United States)

    Verslues, Paul E

    2017-01-01

    Drought and low water potential induce large increases in Abscisic Acid (ABA ) content of plant tissue. This increased ABA content is essential to regulate downstream stress resistance responses; however, the mechanisms regulating ABA accumulation are incompletely known. Thus, the ability to accurately quantify ABA at high throughput and low cost is important for plant stress research. We have combined and modified several previously published protocols to establish a rapid ABA analysis protocol using gas chromatography-tandem mass spectrometry (GC-MS/MS). Derivatization of ABA is performed with (trimethylsilyl)-diazomethane rather than the harder to prepare diazomethane. Sensitivity of the analysis is sufficient that small samples of low water potential treated Arabidopsis thaliana seedlings can be routinely analyzed in reverse genetic studies of putative stress regulators as well as studies of natural variation in ABA accumulation.

  6. Determination of prilocaine HCl in bulk drug and pharmaceutical formulation by GC-NPD method

    Directory of Open Access Journals (Sweden)

    Atila Alptug

    2013-01-01

    Full Text Available The novel analytical method was developed and validated for determination of prilocaine HCl in bulk drug and pharmaceutical formulation by gas chromatography-nitrogen phosphorus detection (GC-NPD. The chromatographic separation was performed using a HP-5MS column. The calibration curve was linear over the concentration range of 40-1000 ng ml-1 with a correlation coefficient of 0.9998. The limits of detection (LOD and quantification (LOQ of method were 10 ng ml-1 and 35 ng ml-1, respectively. The within-day and between-day precision, expressed as the percent relative standard deviation (RSD% was less than 5.0%, and accuracy (percent relative error was better than 4.0%. The developed method can be directly and easily applied for determination of prilocaine HCl in bulk drug and pharmaceutical formulation using internal standard methodology.

  7. Radioimmunoassay screening and GC/MS confirmation of whole blood samples for drugs of abuse

    Energy Technology Data Exchange (ETDEWEB)

    Spiehler, V.R.; Sedgwick, P.

    From 1981 to 1984, an average of 300 radioimmunoassay screens on whole blood were performed each week in the authors laboratory. Most samples were screened for opiates phencyclidine and its analogs, barbiturates, and cocaine or its metabolite benzoylecgonine. A commercially available radioimmunoassay was used with modifications to facilitate screening of whole blood. Increasing sample size increased the sensitivity of the assay. Changing reagent concentration (1:1 dilution), incubation time, sample matrix (water, urine, or blood), or fraction counted (precipitate or supernatant) did not affect the utility of the standard curve or the sensitivity of the assay. All positive results for phencyclidine, opiates, cocaine, and related compounds were confirmed by GC/MA. Barbiturate positives were confirmed by UV spectrophotometry.

  8. Study of the red lacquer from a pair of Namban stirrups by Py-GC/MS

    Directory of Open Access Journals (Sweden)

    José Carlos Frade

    2009-01-01

    Full Text Available Oriental lacquer is a material of vegetal origin that is used in the Asian countries as a coating for the most varied kinds of religious and civil use objects. With the Portuguese arrival to the East, the Europeans started to develop a taste for the exotic and exquisite Art of Lacquer. From the 16th century onwards a lacquerware market developed with numerous lacquered objects being brought to Europe. In this work, the red lacquer from a pair of Namban stirrups was studied by Py-GC/MS (pyrolysis-gas chromatography/mass spectrometry. The results were compared with lacquer references, and the lacquer type was identified. Based on the results, the stirrups' lacquering technique and the performance of Py-CG/MS in the identification of oriental lacquers are also discussed.

  9. Analysis of Amaryllidaceae alkaloids from Zephyranthes grandiflora by GC/MS and their cholinesterase activity

    Directory of Open Access Journals (Sweden)

    Lucie Cahlíková

    2011-05-01

    Full Text Available Amaryllidaceae are known as ornamental plants, furthermore some species of this family contain galanthamine, an acetylcholinesterase inhibitor approved for the treatment of Alzheimer's disease, and other alkaloids with interesting pharmacological activity. The chemical composition of alkaloids from Zephyranthes grandiflora Lindl. was analyzed by GC/MS. Seven known compounds, belonging to five structural types of Amaryllidaceae alkaloids, were identified. The alkaloid extract from the bulbs showed promising cholinesterase inhibitory activities against human blood acetylcholinesterase (HuAChE; IC50 39.2±3.0 µg/mL and human plasma butyrylcholinesterase (HuBuChE; IC50 356±9.3 µg/mL.

  10. Analysis of Amaryllidaceae alkaloids from Zephyranthes grandiflora by GC/MS and their cholinesterase activity

    Directory of Open Access Journals (Sweden)

    Lucie Cahlíková

    2011-08-01

    Full Text Available Amaryllidaceae are known as ornamental plants, furthermore some species of this family contain galanthamine, an acetylcholinesterase inhibitor approved for the treatment of Alzheimer's disease, and other alkaloids with interesting pharmacological activity. The chemical composition of alkaloids from Zephyranthes grandiflora Lindl. was analyzed by GC/MS. Seven known compounds, belonging to five structural types of Amaryllidaceae alkaloids, were identified. The alkaloid extract from the bulbs showed promising cholinesterase inhibitory activities against human blood acetylcholinesterase (HuAChE; IC50 39.2±3.0 µg/mL and human plasma butyrylcholinesterase (HuBuChE; IC50 356±9.3 µg/mL.

  11. IDENTIFIKASI SENYAWA AKTIF DAUN PLETEKAN (Ruellia tuberosa L. DENGAN MENGGUNAKAN GC-MS

    Directory of Open Access Journals (Sweden)

    Ida Ayu Nopiari

    2017-02-01

    Full Text Available ABSTRACT The use of traditional medicines in human therapies has been claimed to be much safer than that of synthetic medicines with many negative side effects. Pletekan plant (Ruellia tuberosa L. has been used empirically for years as an antidiabetic as its leaves contain poly phenolic compounds with the ability to stimulate beta cells of the pancreas so that its capability to produce insulin improved. The main objective of our research was to identify active compounds contained in Ruellia tuberosa L. leaves extracted with ethanol. Fractionation of these active compounds was conducted by applying column and thin layer chromatography using Dichlorometan and Ethylacetat with a ratio of 6:3 as eluent. Each active compound resulted from fractionation was identified using GC-MS analysis. The results showed that four active compounds (Hexadecanamide, 9-Octadecenamide, (Z, Octadecenamide and 1,2-Benzenedicarboxylic acid were identified in this analysis. Keywords: Ruellia tuberosa L., identification of active compounds.

  12. Evaluation of the volatile profile of Tuber liyuanum by HS-SPME with GC-MS.

    Science.gov (United States)

    Liu, Changjiao; Li, Yu

    2017-04-01

    The volatile components of Tuber liyuanum were determined by HS-SPME with GC-MS for the first time. The effects of different fibre coating, extraction time, extraction temperature and sample amount were studied to get optimal extraction conditions. The optimal conditions were SPME fibre of Carboxen/PDMS, extraction time of 40 min, extraction temperature of 80 °C, sample amount of 2 g. Under these conditions 57 compounds in volatile of T. liyuanum were detected with a resemblance percentage above 80%. Aldehydes and aromatics were the main chemical families identified. The contribution of 3-Octanone(11.67%), phenylethyl alcohol (10.60%), isopentana (9.29%) and methylbutana (8.06%) for the total volatile profile were more significant in T. liyuanum than other compounds.

  13. Differentiation of Toxic Molds via Headspace SPME-GC/MS and Canine Detection

    Directory of Open Access Journals (Sweden)

    Kenneth G. Furton

    2007-08-01

    Full Text Available Indoor mold growth has recently become a concern in the legal world in regards to insurance litigation. Hazardous mold exposure to humans has been linked to many acute and chronic adverse health effects including death. As it grows, mold produces several types of primary and secondary metabolites, including microbial volatile organic compounds (MVOCs. Microbial volatile organic compound emission may be used as a preliminary indication of a mold infestation that is invisible to the unaided eye. The objective of the study is to identify the unique odor signatures of three species of molds, Aspergillus versicolor, Penicillium chrysogenum, and Stachybotrys chartarum by SPME-GC/MS analysis. Determining the compounds that are emitted by the selected species has made it possible to conduct validation studies of canine detection of these mold species through a series of field tests.

  14. Qualitative and quantitative assessment of fatty acids of buddleja asiatica by GC-MS

    International Nuclear Information System (INIS)

    Ali, F.; Ali, I.; Bibi, H.; Malik, A.

    2013-01-01

    To analyze the fatty acid contents of Buddleja asiatica Lour,both the non-volatile oil and fat obtained from the n-hexane soluble sub- fraction were subjected to GC/MS using BSTFA (N,O-bis(trimethylsilyl) trifloroacetamide) derivatization. The oil showed the presence of six fatty acids including palmitic acid (46.75 %), linoleic acid (37.80 %), stearic acid (10.98 %), arachidic acid, margaric acid and lignoceric acid (< 3 %) . Analysis of the fat revealed nine fatty acids including lignoceric acid (43.12 %), behenic acid (26.39 %), arachidic acid (9.29 %) and stearic acid (5.3 %). Cerotic acid, montanic acid, melissic acid and palmitic acid were found in low amounts (< 5 %) while trycosylic acid (4.83 %) was the only fatty acid with odd number of carbon atoms. The oil showed a low thermal stability. (author)

  15. Butyltin speciation in sediments from Todos os Santos Bay (Bahia, Brazil by GC-PFPD

    Directory of Open Access Journals (Sweden)

    Juliana Feitosa Felizzola

    2008-01-01

    Full Text Available Butyltin compounds were investigated in surface sediments from 17 stations in Todos os Santos Bay. Analytical conditions for organotin determination in marine sediments were optimized for GC with pulsed flame photometric detection. Detection limits were: 5.4 µg kg-1 for TBT; 0.2 µg kg-1 for DBT; and 2.1 µg kg-1 for MBT, using a 610-nm filter. In general, TBT concentrations were low and in the range of

  16. A tailing genome walking method suitable for genomes with high local GC content.

    Science.gov (United States)

    Liu, Taian; Fang, Yongxiang; Yao, Wenjuan; Guan, Qisai; Bai, Gang; Jing, Zhizhong

    2013-10-15

    The tailing genome walking strategies are simple and efficient. However, they sometimes can be restricted due to the low stringency of homo-oligomeric primers. Here we modified their conventional tailing step by adding polythymidine and polyguanine to the target single-stranded DNA (ssDNA). The tailed ssDNA was then amplified exponentially with a specific primer in the known region and a primer comprising 5' polycytosine and 3' polyadenosine. The successful application of this novel method for identifying integration sites mediated by φC31 integrase in goat genome indicates that the method is more suitable for genomes with high complexity and local GC content. Copyright © 2013 Elsevier Inc. All rights reserved.

  17. Authenticity of raspberry flavor in food products using SPME-chiral-GC-MS

    DEFF Research Database (Denmark)

    Hansen, Anne-Mette Sølvbjerg; Frandsen, Henrik Lauritz; Fromberg, Arvid

    2015-01-01

    A fast and simple method for authenticating raspberry flavors from food products was developed. The two enantiomers of the compound (E)-α-ionone from raspberry flavor were separated on a chiral gas chromatographic column. Based on the ratio of these two enantiomers the naturalness of a raspberry...... flavor can be evaluated due to the fact that a natural flavor will consist almost exclusively of the R enantiomer, while a chemical synthesis of the same compound will result in a racemic mixture. 27 food products containing raspberry flavors where investigated using SPME-chiral-GC-MS. We found raspberry...... distribution of the R and S isomer. Two products were labelled to contain natural raspberry flavors but were found to contain almost equal amounts of both enantiomers indicating a presence of synthetic raspberry flavors only. Additionally, two products labelled to contain both raspberry juice and flavor showed...

  18. GC-FTIR-MS analysis of volatile radiolytic products in the radiolysis of nitroaniline

    International Nuclear Information System (INIS)

    Kuruc, J.; Sahoo, M.K.; Kubinec, R.

    1993-01-01

    A good deal of products formed in the γ-radiolysis of isomeric nitroaniline solutions in carbon tetrachloride have been identified using GC-FTIR-MS technique. Tetrachloroethylene, chlorobenzene, hexachloroethane isomeric di-, tri- and tetrachlorobenzenes and chloroisocyanatobenzenes are among the important products formed in the radiolysis. Formation of dichlorobenzene is the result of ipso-substitution of both the nitro and aniline group by chlorine atom and the subsequent chloration of dichlorobenzene results in the formation of polychlorobenzenes. Chloroisocyanatobenzene is proposed to be the product arising from the interaction of dichlorocarbene and the nitro group of nitroaniline followed by chlorination of the resulting product, isocyanatobenzene. A 94% yield of undissolved 1,2-aminonitrobenzene chloride salt is obtained from the radiolysis of o-nitroaniline solution in carbon tetrachloride with a radiation yield of 1.83 molecules per 100 eV absorbed energy for an irradiation dose of 267 kGy. (author) 9 refs.; 3 figs.; 2 tabs

  19. GC-MS analysis and cardiovascular activity of the essential oil of Ocotea duckei

    Directory of Open Access Journals (Sweden)

    José M. Barbosa-Filho

    Full Text Available The essential oils obtained by steam distillation from the roots, stems, leaves and fruits of Ocotea duckei had their composition analyzed by GC-MS. The pharmacological activity of these oils was also evaluated showing significant cardiovascular effects. Forty-nine substances were identified, consisting of a complex mixture of monoterpenes (45% and sesquiterpenes (55%. The fruits yielded (1.9% more essential oil than the stems (1.0%, roots (0.8% and leaves (0.7%. The main component in the oil of the leaves was trans-caryophyllene (60.54%, in the stem bark beta-eudesmol (27.51% and in the fruits, dl-limonene (30.12%. The predominant essential oil component in the roots was elemol (24.31%. In non-anaesthetized normotensive rats, the essential oils from different parts of Ocotea duckei (leaves, fruits, stem and roots induced significant (p < 0.05 hypotension followed by bradycardia.

  20. Gc-ms, hplc profiling, antioxidant, antimicrobial and cytotoxicity studies of malcolmia africana leaves

    International Nuclear Information System (INIS)

    Bokhari, T.H.; Rasool, N.; Riaz, M.; Riaz, M.

    2014-01-01

    Plants are known to be the richest source of natural antioxidant and antimicrobial properties. The use of herbs and medicinal plants as the first medicines is a universal phenomenon. The present study was carried out to examine the antioxidant, antimicrobial and cytotoxicity potential Malcolmia africana leaves extract, fraction, essential oil and fixed oil. The whole plant was extracted with absolute methanol and further fractionated with increasing polarity based absolute solvents. Different fractions were taken by solvent extraction method and their antimicrobial activities were determined. The IC50 and % inhibition by linoleic acid oxidation was evaluated for the antioxidant studies. The cytotoxicity of the plant extract and fractions were assayed against human blood erythrocytes (RBCs). The DPPH scavenging and linoleic acid oxidation assays were carried out. Qualitative and quantitative analysis of secondary metabolites was also carried out. The presence of phenolics was also studied by HPLC. The GC-MS analysis of Malcolmia africana essential oil and fixed oil was also carried out. (author)

  1. [Analysis of chemical constituents of volatile components from Jia Ga Song Tang by GC-MS].

    Science.gov (United States)

    Tan, Qing-long; Xiong, Tian-qin; Liao, Jia-yi; Yang, Tao; Zhao, Yu-min; Lin, Xi; Zhang, Cui-xian

    2014-10-01

    To analyze the chemical components of volatile components from Jia Ga Song Tang. The volatile oils were extracted by water steam distillation. The chemical components of essential oil were analyzed by GC-MS and quantitatively determined by a normalization method. 103 components were separated and 87 components were identified in the volatile oil of Zingiberis Rhizoma. 58 components were separated and 38 components were identified in the volatile oil of Myristicae Semen. 49 components were separated and 38 components were identified in the volatile oil of Amomi Rotundus Fructus. 89 components were separated and 63 components were identified in the volatile oil of Jia Ga Song Tang. Eucalyptol, β-phellandrene and other terpenes were the main compounds in the volatile oil of Jia Ga Song Tang. Changes in the kinds and content of volatile components can provide evidences for scientific and rational compatibility for Jia Ga Song Tang.

  2. GC/MS analysis of pesticides in the Ferrara area (Italy) surface water: a chemometric study.

    Science.gov (United States)

    Pasti, Luisa; Nava, Elisabetta; Morelli, Marco; Bignami, Silvia; Dondi, Francesco

    2007-01-01

    The development of a network to monitor surface waters is a critical element in the assessment, restoration and protection of water quality. In this study, concentrations of 42 pesticides--determined by GC-MS on samples from 11 points along the Ferrara area rivers--have been analyzed by chemometric tools. The data were collected over a three-year period (2002-2004). Principal component analysis of the detected pesticides was carried out in order to define the best spatial locations for the sampling points. The results obtained have been interpreted in view of agricultural land use. Time series data regarding pesticide contents in surface waters has been analyzed using the Autocorrelation function. This chemometric tool allows for seasonal trends and makes it possible to optimize sampling frequency in order to detect the effective maximum pesticide content.

  3. GC/MS Analysis of Pesticides in the Ferrara Area (Italy) Surface Water: A Chemometric Study

    International Nuclear Information System (INIS)

    Pasti, L.; Dondi, F.; Nava, E.; Morelli, M.; Bignami, S.

    2007-01-01

    The development of a network to monitor surface waters is a critical element in the assessment, restoration and protection of water quality. In this study, concentrations of 42 pesticides - determined by GC-MS on samples from 11 points along the Ferrara area rivers - have been analyzed by chemometric tools. The data were collected over a three-year period (2002-2004). Principal component analysis of the detected pesticides was carried out in order to define the best spatial locations for the sampling points. The results obtained have been interpreted in view of agricultural land use. Time series data regarding pesticide contents in surface waters has been analyzed using the Autocorrelation function. This chemometric tool allows for seasonal trends and makes it possible to optimize sampling frequency in order to detect the effective maximum pesticide content

  4. The determination of quizalofop-p-tefuryl, Pantera, and metabolites in soils using GC/MSD

    Energy Technology Data Exchange (ETDEWEB)

    Parkins, M.D. [Uniroyal Chemical Co. Inc., Middlebury, CT (United States); Bruns, G. [EnviroTest Labs., Inc., Edmonton, Alberta (Canada)

    1995-12-01

    A published procedure for the analysis of herbicides in soil and sediment was adapted for determining residues of Pantera, quizalofop-p-tefuryl, and its metabolites. Soil is extracted by shaking with a solvent mixture of acetone/0.05N HCL, followed by 0.1 N KOH. The extracts are combined, acidified and then partitioned with methylene chloride. The organic phase is concentrated to 1.0 mL. One half the sample is reacted with diazomethane and analyzed for parent compound and the methyl derivative of the acid metabolite, quizalofop, by GC/MSD with no further workup. The other half is reacted with diazomethane using an elevated temperature, to form volatile methyl derivatives of the metabolites; chlorohydroxyquinoxaline, and chloroquinoxaline phenol. Recoveries were determined at 0.02 ppm, the level of detection, and at 0.20 ppm. The average recovery value for all analytes was greater than 90%.

  5. Identification and measurement of pesticide contaminants in food products by electron impact GC/MS

    International Nuclear Information System (INIS)

    Tusa, Florina; Moldovan, Zaharie; Vlassa, Mircea

    2009-01-01

    The paper concern is determination of eight pesticides in food products samples. The target compounds are: Lindane, Heptachlor, Aldrin, o,p-DDE, Dieldrin, Endrin, p,p'-DDT, and Methoxychlor. The compounds quantities were performed from chromatographic area obtained in full scan GC/MS mode after baseline separation and by comparation with surrogate internal standard area (Diphenylamine). The samples were concentrated by extraction with organic solvents (acetone) by Solid-Liquid Extraction (SLE) procedures the recovery factors being better than 80% except for Heptachlors. The coefficient of correlation of detector response function was better than 0.913 and LOQ under 0.015 μg/g. The method enables to determine pesticides at low μg/g in food supplements.

  6. Miniature GC: Minicell ion mobility spectrometer (IMS) for astrobiology planetary missions

    Science.gov (United States)

    Kojiro, Daniel R.; Holland, Paul M.; Stimac, Robert M.; Kaye, William J.; Takeuchi, Norishige

    2006-01-01

    Astrobiology flight experiments require highly sensitive instrumentation for in situ analysis of volatile chemical species and minerals present in the atmospheres and surfaces of planets, moons, and asteroids. The complex mixtures encountered place a heavy burden on the analytical instrumentation to detect and identify all species present. The use of land rovers and balloon aero-rovers place additional emphasis on miniaturization of the analytical instrumentation. In addition, smaller instruments, using tiny amounts of consumables, allow the use of more instrumentation and/or longer mission life for stationary landers/laboratories. We describe here the development of a miniature GC - Minicell Ion Mobility Spectrometer (IMS) under development through NASA's Astrobiology Science and Technology Instrument Development (ASTID) Program and NASA's Small Business Innovative Research (SBIR) Program.

  7. Development and validation of a method for detection and quantification of ochratoxin A in green coffee using liquid chromatography coupled to mass spectrometry Desenvolvimento e validação de metodologia na detecção e na quantificação de Ocratoxina A no café verde utilizando cromatografia líquida acoplada à espectrometria de massas

    Directory of Open Access Journals (Sweden)

    Raquel Duarte da Costa Cunha Bandeira

    2012-12-01

    Full Text Available A method using Liquid Chromatography Tanden Mass Spectrometry (LC-MS/MS with matrix-matched calibration curve was developed and validated for determining ochratoxin A (OTA in green coffee. Linearity was found between 3.0 and 23.0 ng.g-1. Mean recoveries ranged between 90.45% and 108.81%; the relative standard deviation under repeatability and intermediate precision conditions ranged from 5.39% to 9.94% and from 2.20% to 14.34%, respectively. The limits of detection and quantification were 1.2 ng.g-1 and 3.0 ng.g-¹, respectively. The method developed was suitable and contributed to the field of mycotoxin analysis, and it will be used for future production of the Certified Reference Material (CRM for OTA in coffee.Um método utilizando Cromatografia Líquida de Alta Eficiência-Espectrometria de Massas Sequencial (CLAE-EM/EM com curva de calibração em matriz foi desenvolvido e validado para a determinação de ocratoxina A (OTA em café verde. A linearidade foi demonstrada entre 3,0 e 23,0 ng.g-1. As recuperações médias variaram entre 90,45% e 108,81%; o desvio padrão relativo sob condições de repetitividade e precisão intermediária foram de 5,39% e 9,94% e de 2,20% e 14,34%, respectivamente. Os limites de detecção e quantificação foram 1,2 ng.g-1 e 3,0 ng.g-, respectivamente. O método desenvolvido foi adequado, contribuiu para o campo de análises em micotoxinas e será usado para a futura produção de Material de Referência Certificado (MRC para OTA em café.

  8. Determinação simultânea de teobromina, teofilina e cafeína em chás por cromatografia líquida de alta eficiência Simultaneous determination of theobromine, theophylline and caffeine in teas by high performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Adriana Barreto Alves

    2002-06-01

    Full Text Available Para a realização deste trabalho, foram analisadas 10 amostras de diferentes tipos e marcas de chás com o objetivo de se quantificar teobromina, teofilina e cafeína simultaneamente. Para tanto, otimizou-se técnica de cromatografia líquida de alta eficiência (CLAE baseada na ISO 10095 (1992, utilizando-se coluna Inertsil ODS-3 (150x4 mm, 5 mm, fase móvel de ácido acético 1% + acetonitrila (95:5, v/v, fluxo de 1 mL/min e detector de UV/VIS ajustado em 273 nm. Os resultados de cafeína obtidos por esse método foram comparados com os obtidos por um método espectrofotométrico de acordo com Schormüller (1970. Não houve diferença significativa nos resultados de cafeína nas amostras de chá preto obtidos pelos dois métodos. As amostras de chá preto foram as que apresentaram maiores teores de teobromina e cafeína e nenhuma das amostras apresentou quantidades significativas de teofilina.To carry out this study, 10 samples of different kinds and brands of teas were analyzed with the purpose of quantifying simultaneously theobromine, theophylline and caffeine. For this, high performance liquid chromatography (HPLC was used based on ISO 10095 (1992. The conditions were: a reversed phase column (Inertisil ODS-3, 150x4 mm, 5 mm; acetic acid 1% + acetonitrile (95:5, v/v as mobile phase; flow of 1 ml/min and UV-VIS detector set at 273 nm. The results of caffeine obtained by this method were compared with those using a spectrophotometric method according to Schormüller (1970. In the case of black tea, no difference was observed in the caffeine, by both methods. The samples of black tea had the highest amounts of theobromine and caffeine and no sample had a significant amount of theophylline.

  9. Determinação de taninos e metilxantinas no guaraná em pó (Paullinia cupana Kunth, Sapindaceae por cromatografia líquida de alta eficiência Determination of tannins and methylxanthines in powdered guarana (Paullinia cupana Kunth, Sapindaceae by high performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Sandra A. Sousa

    2010-12-01

    Full Text Available As sementes de guaraná (Paullinia cupana Kunth, Sapindaceae são utilizadas como estimulante e os principais constituintes químicos são as metilxantinas e os taninos, tais como catequina e epicatequina. Este trabalho teve por objetivo investigar um método por cromatografia líquida de alta eficiência (CLAE para quantificar, simultaneamente, cafeína, teofilina, teobromina, catequina e epicatequina em pó de guaraná. Os valores obtidos foram comparados com os resultados encontrados no método espectrofotométrico da Farmacopéia Brasileira IV ed. Pelo método cromatográfico, os teores de metilxantinas e taninos totais foram de 4,04% e 1,48%, respectivamente. Os teores de metilxantinas e taninos totais, obtidos pelo método espectrofotométrico, foram de 4,88% e 4,05%, respectivamente. Acredita-se que, nas condições experimentais empregadas, o método espectrofotométrico não foi específico, quantificando outras substâncias fenólicas presentes no guaraná. Portanto, sugere-se o emprego desse método cromatográfico no controle de qualidade do guaraná em pó, por ser preciso, sensível, específico e rápido.The seeds of Paullinia cupana Kunth, Sapindaceae, are used as a stimulant and the main chemical constituents are the methylxanthines and tannins, as catechin and epicatechin. This study aimed to investigate a method by high performance liquid chromatography (HPLC to quantify both caffeine, theophylline, theobromine, catechin and epicatechin in powdered of P. cupana. The values obtained were compared with the results of the spectrophotometric method of the Brazilian Pharmacopoeia IV ed. For the chromatographic method, the levels of methylxanthines and total tannins were 4.04% and 1.48%, respectively. The levels of methylxanthines and total tannins obtained by the spectrophotometric method, were 4.88% and 4.05%, respectively. It is believed that, under our experimental conditions, the spectrophotometric method was not specific and

  10. Desenvolvimento e aplicação de metodologia por cromatografia em camada delgada para determinação do perfil de alcalóides oxindólicos pentacíclicos nas espécies sul-americanas do gênero Uncaria

    Directory of Open Access Journals (Sweden)

    Ligia M.M. Valente

    Full Text Available O gênero Uncaria (Rubiaceae é representado na América do Sul e Central por duas espécies: U. tomentosa (Willd. DC. e U. guianensis (Aubl. Gmel., conhecidas popularmente como unha-de-gato. Ambas são trepadeiras perenes, sendo empregadas na prevenção e cura de várias doenças. Nessas plantas são encontrados alcalóides oxindólicos e indólicos, triterpenos glicosilados, taninos e flavonóides. Seis alcalóides oxindólicos pentacíclicos, considerados seus marcadores: especiofilina, mitrafilina, uncarina F, isomitrafilina, pteropodina e isopteropodina, são usados na padronização do material vegetal e fitoterápicos derivados. O presente trabalho descreve o desenvolvimento de metodologia analítica qualitativa utilizando cromatografia em camada delgada (CCD para determinação do perfil dos seis alcalóides oxindólicos pentacíclicos marcadores das espécies. O desenvolvimento do método incluiu a comparação entre o uso do extrato metanólico bruto, e de frações enriquecidas obtidas por partição ácido-base clássica ou pelo uso de resina básica Poliamida 6. Utilizou-se gel de sílica como fase estacionária, e variaram-se alguns parâmetros como: eluentes, concentração da amostra, espaço de eluição e tipos de reveladores. O método desenvolvido em CCD mostrou-se confiável, reprodutível e seletivo para os alcalóides alvos, sendo aplicado na análise de amostras de folhas e caule das duas espécies e também de fitoterápicos comerciais à base de U. tomentosa.

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

    KAUST Repository

    Chen, Yin

    2015-11-02

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

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

    KAUST Repository

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

    2015-01-01

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

  13. Variable stars in the VVV globular clusters. I. 2MASS-GC 02 and Terzan 10

    Energy Technology Data Exchange (ETDEWEB)

    Alonso-García, Javier; Dékány, István; Catelan, Márcio; Ramos, Rodrigo Contreras; Gran, Felipe; Leyton, Paul; Minniti, Dante [Instituto de Astrofísica, Facultad de Física, Pontificia Universidad Católica de Chile, Av. Vicuña Mackenna 4860, 782-0436 Macul, Santiago (Chile); Amigo, Pía, E-mail: jalonso@astro.puc.cl, E-mail: idekany@astro.puc.cl, E-mail: mcatelan@astro.puc.cl, E-mail: rcontrer@astro.puc.cl, E-mail: fgran@astro.puc.cl, E-mail: pia.amigo@uv.cl, E-mail: pleyton@astro.puc.cl, E-mail: dante@astrofisica.cl [Millennium Institute of Astrophysics, Av. Vicuña Mackenna 4860, 782-0436 Macul, Santiago (Chile)

    2015-03-01

    The VISTA Variables in the Vía Láctea (VVV) ESO Public Survey is opening a new window to study inner Galactic globular clusters (GCs) using their variable stars. These GCs have been neglected in the past due to the difficulties caused by the presence of elevated extinction and high field stellar densities in their lines of sight. However, the discovery and study of any present variables in these clusters, especially RR Lyrae stars, can help to greatly improve the accuracy of their physical parameters. It can also help to shed some light on the questions raised by the intriguing Oosterhoff dichotomy in the Galactic GC system. In a series of papers we plan to explore variable stars in the GCs falling inside the field of the VVV survey. In this first paper, we search for and study the variables present in two highly reddened, moderately metal-poor, faint, inner Galactic GCs: 2MASS-GC 02 and Terzan 10. We report the discovery of sizable populations of RR Lyrae stars in both GCs. We use near-infrared period–luminosity relations to determine the color excess of each RR Lyrae star, from which we obtain both accurate distances to the GCs and the ratios of the selective-to-total extinction in their directions. We find the extinction toward both clusters to be elevated, non-standard, and highly differential. We also find both clusters to be closer to the Galactic center than previously thought, with Terzan 10 being on the far side of the Galactic bulge. Finally, we discuss their Oosterhoff properties, and conclude that both clusters stand out from the dichotomy followed by most Galactic GCs.

  14. Quantification of Polyfunctional Thiols in Wine by HS-SPME-GC-MS Following Extractive Alkylation

    Directory of Open Access Journals (Sweden)

    Lauren E. Musumeci

    2015-07-01

    Full Text Available Analyses of key odorous polyfunctional volatile thiols in wines (3-mercaptohexanol (3-MH, 3-mercaptohexylacetate (3-MHA, and 4-mercapto-4-methyl-2-pentanone (4-MMP are challenging due to their high reactivity and ultra-trace concentrations, especially when using conventional gas-chromatography electron impact mass spectrometry (GC-EI-MS. We describe a method in which thiols are converted to pentafluorobenzyl (PFB derivatives by extractive alkylation and the organic layer is evaporated prior to headspace solid phase microextraction (HS-SPME and GC-EI-MS analysis. Optimal parameters were determined by response surface area modeling. The addition of NaCl solution to the dried SPME vials prior to extraction resulted in up to less than fivefold improvement in detection limits. Using 40 mL wine samples, limits of detection for 4-MMP, 3-MH, and 3-MHA were 0.9 ng/L, 1 ng/L, and 17 ng/L, respectively. Good recovery (90%–109% and precision (5%–11% RSD were achieved in wine matrices. The new method was used to survey polyfunctional thiol concentrations in 61 commercial California and New York State wines produced from V. vinifera (Riesling, Gewürztraminer, Cabernet Sauvignon, Sauvignon blanc and non-varietal rosé wines, V. labruscana (Niagara, and Vitis spp. (Cayuga White. Mean 4-MMP concentrations in New York Niagara (17 ng/L were not significantly different from concentrations in Sauvignon blanc, but were significantly higher than 4-MMP in other varietal wines.

  15. GC-MS analysis of clove (Syzygium aromaticum) bud essential oil from Java and Manado

    Science.gov (United States)

    Amelia, B.; Saepudin, E.; Cahyana, A. H.; Rahayu, D. U.; Sulistyoningrum, A. S.; Haib, J.

    2017-07-01

    The largest clove production contributors in Indonesia are mostly coming from Java and Manado. Different flavor among clove origins is caused by chemical constituents in clove oil. Unfortunately, scientific research and publications about flavor in clove from Indonesia's origin are still limited. The objective of this research is to determine significant differences of constituents in terms of flavor in clove oil originated from Java and Manado. The essential oils were isolated from cut clove bud samples by steam distillation method. The chemical constituents of clove bud oil were analyzed by using gas chromatography-mass spectrometry (GC-MS). Constituents were then identified by comparing the results of the chromatogram and reference retention time using Wiley mass spectra library (Wiley W9N11). Thirty-six and thirty-four chemical constituents were identified based on GC-MS from clove oil collected from Java and Manado, respectively. Major classes of compounds are sesquiterpenes, phenyl propanoid, oxygenated sesquiterpenes, and esters. Different compositions in major constituents were found between both origins. Clove Java contained eugenol (55.60 %), eugenyl acetate (20.54 %), caryophyllene (14.84 %), and α-humulene (2.75 %). While, in clove Manado, the composition were eugenol (74.64 %), caryophyllene (12.79 %), eugenyl acetate (8.70 %), and α-humulene (1.53 %). Moreover, minor constituents β-elemene (0.04 %), α-cadinene (0.05 %) and ledol (0.06 %) were existed only in clove Java, while clove Manado had some unique minor constituents which were not found in clove Java, i.e. β-gurjunene (0.04 %), γ-cadinene %), and humulene oxide (0.05 %). In conclusion, both clove oils from Java and Manado contained same major chemical constituents but different in their composition. In addition, some minor constituents existed only in specific origin.

  16. Analysis of iodine content in seaweed by GC-ECD and estimation of iodine intake

    Directory of Open Access Journals (Sweden)

    Tai Sheng Yeh

    2014-06-01

    Full Text Available Edible seaweed products have been consumed in many Asian countries. Edible seaweeds accumulate iodine from seawater, and are therefore a good dietary source of iodine. An adequate consumption of seaweed can eliminate iodine deficiency disorders, but excessive iodine intake is not good for health. The recommended dietary reference intake of 0.15 mg/d and 0.14 mg/d for iodine has been established in the United States and Taiwan, respectively. In this study, 30 samples of seaweed were surveyed for iodine content. The samples included 10 nori (Porphyra, 10 wakame (Undaria, and 10 kombu (Laminaria products. The iodine in seaweed was derivatized with 3-pentanone and detected by gas chromatography-electron capture detector (GC-ECD. The method detection limit was 0.5 mg/kg. The iodine content surveyed for nori was 29.3–45.8 mg/kg, for wakame 93.9–185.1 mg/kg, and for kombu 241–4921 mg/kg. Kombu has the highest average iodine content 2523.5 mg/kg, followed by wakame (139.7 mg/kg and nori (36.9 mg/kg. The GC-ECD method developed in this study is a low-cost alternative to inductively coupled plasma-optical emission spectroscopy for iodine detection in seaweeds. The iodine intake from seaweed in the current survey was calculated and compared with the iodine dietary reference intake of Taiwan. The risk and benefit of seaweed consumption is also discussed.

  17. Fully Automated Trimethylsilyl (TMS) Derivatisation Protocol for Metabolite Profiling by GC-MS.

    Science.gov (United States)

    Zarate, Erica; Boyle, Veronica; Rupprecht, Udo; Green, Saras; Villas-Boas, Silas G; Baker, Philip; Pinu, Farhana R

    2016-12-29

    Gas Chromatography-Mass Spectrometry (GC-MS) has long been used for metabolite profiling of a wide range of biological samples. Many derivatisation protocols are already available and among these, trimethylsilyl (TMS) derivatisation is one of the most widely used in metabolomics. However, most TMS methods rely on off-line derivatisation prior to GC-MS analysis. In the case of manual off-line TMS derivatisation, the derivative created is unstable, so reduction in recoveries occurs over time. Thus, derivatisation is carried out in small batches. Here, we present a fully automated TMS derivatisation protocol using robotic autosamplers and we also evaluate a commercial software, Maestro available from Gerstel GmbH. Because of automation, there was no waiting time of derivatised samples on the autosamplers, thus reducing degradation of unstable metabolites. Moreover, this method allowed us to overlap samples and improved throughputs. We compared data obtained from both manual and automated TMS methods performed on three different matrices, including standard mix, wine, and plasma samples. The automated TMS method showed better reproducibility and higher peak intensity for most of the identified metabolites than the manual derivatisation method. We also validated the automated method using 114 quality control plasma samples. Additionally, we showed that this online method was highly reproducible for most of the metabolites detected and identified (RSD TMS method has been applied to analyse a large number of complex plasma samples. Furthermore, we found that this method was highly applicable for routine metabolite profiling (both targeted and untargeted) in any metabolomics laboratory.

  18. Fully Automated Trimethylsilyl (TMS Derivatisation Protocol for Metabolite Profiling by GC-MS

    Directory of Open Access Journals (Sweden)

    Erica Zarate

    2016-12-01

    Full Text Available Gas Chromatography-Mass Spectrometry (GC-MS has long been used for metabolite profiling of a wide range of biological samples. Many derivatisation protocols are already available and among these, trimethylsilyl (TMS derivatisation is one of the most widely used in metabolomics. However, most TMS methods rely on off-line derivatisation prior to GC-MS analysis. In the case of manual off-line TMS derivatisation, the derivative created is unstable, so reduction in recoveries occurs over time. Thus, derivatisation is carried out in small batches. Here, we present a fully automated TMS derivatisation protocol using robotic autosamplers and we also evaluate a commercial software, Maestro available from Gerstel GmbH. Because of automation, there was no waiting time of derivatised samples on the autosamplers, thus reducing degradation of unstable metabolites. Moreover, this method allowed us to overlap samples and improved throughputs. We compared data obtained from both manual and automated TMS methods performed on three different matrices, including standard mix, wine, and plasma samples. The automated TMS method showed better reproducibility and higher peak intensity for most of the identified metabolites than the manual derivatisation method. We also validated the automated method using 114 quality control plasma samples. Additionally, we showed that this online method was highly reproducible for most of the metabolites detected and identified (RSD < 20 and specifically achieved excellent results for sugars, sugar alcohols, and some organic acids. To the very best of our knowledge, this is the first time that the automated TMS method has been applied to analyse a large number of complex plasma samples. Furthermore, we found that this method was highly applicable for routine metabolite profiling (both targeted and untargeted in any metabolomics laboratory.

  19. Amplification of a GC-rich heterochromatin in the freshwater fish Leporinus desmotes (Characiformes, Anostomidae

    Directory of Open Access Journals (Sweden)

    Vladimir Pavan Margarido

    2000-09-01

    Full Text Available This is the first description of the karyotype of Leporinus desmotes. The diploid female number was 2n = 54 meta- and submetacentric chromosomes. The nucleolar organizing regions (NORs were studied by silver nitrate staining and rDNA fluorescence in situ hybridization (FISH and were found to be located in the telomeric region of the long arm of the 9th pair. C-banding revealed centromeric and telomeric heterochromatin segments in most chromosomes. Intercalar blocks of heterochromatin were observed in the long arm of six chromosome pairs. Besides a NOR-adjacent heterochromatin, all of the intercalar heterochromatic segments were brightly fluorescent by mithramycin staining. These data suggest that a unique amplification of a primordial GC-rich heterochromatin, probably NOR-associated, may have taken place in the karyotype diversification of this Leporinus species.Esta é a primeira descrição do cariótipo de Leporinus desmotes fêmea. O número diplóide encontrado foi 2n = 54 cromossomos meta- e submetacêntricos. As regiões organizadoras de nucléolos (NORs foram estudadas através da impregnação pela prata e por hibridização in situ com sondas de DNAr (FISH, e foram localizadas na região telomérica do braço longo do 9º par. Heterocromatinas centromérica e telomérica foram reveladas pelo bandamento C na maioria dos cromossomos. Adicionalmente, grande quantidade de heterocromatina intercalar ou subtelomérica foi também observada. Diferenciação composicional na maior parte da heterocromatina identificada em L. desmotes pode ser inferida através da coloração pela mitramicina, caracterizando um caso peculiar de amplificação de segmentos heterocromáticos ricos em bases GC neste grupo de peixes.

  20. California serogroup GC (G1) glycoprotein is the principal determinant of pH-dependent cell fusion and entry

    International Nuclear Information System (INIS)

    Plassmeyer, Matthew L.; Soldan, Samantha S.; Stachelek, Karen M.; Martin-Garcia, Julio; Gonzalez-Scarano, Francisco

    2005-01-01

    Members of the California serogroup of orthobunyaviruses, particularly La Crosse (LAC) and Tahyna (TAH) viruses, are significant human pathogens in areas where their mosquito vectors are endemic. Previous studies using wild-type LAC and TAH181/57, a highly neurovirulent strain with low neuroinvasiveness (Janssen, R., Gonzalez-Scarano, F., Nathanson, N., 1984. Mechanisms of bunyavirus virulence. Comparative pathogenesis of a virulent strain of La Crosse and an avirulent strain of Tahyna virus. Lab. Invest. 50 (4), 447-455), have demonstrated that the neuroinvasive phenotype maps to the M segment, the segment that encodes the two viral glycoproteins GN (G2) and GC (G1), as well as a non-structural protein NSm. To further define the role of GN and GC in fusion and entry, we prepared a panel of recombinant M segment constructs using LAC, TAH181/57, and V22F, a monoclonal-resistant variant of LAC with deficient fusion function. These M segment constructs were then tested in two surrogate assays for virus entry: a cell-to-cell fusion assay based on T7-luciferase expression, and a pseudotype transduction assay based on the incorporation of the bunyavirus glycoproteins on an MLV backbone. Both assays demonstrated that GC is the principal determinant of virus fusion and cell entry, and furthermore that the region delineated by amino acids 860-1442, corresponding to the membrane proximal two-thirds of GC, is key to these processes. These results, coupled with structural modeling suggesting homologies between the carboxy region of GC and Sindbis virus E1, suggest that the LAC GC functions as a type II fusion protein

  1. Quantitative analysis of replication-related mutation and selection pressures in bacterial chromosomes and plasmids using generalised GC skew index

    Directory of Open Access Journals (Sweden)

    Suzuki Haruo

    2009-12-01

    Full Text Available Abstract Background Due to their bi-directional replication machinery starting from a single finite origin, bacterial genomes show characteristic nucleotide compositional bias between the two replichores, which can be visualised through GC skew or (C-G/(C+G. Although this polarisation is used for computational prediction of replication origins in many bacterial genomes, the degree of GC skew visibility varies widely among different species, necessitating a quantitative measurement of GC skew strength in order to provide confidence measures for GC skew-based predictions of replication origins. Results Here we discuss a quantitative index for the measurement of GC skew strength, named the generalised GC skew index (gGCSI, which is applicable to genomes of any length, including bacterial chromosomes and plasmids. We demonstrate that gGCSI is independent of the window size and can thus be used to compare genomes with different sizes, such as bacterial chromosomes and plasmids. It can suggest the existence of different replication mechanisms in archaea and of rolling-circle replication in plasmids. Correlation of gGCSI values between plasmids and their corresponding host chromosomes suggests that within the same strain, these replicons have reproduced using the same replication machinery and thus exhibit similar strengths of replication strand skew. Conclusions gGCSI can be applied to genomes of any length and thus allows comparative study of replication-related mutation and selection pressures in genomes of different lengths such as bacterial chromosomes and plasmids. Using gGCSI, we showed that replication-related mutation or selection pressure is similar for replicons with similar machinery.

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

    Science.gov (United States)

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

    2012-01-01

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

  3. Modified Method for Detection of Benzoylecgonine in Human Urine by GC-MS: Derivatization Using Pentafluoropropanol/Acetic Anhydride.

    Science.gov (United States)

    Serafin, Michelle C; Paulemon, Kasandra M; Fuller, Zachary J; Bronner, William E

    2017-05-01

    An existing GC-MS method for detecting benzoylecgonine (BZE) in urine was modified by changing derivatizing reagents. This method modification presents a cost-effective alternative derivatization procedure for the detection of BZE in urine by GC-MS. The combination of pentafluoropropanol and acetic anhydride was found to produce the same reaction product for BZE as pentafluoropropanol with pentafluoropropionic anhydride, while reducing reagent cost. With no anhydride present, derivatization of BZE by pentafluoropropanol did not occur. Published by Oxford University Press 2017. This work is written by (a) US Government employee(s) and is in the public domain in the US.

  4. Methods in the use of GC/C/IRMS for the analysis of biochemical and pollutant isotope signatures of compounds

    International Nuclear Information System (INIS)

    Macko, S.A.; Engel, M.H.

    2001-01-01

    The potential for application of GC/C/IRMS analysis to any multitude of environmental, ecological or biochemical research areas is only beginning to be realized. Extension of compound-specific isotope analytical data derived from modern organisms and settings to yield interpretations of ancient depositional environments certainly appears possible. Further application of GC/C/IRMS approaches to understand the cycling of carbon and nitrogen, the identification and alteration of pollutants, or resolve metabolic relationships between compounds in living or extinct organisms are all within the scope of future research. (author)

  5. GC-MS analysis, evaluation of phytochemicals, anti-oxidant, thrombolytic and anti-inflammatory activities of Exacum bicolor

    OpenAIRE

    Appaji Mahesh Ashwini; Latha Puttarudrappa; Belagumba Vijaykumar Ravi; Mala Majumdar

    2015-01-01

    The aim of the present study was to investigate the GC-MS analysis, phytochemical screening, anti-oxidant, thrombolytic and anti-inflammatory activities of methanol extract of leaves of Exacum bicolor. FTIR analysis confirmed the presence of alcohol, phenols, alkanes, aromatic compounds, aldehyde and ethers. GC-MS analysis revealed the presence of eight phyto-constituents. The total phenol, flavonoid and alkaloid contents were 18.0 ± 0.2 mg/GAE/g, 13.1 ± 0.4 mg QE/g and 108.0 ± 1.2 mg AE/g re...

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

    Science.gov (United States)

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

    2016-01-01

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

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

    Directory of Open Access Journals (Sweden)

    SELOUA ELMRABEH

    2015-05-01

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

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

    Science.gov (United States)

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

    2014-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Maria Letícia M. Valle

    2004-03-01

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

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

    Directory of Open Access Journals (Sweden)

    Edmilson Cezar Paglia

    2008-08-01

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

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

    Science.gov (United States)

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

    2015-10-01

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

  12. ThP05 Biogeneration of Volatile Selenium Compounds in Biosolids/Biofuels and Quantification by VD/GC/ICPMS

    Science.gov (United States)

    A noval analytical approach that uses VD/GC/ICPMS for the on-line extraction and quantificationof volatile organopmetalloids is described. Several species of arsenic, selenium, antimony, bismuth and tellurium are amenable to this technique. Preliminary results of a study on the...

  13. GC-O, volatile and qualitative differences in locally grown rabbiteye and southern highbush blueberries, and juices

    Science.gov (United States)

    Southern and southeastern US production of blueberries has increased markedly in recent years. Gas chromatography-olfactometry (GC-O) and volatile and semi-volatile compounds are seldom reported in rabbiteye blueberry (RAB). Few comparisons have been made between the organoleptic differences betwe...

  14. Supramolecular Switches Based on the Guanine–Cytosine (GC) Watson–Crick Pair: Effect of Neutral and Ionic Substituents

    NARCIS (Netherlands)

    Guerra, C.F.; van der Wijst, T.; Bickelhaupt, F.M.

    2006-01-01

    We have theoretically analyzed Watson–Crick guanine–cytosine (GC) base pairs in which purine-C8 and/or pyrimidine-C6 positions carry a substituent X = NH−, NH2, NH3+ (N series), O−, OH, or OH2+ (O series), using the generalized gradient approximation (GGA) of density functional theory at the

  15. A novel mitochondrial mutation m.8989G>C associated with neuropathy, ataxia, retinitis pigmentosa - the NARP syndrome

    DEFF Research Database (Denmark)

    Duno, Morten; Wibrand, Flemming; Baggesen, Kirsten

    2013-01-01

    mitochondrial point mutation, m.8989G>C, in a patient presenting with neuropathy, ataxia and retinitis pigmentosa constituting the classical NARP phenotype. This mutation alters the amino acid right next to canonical NARP mutation. We suggest that classic NARP syndrome relates to a defined dysfunction of p...

  16. Bromination of Aromatic Compounds by Residual Bromide in Sodium Chloride Matrix Modifier Salt During Heated Headspace GC/MS Analysis

    Science.gov (United States)

    Analytical artifacts attributed to the bromination of toluene, xylenes, and trimethylbenzenes were found during the heated headspace gas chromatography/mass spectrometry (GC/MS) analysis of aqueous samples. The aqueous samples were produced from Fenton-like chemical oxidation rea...

  17. Improved Separation of Complex Polycyclic Aromatic Hydrocarbon Mixtures Using Novel Column Combinations in GC×GC/ToF-MS

    Science.gov (United States)

    Manzano, Carlos; Hoh, Eunha; Simonich, Staci L. Massey

    2012-01-01

    Complex mixtures of polycyclic aromatic hydrocarbons (PAHs) are difficult to resolve because of the high degree of overlap in compound vapor pressures, boiling points and mass spectral fragmentation patterns. The objective of this research was to improve the separation of complex PAH mixtures (including 97 different parent, alkyl-, nitro-, oxy-, thio-, chloro-, bromo-, and high molecular weight PAHs) using GC×GC/ToF-MS by maximizing the orthogonality of different GC column combinations and improving the separation of PAHs from the sample matrix interferences, including unresolved complex mixtures (UCM). Four different combinations of non-polar, polar, liquid crystal and nano-stationary phase columns were tested. Each column combination was optimized and evaluated for orthogonality using a method based on conditional entropy that considers the quantitative peak distribution in the entire two-dimensional space. Finally, an atmospheric particulate matter with diameter column in the first dimension and a 1.2 m × 0.10 mm × 0.10 µm NSP-35 nano-stationary phase column in the second dimension. In addition, the use of this column combination in GC×GC/ToF-MS resulted in significantly shorter analysis times (176 min) for complex PAH mixtures compared to one-dimensional GC/MS (257 min), as well as potentially reduced sample preparation time. PMID:22769970

  18. Determination of Glyphosate Levels in Breast Milk Samples from Germany by LC-MS/MS and GC-MS/MS

    NARCIS (Netherlands)

    Steinborn, Angelika; Alder, Lutz; Michalski, Britta; Zomer, Paul; Bendig, Paul; Martinez, Sandra Aleson; Mol, Hans G.J.; Class, Thomas J.; Costa Pinheiro, Nathalie

    2016-01-01

    This study describes the validation and application of two independent analytical methods for the determination of glyphosate in breast milk. They are based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) and gas chromatography-tandem mass spectrometry (GC-MS/MS), respectively. For

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

    Science.gov (United States)

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

    2017-01-01

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

  20. Comparison of the volatile profiles of the crumb of gluten-free breads by DHE-GC/MS

    DEFF Research Database (Denmark)

    Pico, Joana; Hansen, Åse Solvej; Petersen, Mikael Agerlin

    2017-01-01

    starch, respectively, were evaluated. Wheat bread was used as a reference and dynamic headspace extraction together with GC/MS was employed. It was found that the whole grain breads, made with teff, quinoa and amaranth flours, presented a stronger aroma with higher number of important aroma contributors...

  1. Evaluation of modulators and electron-capture detectors for comprehensive two-dimensional GC of halogenated organic compounds

    NARCIS (Netherlands)

    Kristenson, E.M.; Korytar, P.; Danielsson, C.; Kallio, M.; Brandt, M.; Makela, J.; Vreuls, R.J.J.; Beens, J.; Brinkman, U.A.T.

    2003-01-01

    Different cryogenic and a heated GC×GC modulator(s) were evaluated and compared for the analysis of high-boiling halogenated compounds. The cryogenic modulators investigated were: (i) the longitudinally modulated cryogenic system; (ii) the liquid-nitrogen-cooled jet modulator (KT2001); (iii) a

  2. USE OF GC-MS/COMBUSTION/IRMS TO IDENTIFY AND DETERMINE THE STABLE CARBON ISOTOPIC RATIO OF INDIVIDUAL LIPIDS

    Science.gov (United States)

    A system that couples a gas chromatograph (GC) via a split to a quadrapole mass spectrometer (MS) and, through a combustion interface, to an isotope ratio mass spectrometer (IRMS) allows the simultaneous detection of electron impact mass spectra and stable carbon isotope ratio an...

  3. Modeling gas solubilities in imidazolium based ionic liquids with the [Tf2N] anion using the GC-EoS

    NARCIS (Netherlands)

    Pereda, Selva; Raeissi, Sonia; Andreatta, A.E. (Alfonsina); Bottini, Susana B.; Kroon, Maaike; Peters, Cor

    2016-01-01

    The group contribution equation of state (GC-EoS) is extended to model gas solubilities in the homologous 1-alkyl-3-methylimidazolium bis(trifluoromethyl-sulfonyl) imide family. The gases considered in this work are CO2, CO, H2, CH4, and C2H6. The model parameters were estimated on the basis of 1400

  4. 13 CFR 134.707 - When does the D/GC transmit the protest file and to whom?

    Science.gov (United States)

    2010-01-01

    ... Appeals From Women-Owned Small Business Concern (WOSB) and Economically Disadvantaged WOSB Concern (EDWOSB... 13 Business Credit and Assistance 1 2010-01-01 2010-01-01 false When does the D/GC transmit the protest file and to whom? 134.707 Section 134.707 Business Credit and Assistance SMALL BUSINESS...

  5. Using Py-GC/MS to detect and measure silicone defoamers in pulp fibres and mill deposits

    CSIR Research Space (South Africa)

    Sithole, Bruce

    2013-09-01

    Full Text Available in deposits. In this work, for the first time, Py-GC/MS has been used to analyse for silicone defoamers in pulp and paper matrices. This work demonstrates that the technique is ideal for analysis and characterisation of silicone defoamers on pulp fibres...

  6. Measurement of imidacloprid in xylem fluid from eastern hemlock (Tsuga canadensis) by derivitization/GC/MS and ELISA

    Science.gov (United States)

    Anthony Lagalante; Peter Greenbacker; Jonathan Jones; Richard Turcotte; Bradley Onken

    2007-01-01

    Imidacloprid is a nonvolatile insecticide and its direct quantification is not possible by gas chromatography. In order to ascertain imidacloprid levels in soil and trunk injection treated trees, a sensitive and selective method has been developed using GC/MS to measure the imidacloprid levels in xylem fluid exudates. In May 2005, a stand of hemlock trees in West...

  7. Soil organic matter chemistry changes upon secondary succession in Imperata Grasslands , Indonesia: A pyrolysis - GC/MS study

    NARCIS (Netherlands)

    Yassir, I.; Buurman, P.

    2012-01-01

    The chemical composition of soil organic matter (SOM) following secondary succession in Imperata grassland was investigated by Pyrolysis-Gas Chromatography/Mass Spectrometry (GC/MS). We studied 46 samples from different stages of succession using plots that last burned 3 and 9 years previously,

  8. Solid phase microextraction headspace sampling of chemical warfare agent contaminated samples : method development for GC-MS analysis

    Energy Technology Data Exchange (ETDEWEB)

    Jackson Lepage, C.R.; Hancock, J.R. [Defence Research and Development Canada, Medicine Hat, AB (Canada); Wyatt, H.D.M. [Regina Univ., SK (Canada)

    2004-07-01

    Defence R and D Canada-Suffield (DRDC-Suffield) is responsible for analyzing samples that are suspected to contain chemical warfare agents, either collected by the Canadian Forces or by first-responders in the event of a terrorist attack in Canada. The analytical techniques used to identify the composition of the samples include gas chromatography-mass spectrometry (GC-MS), liquid chromatography-mass spectrometry (LC-MS), Fourier-transform infrared spectroscopy (FT-IR) and nuclear magnetic resonance spectroscopy. GC-MS and LC-MS generally require solvent extraction and reconcentration, thereby increasing sample handling. The authors examined analytical techniques which reduce or eliminate sample manipulation. In particular, this paper presented a screening method based on solid phase microextraction (SPME) headspace sampling and GC-MS analysis for chemical warfare agents such as mustard, sarin, soman, and cyclohexyl methylphosphonofluoridate in contaminated soil samples. SPME is a method which uses small adsorbent polymer coated silica fibers that trap vaporous or liquid analytes for GC or LC analysis. Collection efficiency can be increased by adjusting sampling time and temperature. This method was tested on two real-world samples, one from excavated chemical munitions and the second from a caustic decontamination mixture. 7 refs., 2 tabs., 3 figs.

  9. Trans-acting GC-rich non-coding RNA at var expression site modulates gene counting in malaria parasite.

    Science.gov (United States)

    Guizetti, Julien; Barcons-Simon, Anna; Scherf, Artur

    2016-11-16

    Monoallelic expression of the var multigene family enables immune evasion of the malaria parasite Plasmodium falciparum in its human host. At a given time only a single member of the 60-member var gene family is expressed at a discrete perinuclear region called the 'var expression site'. However, the mechanism of var gene counting remains ill-defined. We hypothesize that activation factors associating specifically with the expression site play a key role in this process. Here, we investigate the role of a GC-rich non-coding RNA (ncRNA) gene family composed of 15 highly homologous members. GC-rich genes are positioned adjacent to var genes in chromosome-central gene clusters but are absent near subtelomeric var genes. Fluorescence in situ hybridization demonstrates that GC-rich ncRNA localizes to the perinuclear expression site of central and subtelomeric var genes in trans. Importantly, overexpression of distinct GC-rich ncRNA members disrupts the gene counting process at the single cell level and results in activation of a specific subset of var genes in distinct clones. We identify the first trans-acting factor targeted to the elusive perinuclear var expression site and open up new avenues to investigate ncRNA function in antigenic variation of malaria and other protozoan pathogens. © The Author(s) 2016. Published by Oxford University Press on behalf of Nucleic Acids Research.

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

    Science.gov (United States)

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

    2017-07-01

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

  11. A GC/MS-based metabolomic approach for reliable diagnosis of phenylketonuria.

    Science.gov (United States)

    Xiong, Xiyue; Sheng, Xiaoqi; Liu, Dan; Zeng, Ting; Peng, Ying; Wang, Yichao

    2015-11-01

    Although the phenylalanine/tyrosine ratio in blood has been the gold standard for diagnosis of phenylketonuria (PKU), the disadvantages of invasive sample collection and false positive error limited the application of this discriminator in the diagnosis of PKU to some extent. The aim of this study was to develop a new standard with high sensitivity and specificity in a less invasive manner for diagnosing PKU. In this study, an improved oximation-silylation method together with GC/MS was utilized to obtain the urinary metabolomic information in 47 PKU patients compared with 47 non-PKU controls. Compared with conventional oximation-silylation methods, the present approach possesses the advantages of shorter reaction time and higher reaction efficiency at a considerably lower temperature, which is beneficial to the derivatization of some thermally unstable compounds, such as phenylpyruvic acid. Ninety-seven peaks in the chromatograms were identified as endogenous metabolites by the National Institute of Standards and Technology (NIST) mass spectra library, including amino acids, organic acids, carbohydrates, amides, and fatty acids. After normalization of data using creatinine as internal standard, 19 differentially expressed compounds with p values of <0.05 were selected by independent-sample t test for the separation of the PKU group and the control group. A principal component analysis (PCA) model constructed by these differentially expressed compounds showed that the PKU group can be discriminated from the control group. Receiver-operating characteristic (ROC) analysis with area under the curve (AUC), specificity, and sensitivity of each PKU marker obtained from these differentially expressed compounds was used to evaluate the possibility of using these markers for diagnosing PKU. The largest value of AUC (0.987) with high specificity (0.936) and sensitivity (1.000) was obtained by the ROC curve of phenylacetic acid at its cutoff value (17.244 mmol/mol creatinine

  12. δ18O analysis of individual carbohydrates - a new method for GC-pyrolysis-IRMS

    Science.gov (United States)

    Lehmann, Marco M.; Fischer, Maria; Zech, Michael; Siegwolf, Rolf T. W.; Saurer, Matthias

    2015-04-01

    Measuring the oxygen isotopic composition (δ18O) of various plant tissues is a widely used tool to investigate biochemical and physiological processes. While we have a good understanding about the hydrological cycle in plants with an evaporative enrichment in 18O in leaf water, we still lack knowledge about the biochemical link between the oxygen atoms in leaf water, leaf assimilates, and stem cellulose and associated isotope fractionations. Especially, the influence of different environmental factors on δ18O of individual carbohydrates (i.e. sugars) and thus on δ18O of cellulose is not fully resolved. A better understanding of these processes may improve climatic reconstructions of tree-ring studies about past environmental conditions. However, further progress in this topic is limited since a precise and reliable method to determine δ18O of individual sugars has not been available yet. With our new approach we attempt to overcome this issue by establishing a new methylation derivatization method suitable for GC-pyrolysis -IRMS. A methyl group (CH3) was thereby added to all hydroxyl groups of a sugar (e.g., glucose, fructose, and sucrose) during a catalyzed one-pot reaction overnight in acetonitrile with methyl iodide (CH3-I) and silver oxide, making them amenable for GC analysis. First results show a very good precision for δ18O of sucrose, but also δ18O of other high-abundant sugars such as glucose and fructose could be measured for the first time. We successfully analyzed a standard mix of all three sugars and determined various other carbohydrates not only related to plant sciences (e.g. mannitol, lactose), showing promising δ18O results. First tests with real plant samples were performed to make this method available for determining δ18O of individual carbohydrates of diverse plant tissues. In future, this new methylation derivatization method should allow us analyzing plant samples of different field sites and of lab experiments to investigate the

  13. Organization of GC/MS and LC/MS metabolomics data into chemical libraries

    Directory of Open Access Journals (Sweden)

    DeHaven Corey D

    2010-10-01

    Full Text Available Abstract Background Metabolomics experiments involve generating and comparing small molecule (metabolite profiles from complex mixture samples to identify those metabolites that are modulated in altered states (e.g., disease, drug treatment, toxin exposure. One non-targeted metabolomics approach attempts to identify and interrogate all small molecules in a sample using GC or LC separation followed by MS or MSn detection. Analysis of the resulting large, multifaceted data sets to rapidly and accurately identify the metabolites is a challenging task that relies on the availability of chemical libraries of metabolite spectral signatures. A method for analyzing spectrometry data to identify and Quantify Individual Components in a Sample, (QUICS, enables generation of chemical library entries from known standards and, importantly, from unknown metabolites present in experimental samples but without a corresponding library entry. This method accounts for all ions in a sample spectrum, performs library matches, and allows review of the data to quality check library entries. The QUICS method identifies ions related to any given metabolite by correlating ion data across the complete set of experimental samples, thus revealing subtle spectral trends that may not be evident when viewing individual samples and are likely to be indicative of the presence of one or more otherwise obscured metabolites. Results LC-MS/MS or GC-MS data from 33 liver samples were analyzed simultaneously which exploited the inherent biological diversity of the samples and the largely non-covariant chemical nature of the metabolites when viewed over multiple samples. Ions were partitioned by both retention time (RT and covariance which grouped ions from a single common underlying metabolite. This approach benefitted from using mass, time and intensity data in aggregate over the entire sample set to reject outliers and noise thereby producing higher quality chemical identities. The

  14. Towards minimizing measurement uncertainty in total petroleum hydrocarbon determination by GC-FID

    Energy Technology Data Exchange (ETDEWEB)

    Saari, E.

    2009-07-01

    Despite tightened environmental legislation, spillages of petroleum products remain a serious problem worldwide. The environmental impacts of these spillages are always severe and reliable methods for the identification and quantitative determination of petroleum hydrocarbons in environmental samples are therefore needed. Great improvements in the definition and analysis of total petroleum hydrocarbons (TPH) were finally introduced by international organizations for standardization in 2004. This brought some coherence to the determination and, nowadays, most laboratories seem to employ ISO/DIS 16703:2004, ISO 9377-2:2000 and CEN prEN 14039:2004:E draft international standards for analysing TPH in soil. The implementation of these methods, however, usually fails because the reliability of petroleum hydrocarbon determination has proved to be poor.This thesis describes the assessment of measurement uncertainty for TPH determination in soil. Chemometric methods were used to both estimate the main uncertainty sources and identify the most significant factors affecting these uncertainty sources. The method used for the determinations was based on gas chromatography utilizing flame ionization detection (GC-FID).Chemometric methodology applied in estimating measurement uncertainty for TPH determination showed that the measurement uncertainty is in actual fact dominated by the analytical uncertainty. Within the specific concentration range studied, the analytical uncertainty accounted for as much as 68-80% of the measurement uncertainty. The robustness of the analytical method used for petroleum hydrocarbon determination was then studied in more detail. A two-level Plackett-Burman design and a D-optimal design were utilized to assess the main analytical uncertainty sources of the sample treatment and GC determination procedures. It was also found that the matrix-induced systematic error may also significantly reduce the reliability of petroleum hydrocarbon determination

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

    Directory of Open Access Journals (Sweden)

    Paulo Tarso L. Botteon

    2008-06-01

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

  16. Role of the NO/sGC/PKG signaling pathway of hippocampal CA1 in morphine-induced reward memory.

    Science.gov (United States)

    Shen, Fang; Li, Yi-Jing; Shou, Xiao-Jing; Cui, Cai-Lian

    2012-09-01

    Evidence suggests that the nitric oxide (NO)/soluble guanylyl cyclase (sGC)/cGMP dependent protein kinase (PKG) signaling pathway plays a key role in memory processing, but the actual participation of this signaling cascade in the hippocampal CA1 during morphine-induced reward memory remains unknown. In this study, we investigated the role of the NO/sGC/PKG signaling pathway in the CA1 on morphine-induced reward memory using a conditioned place preference (CPP) paradigm. We found that rats receiving an intraperitoneal (i.p.) injection of 4mg/kg morphine exhibited CPP, whereas rats treated with only 0.2mg/kg morphine failed to produce CPP. Intra-CA1 injection of the neuronal NO synthase (nNOS) inhibitor 7-NI, the sGC inhibitor ODQ or the PKG inhibitor Rp-8-Br-PET-cGMPS had no effect on the acquisition of CPP by 4mg/kg morphine. Intra-CA1 injection of 7-NI blocked the consolidation of CPP induced by 4mg/kg morphine, and this amnesic effect of 7-NI was mimicked by ODQ and Rp-8-Br-PET-cGMPS. Intra-CA1 injection of the NOS substrate L-arg or the sGC activator YC-1 with an ineffective dose of morphine (0.2mg/kg, i.p.) elicited CPP. This response induced by L-arg or YC-1 was reversed by pre-microinjection of Rp-8-Br-PET-cGMPS in the CA1. These results indicated that the activation of the NO/sGC/PKG signaling pathway in the CA1 is necessary for the consolidation of morphine-related reward memory. Copyright © 2012 Elsevier Inc. All rights reserved.

  17. Photocatalytic reduction of CO2 into hydrocarbon solar fuels over g-C3N4-Pt nanocomposite photocatalysts.

    Science.gov (United States)

    Yu, Jiaguo; Wang, Ke; Xiao, Wei; Cheng, Bei

    2014-06-21

    Photocatalytic reduction of CO2 into renewable hydrocarbon fuels is an alternative way to develop reproducible energy, which is also a promising way to solve the problem of the greenhouse effect. In this work, graphitic carbon nitride (g-C3N4) was synthesized by directly heating thiourea at 550 °C and then a certain amount of Pt was deposited on it to form g-C3N4-Pt nanocomposites used as catalysts for photocatalytic reduction of CO2 under simulated solar irradiation. The main products of photocatalysis were CH4, CH3OH and HCHO. The deposited Pt acted as an effective cocatalyst, which not only influenced the selectivity of the product generation, but also affected the activity of the reaction. The yield of CH4 first increased upon increasing the amount of Pt deposited on the g-C3N4 from 0 to 1 wt%, then decreased at 2 wt% Pt loading. The production rates of CH3OH and HCHO also increased with the content of Pt increasing from 0 to 0.75 wt% and the maximum yield was observed at 0.75 wt%. The Pt nanoparticles (NPs) could facilitate the transfer and enrichment of photogenerated electrons from g-C3N4 to its surface for photocatalytic reduction of CO2. At the same time, Pt was also used a catalyst to promote the oxidation of products. The transient photocurrent response further confirmed the proposed photocatalytic reduction mechanism of CO2. This work indicates that the deposition of Pt is a good strategy to improve the photoactivity and selectivity of g-C3N4 for CO2 reduction.

  18. Urinary amino acid analysis: a comparison of iTRAQ-LC-MS/MS, GC-MS, and amino acid analyzer.

    Science.gov (United States)

    Kaspar, Hannelore; Dettmer, Katja; Chan, Queenie; Daniels, Scott; Nimkar, Subodh; Daviglus, Martha L; Stamler, Jeremiah; Elliott, Paul; Oefner, Peter J

    2009-07-01

    Urinary amino acid analysis is typically done by cation-exchange chromatography followed by post-column derivatization with ninhydrin and UV detection. This method lacks throughput and specificity. Two recently introduced stable isotope ratio mass spectrometric methods promise to overcome those shortcomings. Using two blinded sets of urine replicates and a certified amino acid standard, we compared the precision and accuracy of gas chromatography/mass spectrometry (GC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) of propyl chloroformate and iTRAQ derivatized amino acids, respectively, to conventional amino acid analysis. The GC-MS method builds on the direct derivatization of amino acids in diluted urine with propyl chloroformate, GC separation and mass spectrometric quantification of derivatives using stable isotope labeled standards. The LC-MS/MS method requires prior urinary protein precipitation followed by labeling of urinary and standard amino acids with iTRAQ tags containing different cleavable reporter ions distinguishable by MS/MS fragmentation. Means and standard deviations of percent technical error (%TE) computed for 20 amino acids determined by amino acid analyzer, GC-MS, and iTRAQ-LC-MS/MS analyses of 33 duplicate and triplicate urine specimens were 7.27+/-5.22, 21.18+/-10.94, and 18.34+/-14.67, respectively. Corresponding values for 13 amino acids determined in a second batch of 144 urine specimens measured in duplicate or triplicate were 8.39+/-5.35, 6.23+/-3.84, and 35.37+/-29.42. Both GC-MS and iTRAQ-LC-MS/MS are suited for high-throughput amino acid analysis, with the former offering at present higher reproducibility and completely automated sample pretreatment, while the latter covers more amino acids and related amines.

  19. Urinary Amino Acid Analysis: A Comparison of iTRAQ®-LC-MS/MS, GC-MS, and Amino Acid Analyzer

    Science.gov (United States)

    Kaspar, Hannelore; Dettmer, Katja; Chan, Queenie; Daniels, Scott; Nimkar, Subodh; Daviglus, Martha L.; Stamler, Jeremiah; Elliott, Paul; Oefner, Peter J.

    2009-01-01

    Urinary amino acid analysis is typically done by cation-exchange chromatography followed by post-column derivatization with ninhydrin and UV detection. This method lacks throughput and specificity. Two recently introduced stable isotope ratio mass spectrometric methods promise to overcome those shortcomings. Using two blinded sets of urine replicates and a certified amino acid standard, we compared the precision and accuracy of gas chromatography/mass spectrometry (GC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) of propyl chloroformate and iTRAQ® derivatized amino acids, respectively, to conventional amino acid analysis. The GC-MS method builds on the direct derivatization of amino acids in diluted urine with propyl chloroformate, GC separation and mass spectrometric quantification of derivatives using stable isotope labeled standards. The LC-MS/MS method requires prior urinary protein precipitation followed by labeling of urinary and standard amino acids with iTRAQ® tags containing different cleavable reporter ions distinguishable by MS/MS fragmentation. Means and standard deviations of percent technical error (%TE) computed for 20 amino acids determined by amino acid analyzer, GC-MS, and iTRAQ®-LC-MS/MS analyses of 33 duplicate and triplicate urine specimens were 7.27±5.22, 21.18±10.94, and 18.34±14.67, respectively. Corresponding values for 13 amino acids determined in a second batch of 144 urine specimens measured in duplicate or triplicate were 8.39±5.35, 6.23±3.84, and 35.37±29.42. Both GC-MS and iTRAQ®-LC-MS/MS are suited for high-throughput amino acid analysis, with the former offering at present higher reproducibility and completely automated sample pretreatment, while the latter covers more amino acids and related amines. PMID:19481989

  20. Estimation of Environment-Related Properties of Chemicals for Design of Sustainable Processes: Development of Group-Contribution+ (GC+) Property Models and Uncertainty Analysis

    Science.gov (United States)

    The aim of this work is to develop group-contribution+ (GC+) method (combined group-contribution (GC) method and atom connectivity index (CI) method) based property models to provide reliable estimations of environment-related properties of organic chemicals together with uncert...