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1.
Acta bioquím. clín. latinoam ; 54(1): 61-68, mar. 2020. graf, tab
Article in Spanish | LILACS | ID: biblio-1130580

ABSTRACT

El uso de bisfenol-A (BPA) a nivel de la industria global se ha venido incrementando en los ultimos anos, y fueron los mercados emergentes los impulsores de esta demanda creciente. Las aplicaciones de BPA en la industria de los alimentos y bebidas representan solo del 3 al 4% del consumo global de policarbonato, pero su uso esta siendo reexaminado debido a que se conocieron varios trabajos cientificos que indican la existencia de una relacion directa entre el BPA y los efectos adversos para la salud. La contaminacion de los alimentos y bebidas se produce por migracion del BPA desde los envases que los contienen (alimentos enlatados, vinos, etc.), y es la principal fuente de exposicion en el humano. Para evaluar dicha exposicion se desarrollo y valido un metodo analitico por cromatografia gaseosa acoplada a espectrometria de masa para la cuantificacion de BPA total en orina de mujeres embarazadas atendidas en el Hospital Italiano de Buenos Aires en el ano 2013, con un limite de cuantificacion de 2,0 ng/mL y un limite de deteccion de 0,8 ng/mL. De las 149 muestras de orina analizadas, el 66,4% fueron cuantificables, con la mediana de BPA total de 4,8 ng/mL (4,3 ng/mg de creatinina) y la media geometrica de 4,8 ng/mL (4,7 ng/mg de creatinina).


The use of bisphenol-A (BPA) at the level of the global industry has been increasing in recent years, with emerging markets being the drivers of this growing demand. BPA applications in the food and beverage industry represent only 3 to 4% of the global consumption of polycarbonate, but its use is being reexamined because several scientific works were reported indicating the existence of a direct relationship between BPA and adverse effects on health. The contamination of food and beverages is produced by the migration of BPA from the containers that hold them (canned foods, wines, etc.) and it is the main source of exposure in humans. To evaluate this exposure, an analytical method was developed by gas chromatography coupled to mass spectrometry for the quantification of total BPA in urine of pregnant women treated at the Hospital Italiano de Buenos Aires in 2013, with a limit of quantification of 2.0 ng/mL and of detection of 0.8 ng/mL. Of the 149 urine samples analyzed, 66.4% were quantifiable, with a median total BPA of 4.8 ng/mL (4.3 ng/mg creatinine) and a geometric mean of 4.8 ng/mL (4.7 ng/mg creatinine).


O uso de bisfenol-A (BPA) ao nivel da industria global foi aumentando nos ultimos anos, e foram os mercados emergentes que deram impulso a essa demanda crescente. As aplicacoes de BPA na industria de alimentos e bebidas representam apenas 3 a 4% do consumo global de policarbonato, mas seu uso esta sendo reexaminado visto que varios trabalhos cientificos indicando a existencia de uma relacao direta entre o BPA e os efeitos adversos na saude foram conhecidos. A contaminacao dos alimentos e bebidas e produzida pela migracao de BPA das embalagens que os contem (alimentos enlatados, vinhos, etc.) e e a principal fonte de exposicao em humanos. Para avaliar esta exposicao, foi desenvolvido e avaliado um metodo analitico por cromatografia gasosa acoplada a espectrometria de massas para a quantificacao do BPA total na urina de gestantes atendidas no Hospital Italiano de Buenos Aires em 2013, com um limite de quantificacao de 2,0 ng/mL e um limite de deteccao de 0,8 ng/mL. Das 149 amostras de urina analisadas, 66,4% foram quantificaveis, com uma mediana de BPA total de 4,8 ng/mL (4,3 ng/mg de creatinina) e a media geometrica de 4,8 ng/mL (4,7 ng/mg de creatinina).


Subject(s)
Humans , Female , Pregnancy , Urine , Pregnancy/urine , Endocrine Disruptors , Gas Chromatography-Mass Spectrometry/methods , Mass Spectrometry/methods , Toxicology/statistics & numerical data , Food Industry , Health , Chromatography, Gas/methods , Food and Beverages , Pregnant Women , Drug-Related Side Effects and Adverse Reactions , Food
2.
Bol. latinoam. Caribe plantas med. aromát ; 18(5): 492-503, sept. 2019. tab, ilus
Article in English | LILACS | ID: biblio-1008286

ABSTRACT

The aim of the present work was to optimize the main experimental variables of a procedure using HS-SPME/GC-MS as the analytical methodology to establish the profile of the volatile compounds present in aerial parts of Hedeoma multiflorum Benth. The influence of the type of fiber, equilibrium time, extraction time and extraction temperature on the composition of the volatile compounds was determined using response surface methodology (RSM), and the parameters of the models were corroborated by multiple linear regressions. The results showed that the regression models generated adequately explained the data variation and represented the relationships between the parameters and their responses. The optimal analysis conditions from the contour plots were established (DVB/CAR/PDMS fiber, with a 10 min equilibrium time, 10 min extraction time, and 40°C). Under these conditions, 41 volatile components in the whole plant were determined, which represents more than those reported using hydrodistillation.


El objetivo del presente trabajo fue optimizar las principales variables experimentales de un procedimiento HS-SPME/GC para establecer el perfil de compuestos volátiles presentes en la parte aérea de Hedeoma multiflorum Benth. Se determinó la influencia de las variables tipo de fibra, tiempo de equilibrio, tiempo de extracción y temperatura de extracción sobre la composición de los volátiles, utilizando una met odología de superficie de respuesta (RSM) y los parámetros del modelo se corroboraron por regresión lineal múltiple. Los resultados demostraron que los modelos de regresión generados explican adecuadamente la variación de los datos y representaron significativamente las relaciones reales entre los parámetros y sus respuestas. Las condiciones óptimas de análisis fueron establecidas (DVB/CAR/PDMS, con un tiempo de equilibrio de 10 minutos, un tiempo de extracción de 10 minutos y trabajando a 40°C). Utilizando esta metodología, se determinaron 41 componentes volátiles en planta entera, más que los reportados mediante hidrodestilación.


Subject(s)
Hedeoma , Solid Phase Microextraction/methods , Volatile Organic Compounds/chemistry , Gas Chromatography-Mass Spectrometry/methods
3.
São Paulo; s.n; s.n; 2019. 50 p. ilus, graf, tab.
Thesis in Portuguese | LILACS | ID: biblio-1007412

ABSTRACT

O uso de óleos essenciais na indústria de fragrância tem crescido a cada ano. A indústria de cosméticos, em geral, tem buscado este tipo de ingrediente com o objetivo de agregar atributos únicos e melhores aos seus produtos e assim entregar, ao consumidor final, diferenciais que poderão valorizar suas formulações, além de simplesmente perfumar. O benefício de usar óleos naturais ou acordes de seus principais componentes em formulações de fragrâncias é que estes se tornam composições mais ricas, e em muitos casos, capazes de proporcionar perfumação prolongada ao produto, quando comparados àqueles sintetizados. A presença de compostos variados nos óleos, como terpenos e resinas, ajudam a promover singularidades à fragrância e até mesmo servem como inspiração às criações de produtos com descrições olfativas de produtos naturais. Croton tricolor (Euphorbiaceae), segundo avaliação inicial de um perfumista, apresentou excelentes características olfativas, o que facilitou seu uso nos estudos. A análise do óleo essencial de C. tricolor por cromatografia à gás com detector de ionização de chamas (CG/DIC) e cromatografia à gás acoplada à espectrometria de massas (CG/EM) permitiu quantificar e identificar seus principais marcadores, bem como utilizar estas informações para construção de acorde olfativo, reproduzindo o odor do produto natural. O óleo essencial de C. tricolor apresentou como principais componentes o biciclogermacreno (15,4%), espatulenol (10,5%) e o alfa-pineno (6,8%). A partir destes dados foi construído um acorde aromático que reproduziu o odor original, contendo alfa-pineno (7%), álcool fenetílico (5%), óleo de cedro (5%), óleo de laranja (0,5%), limoneno (1%), eucaliptol (0,5%) e nerolidol (0,3%). Os compostos majoritários, biciclogermacreno e espatulenol, não foram adicionados por não serem disponíveis comercialmente, por isso, usaram-se outras matérias-primas semelhantes em perfil olfativo e ofertadas no mercado, como foi o caso do uso de álcool fenetílico, óleo de cedro e óleo de laranja na criação do acorde. Os resultados evidenciaram que a criação de acordes é um método economicamente viável para a reprodução de odores naturais que podem ser utilizados em formulações de fragrâncias, além de ajudar a resolver problemas na produção e comercialização de óleos essenciais como, sazonalidade e reprodutibilidade


The use of essential oils in the fragrance industry has grown every year. The cosmetics industry has generally sought this type of ingredient, with the aim of providing its products with differentiated benefits (unique and better attributes), and thus delivering to the final consumer a differential that can enhance their formulations, besides simply perfuming their products (theirs). The benefit of using natural oils or accords of their major components in fragrance formulations makes them richer, and in many cases capable of providing prolonged perfuming to the final product when compared to synthesized products. The presence of varied compounds in the oils, such as terpenes or (and) resins, helps to promote differentiated fragrance characteristics (singularities/peculiarities to the fragrance), or (and) even to serve as inspiration for product creations with olfactory descriptions of natural products. Croton tricolor (Euphorbiaceae), accordingly to an initial evaluation of a perfumer, presented excellent olfactory characteristics, which facilitated its use in the studies. The analysis of the C. tricolor essential oil by gas chromatography with flame ionization detector (GC/FID) and gas chromatography coupled to mass spectrometry (GC/MS) allowed to quantify and identify their main markers, as well as to use this information to construct an olfactory accord that reproduces the odor of natural products. The C. tricolor essential oil had as main components bicyclogermacrene (15.4%), spathulenol (10.5%) and alpha pinene (6.8%). From these data, an aromatic accord was created reproducing the original odor containing alpha pinene (7%), phenethyl alcohol (5%), cedar oil (5%), orange oil (0.5%), limonene (1%), eucalyptol (0.5%) and nerolidol (0.3%). Some of the major compounds, bicyclogermacrene and spatulenol, could not be added because they were not commercially available. In these cases (therefore), other products (raw materials) with similar olfactory characteristics (olfactory profile) and commercially viable (offered on the market) were used, such as the use of phenethyl alcohol, cedar oil and orange oil in the accord creation. The results showed that accord creation is an economically viable method for the reproduction of natural odors that can be used in fragrance formulations and may help to solve problems that exist in the production and commercialization of essential oils such as production seasonality and reproducibility


Subject(s)
Perfume/chemistry , Oils, Volatile/analysis , Euphorbiaceae/anatomy & histology , Cosmetic Industry , Gas Chromatography-Mass Spectrometry/methods , Odorants
4.
São Paulo; s.n; s.n; 2019. 214 p. graf, tab.
Thesis in Portuguese | LILACS | ID: biblio-995689

ABSTRACT

Cloropropanóis são um grupo conhecido de contaminantes relacionados ao processamento de alimentos. Eles são formados na reação entre lipídeos e cloretos quando submetidos ao tratamento térmico, e podem ser encontrados na forma livre ou ligada. O 3-monocloro-1,2-propanediol (3-MCPD), é classificado pela IARC como possível carcinógeno humano (grupo 2B). O glicidol (e seus ésteres), é classificado também pela IARC como uma substância provavelmente carcinogênica para seres humanos (grupo 2A), e, recentemente, vem sendo encontrado em alimentos. O objetivo deste trabalho foi avaliar a presença do 3-MCPD e do glicidol em óleos vegetais comestíveis utilizando a cromatografia gasosa com detector de massa triplo quadrupolo MS/MS. A técnica utilizada foi a preconizada pela AOCS Cd 29c-13, sendo uma análise indireta, e foi possível adaptá-la visando as determinações do 3-MCPD e glicidol através da construção de curvas de calibração e análises de amostras de referência. O método foi validado e os resultados indicaram o limite de detecção do composto 3-MCPD, de 42,4 µg/kg e o limite de quantificação de 50 µg/kg, e para o Glicidol indicaram o limite de detecção de 43,5 µg/kg e limite de quantificação de 50 µg/kg. Os resultados para 3-MCPD obtidos nos ensaios da curva de calibração e linearidade demonstraram que o método foi capaz de expressar resultados com boa linearidade (0 - 10 mg/kg , r2, = 0.9991). Os resultados obtidos nos ensaios de exatidão obedeceram aos critérios de 70 a 120% de recuperação, e ±20% de variação entre os resultados de acordo com SANTE (2017). O método em questão demonstrou ser seletivo, uma vez que não foram observados picos interferentes nos tempos de retenção dos compostos estudados. Os ensaios de precisão nos níveis baixos, médio e alto e robustez demonstraram que o método é robusto e preciso, portanto a validação foi considerada adequada ao uso pretendido. Foram analisadas 368 amostras de óleos vegetais (76 amostras de óleo de canola, 48 amostras de óleo de milho, 69 amostras de óleo de algodão, 33 amostras de óleo de palma, 10 amostras de óleo de palmiste, 50 amostras de oleína de palma, 30 amostras de óleo de soja e 51 amostras de óleo de girassol). As concentrações das amostras analisadas apresentaram resultados para 3-MCPD com valores médios entre 203 a 1205 µg/kg. Para o Glicidol os valores foram de 2 a 1198 µg/kg, com elevado o desvio padrão entre os resultados analíticos, onde o óleo de palma apresentou a maior variação de 1600 a 5260 µg/kg. Através da avaliação do risco realizada para o composto 3-MCPD foi possível detectar, utilizando o critério do pior cenário de exposição e resultados analíticos, os valores diários de consumo de óleo de algodão de 0,044 µg/kg p.c., de óleo de girassol 0,045 µg/kg p.c., óleo de canola 0,18 µg/kg p.c., óleo de palma de 0,28 µg/p.c, óleo de milho de 0,0462 µg/kg p.c., e o óleo de soja, de maior consumo no Brasil (72%) apresentou o valor de 0,27 µg/kg p.c. O consumo de todos estes óleos, pela a população brasileira, pode ser considerado seguro ao comparar com o valor de TDI Ingestão Diária Tolerável - de 2µg/kg p.c.. Através da avaliação do risco realizada também utilizando o critério de pior cenário de exposição e e resultados analíticos para o composto glicidol foi possível verificar que os valores diários de consumo de óleo de algodão de 0,061 µg/kg p.c., de óleo de girassol 0,03 µg/kg p.c., óleo de canola 0,13 µg/kg p.c. e de óleo de palma de 0,57 µg/p.c, de óleo de milho de 0,11 µg/kg p.c, e o óleo de soja de maior consumo no Brasil (72%) não ultrapassam o valor de 0,288 µg/kg p.c indicando consumo seguro destes óleos para a população brasileira baseado na TDI de 1000µg/kg p.c


Chloropropanols are a known group of contaminants related to food processing. They are formed during the reaction process between lipids and chlorides when submitted to heat treatment and can be found in free or bound form. The 3-monochloro-1,2-propanediol (3-MCPD), is classified by IARC as a possible human carcinogen (group 2B). Glycidol (and its esters), also classified by IARC as a substance likely to be carcinogenic to humans (group 2A), has recently been found in food. The present study aims to evaluate the presence of 3-MCPD and glycidol in edible vegetable oils using gas chromatography with triple quadrupole MS/MS mass detector. The technique applied is recommended by AOCS, guide Cd 29c-13, an indirect analysis, and allows quantification of 3-MCPD and glycidol by building the calibration curves and analysis of reference samples. The method was validated and the detection limit of the contaminant 3-MCPD of 42,4 µg/kg and the quantification limit of 50 µg/kg was established. For Glycidol the detection limit of was 43,5 µg/kg and quantification limit was 50 µg/kg. The results obtained in the calibration and linearity curves demonstrated that the method could express results with good linearity (0 10 mg/kg, r2, = 0.9991). The results obtained in the trueness trials agreed to the criteria of 70 to 120% of recovery, and ± 20% of variation between the results according to what is preconized by SANTE (2017). The method showed to be selective, since no interfering peaks were observed in the retention times of the studied compounds. The tests performed on low, medium and high values demonstrated the robustness and precision of the method, so the validation was considered completed and suitable for the purpose. A total of 368 vegetable oil samples were analyzed (76 samples of canola oil, 48 samples of corn oil, 69 samples of cottonseed oil, 33 samples of palm oil, 10 samples of kern palm oil, 50 samples of palm olein, 30 samples of soybean oil and 51 samples of sunflower oil). The results found in samples for 3-MCPD were within mean values between 203 and 1205 µg/kg. The results found in samples for glycidol were within mean values between 2 to 1198 µg/kg where palm oil presented the highest variation for glycidol from 1600 to 5260 µg/kg. Through the risk assessment for the contaminant 3-MCPD it was possible to detect the values based on exposed worst case scenario and analytical results. The results for cottom oil were 0,044 µg/kg bw, sunflower 0,045 µg/kg bw, canola 0,18 µg/kg bw and palm oil 0,28 µg/kg bw, corn oil 0,0462 µg/kg bw, and for soybean, which is the most consumed oil in Brazil (72%) the value of 0,27 µg/kg bw. These results indicates safe consumption for these oils based in the Theoretical Daily Ingestion - TDI of 2µg/kg bw. The risk assessment for the glycidol based on exposure worst case scenario and analytical results presented for cottom oil the value of 0,061 µg/kg bw, sunflower 0,03 µg/kg bw, canola oil 0,13 µg/kg bw , palm oil 0,57 µg/kg bw, corn oil 0,11 µg/kg bw and for soybean, which is the most consumed in Brazil - 72% the value of 0,27 µg/kg bw. These results indicates safe consumption for these oils based in the TDI of 1000µg/kg bw


Subject(s)
Oils/analysis , alpha-Chlorohydrin/analysis , Mass Spectrometry/methods , Food Contamination/prevention & control , Risk Assessment , Gas Chromatography-Mass Spectrometry/methods
5.
Braz. J. Pharm. Sci. (Online) ; 54(1): e17151, 2018. tab, graf
Article in English | LILACS | ID: biblio-889444

ABSTRACT

ABSTRACT Our present investigation deals with the phytochemical screening, estimation of total flavonoids, terpenoids and tannin contents to evaluate the anti-diabetic activities of Salacia oblonga stem followed by GC-MS analysis. It explores the natural compounds and the potential α-amylase and α-glucosidase inhibitory actions of stem extracts. The aqueous stem extract was selected from other extracts (ethanol, acetone, petroleum ether and chloroform) for the in vitro study of anti-diabetic activity by alpha amylase and alpha glucosidase inhibitory assays. The stem extract was also analyzed by gas chromatography mass spectrometry to identify the natural chemical components. Phytochemical analysis of aqueous stem extract showed major classes of secondary metabolites such as phenols, flavonoids, alkaloids, terpenoids, tannins, saponins. The total flavonoid, terpenoid, and tannin contents were quantified as 19.82±0.06 mg QE/g, 96.2±0.20 mg/g and 11.25±0.03 mg TAE/g respectively. The percentage inhibition of assays showed maximum inhibitory effects (59.46±0.04% and 68.51±0.01%) at a concentration of 100 mg/mL. The IC50 values of stem extract was found to be 73.56 mg/mL and 80.90 mg/mL for alpha amylase and alpha glucosidase inhibition. Fifteen chemical constituents were found by GC-MS analysis. This study suggest the aqueous stem extract of Salacia oblonga might be considered as potential source of bio active constituents with excellent antidiabetic activity.


Subject(s)
Plant Stems , alpha-Amylases/analysis , alpha-Glucosidases/analysis , Plant Extracts/analysis , Analysis of Variance , Salacia/anatomy & histology , Hypoglycemic Agents , Gas Chromatography-Mass Spectrometry/methods
6.
São Paulo; s.n; s.n; 2018. 79 p. graf, ilus, tab.
Thesis in Portuguese | LILACS | ID: biblio-883230

ABSTRACT

O câncer primário de fígado (CPF) apresenta mau prognóstico, o que torna importante sua quimioprevenção. Nesse sentido, a tributirina (TB), um pró-fármaco do ácido butírico (AB), presente em laticínios e no mel, mostrou-se um agente quimiopreventivo promissor da hepatocarcinogênese experimental. Os efeitos inibitórios da TB têm sido relacionados à inibição do desenvolvimento de lesões pré-neoplásicas, bem como indução de apoptose e hiperacetilação de histonas. A quimioterapia é uma das abordagens mais comuns para o tratamento de diversos tipos de câncer, inclusive o CPF. Neste caso, o tratamento com sorafenibe (SO) é capaz de prolongar a sobrevida média dos pacientes com a doença em fases avançadas em aproximadamente apenas três meses. Em vista disso, são necessários estudos da associação do sorafenibe com outros compostos que possam aumentar a eficácia do tratamento quimioterápico. Desta forma, a associação de fármacos anti-neoplásicos com compostos bioativos dos alimentos pode consistir em uma estratégia potencial para aumentar a eficácia contra o câncer. No presente estudo, foi avaliada a atividade anticarcinogênica da TB e do SO, isoladamente ou em associação, na etapa de progressão da hepatocarcinogênese. Para tanto, foram realizados implantes singênicos no flanco de ratos Fischer-344 a partir de células da linhagem tumoral GP7TB. Quando as neoplasias atingiram 1 cm3, os animais foram aleatorizados em grupos experimentais: Grupo controle (CO), constituído por 10 ratos Fischer 344 que receberam Maltodextrina (300mg/ 100 g. p. c.), controle isocolarico e solução de etanol à 12,5% e Cremofor à 12,5% em agua estéril; Grupo Tributirina (TB), constituído por 9 ratos Fischer 344 que receberam TB (200mg/ 100 g. p. c.) e solução de etanol à 12,5% e Cremofor à 12,5% em água estéril; Grupo sorafenibe (SO) constituído por 9 ratos Fischer 344 que receberam Maltodextrina (300 mg/ 100 g. p. c.), controle isocalorico e tosilato de sorafenibe (3mg / 100 g. p. c. ) em água estéril; Grupo associação da tributirina com o sorafenibe (AS) constituído por 9 ratos Fischer 344 que receberam TB (20 mg/ 100 g. p. c.) e tosiliato de sorafenibe (3mg/ 100 g. p. c.); tratados por administração intragástrica (i.g) diariamente por 5 semanas consecutivas. As concentrações de AB e SO foram analisadas por cromatografia gasosa associada à espectrometria de massa e as neoplasias foram caracterizadas por imunoistoquímica. Em relação à evolução do tamanho das neoplasias o grupo AS apresentou menor (p=0,009) tamanho das mesmas em relação ao grupo CO. No entanto, estas diferenças não atingiram diferenças significativas (p>0,05) entre os grupos TB e CO, bem como entre os grupos SO e CO. Contudo, quando ajustados os valores do tamanho da neoplasia pela latência, observou-se alterações significativas (p<0,05) nos diversos grupos quando comparados ao grupo CO. O grupo SO aumentou a área necrótica das neoplasias, embora esta diferença não tenha atingido diferença significativa (p>0,05), enquanto que o grupo TB reduziu essa área necrótica em relação ao grupo CO (p=0,005). O grupo TB e AS apresentaram significativamente maiores (p<0,05) concentrações hepáticas e neoplásicas de AB em relação ao grupo CO. O grupo SO e AS apresentaram significativamente maiores (p<0,05) concentrações neoplásicas de SO em relação ao grupo CO. Os grupos SO e AS reduziram a expressão de PTEN, quando comparados ao grupo CO, embora esta diferença não tenha atingido diferença significativa (p>0,05). O grupo TB por sua vez expressou maiores niveis de PTEN, embora esta diferença não tenha atigindo significância estatística (p>0,05). Todos os grupos expressaram maiores niveis de caspase 3 clivada quando comparada ao grupo CO (p>0,05). OS grupos TB e SO reduziram a expressão de pERK ½ quando comparados ao grupo CO. embora estas diferenças não tenham atingidos diferença estatística (p>0,05). O grupo AS apresentou maior expressão de pERK ½ quando comparada ao grupo CO, embora esta diferença não tenha atingido diferença significativa (p>0,05). A caracterização das neoplasias do grupo CO foi padronizada por imunoistoquímica, apresentando-se positivas para CK 7, CK8, CK19 e Arginase e negativas para HepPar1 e CK18. Assim, os resultados sugerem que as neoplasias obtidas por implantes com células da linhagem GP7TB apresentam características de CPF oriundo de células tronco neoplásicas. Além disso, os grupos experimentais TB e AS apresentaram atividade anticarcinogênica promissora no modelo de implantes singênicos com células GP7TB, que eventualmente envolvem mecanismos de ação distintos da atividade quimioterápica apresentada pelo SO


Primary liver cancer (PLC) presents poor prognosis, which makes its chemoprevention important. In this sense, tributyrin (TB), a prodrug of butyric acid (AB), present in dairy products and honey, has been shown to be a promising chemopreventive agent for experimental hepatocarcinogenesis. The inhibitory effects of TB have been related to inhibition of the development of pre-neoplastic lesions, as well as induction of apoptosis and hyperacetylation of histones. Chemotherapy is one of the most common approaches for treating various types of cancer, including PLC. In this case, treatment with sorafenib (SO) is able to prolong the average survival of patients with the disease in advanced stages in approximately three months. In view of this, studies of the association of sorafenib with other compounds that may increase the efficacy of chemotherapeutic treatment are necessary. Thus, the association of anti-neoplastic drugs with bioactive compounds in food may be a potential strategy to increase efficacy against cancer. In the present study, the anticarcinogenic activity of TB and SO was evaluated, alone or in combination, in the progression stage of hepatocarcinogenesis. For this purpose, syngenic implants were performed on the flank of Fischer-344 mice from GP7TB tumor cells. When the neoplasms reached 1 cm3, the animals were randomized into experimental groups: Control group (CO), consisting of 10 Fischer 344 rats receiving Maltodextrin (300mg / 100 g.p.c), isocaloric control and 12.5% ethanol solution, and Cremofor to 12.5% in sterile water; Tributyrin group (TB), consisting of 9 Fischer 344 rats that received TB (200mg / 100 g.p.c.) and 12.5% ethanol solution and Cremofor 12.5% in sterile water; Sorafenib group (SO) consisting of 9 Fischer 344 rats receiving maltodextrin (300 mg / 100 g, w / w), isocaloric control and sorafenib tosylate (3 mg / 100 g, w / w) in sterile water; The association group of tributyrin and sorafenib (AS) consisted of 9 Fischer 344 rats receiving TB (20 mg / 100 g p.o.) and sorafenib tosylate (3 mg / 100 g p.o.); treated intragastric (i.g) daily for 5 consecutive weeks. The concentrations of AB and SO were analyzed by gas chromatography associated with mass spectrometry and the neoplasms were characterized by immunohistochemistry. In relation to the evolution of the size of the neoplasias, the AS group presented smaller (p = 0.009) size of the same ones in relation to the CO group. However, these differences did not reach significant differences (p> 0.05) between the TB and CO groups, as well as between the SO and CO groups. However, when adjusted for size of the neoplasm by latency, significant changes (p <0.05) were observed in the different groups when compared to the CO group. The SO group increased the necrotic area of the neoplasias, although this difference did not reach a significant difference (p> 0.05), while the TB group reduced this necrotic area in relation to the CO group (p = 0.005). The TB and AS groups presented significantly higher (p <0.05) hepatic and neoplastic AB concentrations than the CO group. The SO and AS groups presented significantly higher (p <0.05) neoplastic concentrations of SO in relation to the CO group. The SO and AS groups reduced the PTEN expression when compared to the CO group, although this difference did not reach a significant difference (p> 0.05). The TB group in turn expressed higher levels of PTEN, although this difference did not increase statistical significance (p> 0.05). All groups expressed higher levels of caspase 3 cleaved when compared to the CO group (p> 0.05). The TB and SO groups reduced the expression of pERK ½ when compared to the CO group. although these differences did not reach statistical difference (p> 0.05). The AS group presented higher pERK ½ expression when compared to the CO group, although this difference did not reach a significant difference (p> 0.05). Characterization of the neoplasias of the CO group was standardized by immunohistochemistry, presenting positive for CK 7, CK8, CK19 and Arginase and negative for HepPar1 and CK18. Thus, the results suggest that the neoplasias obtained by implants with GP7TB cells present CPF characteristics originating from neoplastic stem cells. In addition, the experimental groups TB and AS presented promising anticarcinogenic activity in the model of syngeneic implants with GP7TB cells, which eventually involve mechanisms of action distinct from the chemotherapy activity presented by SO


Subject(s)
Animals , Male , Rats , Anticarcinogenic Agents/analysis , Liver Neoplasms/prevention & control , Pharmaceutical Preparations/analysis , Blotting, Western/instrumentation , Butyric Acid/agonists , Carcinoma, Hepatocellular , Data Interpretation, Statistical , Gas Chromatography-Mass Spectrometry/methods , Immunohistochemistry/methods , Tumor Cells, Cultured/classification
7.
São Paulo; s.n; s.n; 2018. 107 p. graf, tab.
Thesis in Portuguese | LILACS | ID: biblio-885107

ABSTRACT

Estima-se atualmente que mais de 5% da população mundial vem fazendo uso recreativo de algum tipo de substância psicoativa, sendo que o direito a esse uso é tema recorrente da sociedade contemporânea. Por apresentar riscos associados à saúde e a segurança das populações, o uso abusivo dessas substâncias tem instigado a toxicologia social na busca de respostas, com as quais se possa caracterizar, analisar e gerenciar esses riscos. Drogas de grande consumo no Brasil são a anfetamina, cocaína e Cannabis sativa. Esta tese desenvolveu uma nova metodologia para detectar e quantificar anfetamina, cocaína e tetrahidrocanabinol em sangue total, com uso de microextração em fase líquida via fibra de polipropileno (HF-LPME), seguida de cromatografia gasosa acoplada a espectrometria de massa (GC-MS). Trata-se de uma técnica que apresenta vantagens sobre as tradicionais, uma vez que demanda quantidades menores de solvente orgânico, diminuindo riscos e custos de processo. Também propôs um estudo com a aplicação dos métodos em 69 amostras de sangue de vivos e de post mortem, as quais foram obtidas por convênio com a superintendência da polícia técnica científica de São Paulo (SPTC/SP). Os métodos desenvolvidos foram validados de acordo com diretrizes internacionais de interesse forense. Como resultado da validação, os métodos desenvolvidos se mostraram precisos e exatos para anfetamina e cocaína. O limite de detecção da cocaína foi de 5 ng . mL-1 e o limite de quantificação de 10 ng . mL-1. Quanto a anfetamina, os limites de detecção e de quantificação foram de 5 ng . mL-1. A técnica de HF-LPME não foi aplicável ao tetraidrocanabinol (Δ9-THC). Como resultado da análise das amostras, 40% delas apresentaram resultados positivos para cocaína. Desses positivos, 35% foram oriundos das matrizes de sangue de vivos e 64% oriundos de sangue post mortem. Nenhuma delas apresentou resultado quantificável para anfetamina


It is currently estimated that more than 5% of the world's population has been doing recreational use of some kind of psychoactive substances and the legal right to such use is a recurring theme debated by contemporary society. Due to the risks associated with populations health and safety, the abusive use of these substances has been instigating by social toxicology to search for answers to characterize, analyze and manage these risks. Drugs of great consumption in Brazil are, amphetamine cocaine and marijuana. This thesis proposes to develop a new methodology to detect and quantify psychoactive drugs in whole blood with the use of liquid phase microextraction by polypropylene fiber (HFLPME), followed by gas chromatography coupled to mass spectrometry (GC-MS). It is a technique that presents advantages compared with traditional ones, because of the smaller amounts demands of organic solvent, reducing risks and process costs. It also proposes a study with 69 blood samples taken from living persons and post mortem blood samples, which were obtained by agreement with the Superintendency of São Paulo Scientific Technical Police (SPTC / SP). The methods developed were validated according to international guidelines of forensic interest. As a result of the validation, the methods developed were precise and accurate for amphetamine and cocaine. The limit of cocaine detection was 5 ng . mL-1 and the limit of quantification was 10 ng . mL-1. As for amphetamine, the limits of detection and quantification were 5 ng . mL-1. The HF-LPME technique was not applicable to tetrahydrocannabinol (Δ9-THC). As a result of the sample analysis, 40% of them presented positive results for cocaine. Of these, 35% were from blood samples taken from living persons and 64% from the post mortem blood samples. None of the samples presented quantifiable results for amphetamine


Subject(s)
Amphetamine/analysis , Cocaine/analysis , Liquid Phase Microextraction/methods , Autopsy/statistics & numerical data , Dronabinol/analysis , Forensic Toxicology , Gas Chromatography-Mass Spectrometry/methods , Liquid Phase Microextraction/methods , Substance Abuse Detection/statistics & numerical data , Substance-Related Disorders
8.
São Paulo; s.n; s.n; 2017. 143p ilus, graf, tab.
Thesis in Portuguese | LILACS | ID: biblio-876551

ABSTRACT

Apesar dos diversos estudos sobre a presença de cianobactérias e a correlação entre fatores ambientais que influenciam ou desencadeiam florações, é ainda incipiente a informação sobre o controle fisiológico e bioquímico da produção de metabólitos secundários, cianotoxinas e compostos orgânicos voláteis (COVs) nestes organismos. Os COVs mais comumente encontrados em cianobactérias são a geosmina e o 2- metil-isoborneol, compostos que resistem ao tratamento convencional da água, causam mau cheiro e alteram seu gosto, além de bioacumular em peixes e moluscos. Estudos sobre possíveis sistemas de competição (alelopatia) entre linhagens de cianobactérias, ou entre elas e outros organismos, podem contribuir para elucidação do papel da produção de COVs por cianobactérias. Dessa forma, os objetivos deste projeto foram (i) prospectar a produção de COVs e seus efeitos na auto-regulação fisiológica em cianobactérias mantidas em laboratório; e (ii) desenvolver um método analítico, por microextração em fase sólida (SPME) e cromatografia em fase gasosa com detecção por espectrometria de massas (GC-MS), para a determinação destes compostos. Foram realizados ensaios para avaliar os perfis de produção dos COVs em duas linhagens de M. aeruginosa em diferentes fases de crescimento, sob diferentes intensidades luminosas (50, 150 e 250 ?µmol.fótons.m-2.s-1) e também ao longo do ritmo circadiano, avaliando a influência dos períodos claro e escuro. Para avaliar efeitos alelopáticos, exsudatos de uma linhagem de M. aeruginosa produtora de microcistinas foram testados em culturas de outra linhagem de M. aeruginosa não produtora de toxinas por meio de técnicas tradicionais de cultivo com monitoramento do crescimento. Na análise da produção de COVs, por GC-MS, observou-se que se destacam, majoritariamente, os compostos α-ciclocitral, ß-ciclocitral e ß-ionona, sendo o ß-ciclocitral o mais abundante, em todas as condições testadas, para as ambas as linhagens estudadas. A linhagem não toxigênica, no entanto, apresentou produção mais elevada de todos os compostos identificados. Dentre as intensidades luminosas testadas, a intensidade de 250 µmol.fótons.m-2s-1 foi a que apresentou a maior taxa de crescimento para a linhagem LTPNA 08 e relação negativa entre o aumento da irradiância e a produção de ß-ciclocitral. Foram identificadas, também, variações na produção dos compostos α-ciclocitral, ß-ciclocitral e ß-ionona nas linhagens ao longo do ritmo circadiano, sendo as maiores concentrações encontradas no período escuro. Observou-se morte celular e redução na produção de COVs 24 horas após adição de exsudatos pertencentes à linhagem de M. aeruginosa toxigênica em cultivos da linhagem não-toxigênica. Sendo assim, pode-se inferir que a produção dos COVs pode sofrer alterações qualitativas e quantitativas dependendo do estímulo ambiental presente, tanto por interações bióticas (com outros organismos e ritmo circadiano), quanto por fatores abióticos (intensidade luminosa)


There are several studies on the presence of cyanobacteria and the correlation between environmental factors that may influence or trigger blooms. However, information concerning the physiological and biochemical control of the production of secondary metabolites, toxins and volatile organic compounds (VOC) by cyanobacteria is poorly understood. Geosmin and 2-methyl-isoborneolare are commonly found VOC in cyanobacteria, they resist to conventional water treatment and can cause bad smell and taste in the final water. In addition, VOC can bioaccumulate in fish and shellfish. Studies on possible competition systems (allelopathy) either among strains of cyanobacteria or among them and other organisms such as green microalgae, may help to elucidate the role of VOC production by cyanobacteria. Thus, the main objectives of this study are: (i) prospect the production of VOCs and their effects on physiological self-regulation in cyanocrobacteria kept in the laboratory; and (ii) to develop an analytical method, by solid phase microextraction (SPME) and gas chromatography with mass spectrometry detection (GC-MS), for the determination of these compounds. The assays were carried out to evaluate the production profiles of VOCs in two strains of M. aeruginosa at different growth stages under different light intensities (50, 150 and 250 µmol.fótons.m-2.s-1) and also along of the circadian rhythm, evaluating the influence of light and dark periods. To assess allelopathic effects, exudates from a microcystin-producing strain of M. aeruginosa were tested on cultures of another non-toxin producing M. aeruginosa strain by traditional growth monitoring culture techniques. In the analysis of VOC production by GC-MS, it was observed that α-cyclocyclal, ß-cyclocyclal and ß-ionone compounds were the most prominent, with ß-cyclocitral being the most abundant in all conditions tested, for both strains studied. The non-toxigenic lineage, however, showed higher production of all the identified compounds. Among the light intensities tested, the intensity of 250 µmol.fótons.m-2s-1 was the one with the highest growth rate and positive relation between the irradiance increase and the ß-cyclocitral production. Variations in the production of the α-cyclocyclal, ß-cyclocyclal and ß-ionone compounds were also identified in the lines along the circadian rhythm, being the highest concentrations found in the dark period. Cell death and reduction in VOC production were observed 24 hours after addition of exudates belonging to the toxigenic M. aeruginosa lineage in cultures of the non-toxigenic lineage. Thus, it can be inferred that the production of VOCs can undergo qualitative and quantitative changes depending on the environmental stimulus present, both by biotic interactions (with other organisms and circadian rhythm) and by abiotic factors (luminous intensity)


Subject(s)
Cyanobacteria , Volatile Organic Compounds/analysis , Allelopathy , Gas Chromatography-Mass Spectrometry/methods , Microcystis/growth & development , Solid Phase Microextraction/methods
9.
Rev. biol. trop ; 64(3): 1101-1116, jul.-sep. 2016. tab, ilus
Article in English | LILACS | ID: biblio-958199

ABSTRACT

Abstract:Volatile compounds play a vital role in the life cycle of plants, possessing antimicrobial and anti-herbivore activities, and with a significant importance in the food, cosmetic, chemical, and pharmaceutical industry. This study aimed to identify the volatile compounds emitted by flowers of thirteen species belonging to four genera of Bromeliaceae, using headspace solid-phase micro-extraction and detection by gas chromatography-mass spectrometry. A total of 71 volatile compounds belonging to nine chemical groups were identified. The compounds identified represented more than 97 % of the major components in Aechmea bicolor, Ae. bromeliifolia, Ae. distichantha, Ae. fasciata, and Vriesea friburgensis. In the Ananas varieties, over 99 % of the components were identified, and around 90 % in V. simplex. V. friburgensis presented the largest diversity of volatiles with 31 compounds, while Alcantarea nahoumii presented only 14. All three Ananas varieties presented the same 28 compounds in relatively similar abundance, which has been confirmed by principal component analysis. Current taxonomy and pollination syndrome studies available can adequately explain the variation in volatile compounds among species. Rev. Biol. Trop. 64 (3): 1101-1116. Epub 2016 September 01.


ResumenLos compuestos volátiles tienen un papel vital en el ciclo de vida de las plantas. Poseen actividad antimicrobiana y anti-herbivoría biológica y una gran importancia en la industria de alimentos, cosméticos, perfumes, productos químicos y farmacéuticos. Este estudio tuvo como objetivo identificar los compuestos volátiles de trece flores de especies, pertenecientes a cuatro géneros de Bromeliaceae utilizando microextracción en fase sólida mediante cromatografía de gases hifenada con espacio de cabeza acoplada a espectrometría de masas. Se han identificado setenta y un diferentes compuestos volátiles pertenecientes a nueve grupos. Los compuestos identificados representaron más del 97 % de los componentes principales en Aechmea bicolor, Ae. bromeliifolia, Ae. distichantha, Ae. fasciata, Vriesea friburgensis, 99 % en las variedades de Ananas y 90 % en V. Simplex. V. friburgensis mostró la mayor diversidad de compuestos volátiles con 31, mientras que en Al. nahoumii se han encontrado sólo 14 compuestos. Las tres variedades de Ananas presentan los mismos 28 compuestos en cantidades relativamente similares, lo que se confirmó por el análisis de componentes principales. Estudios taxonómicos y síndromes de polinización disponibles podrían explicar la variación de los compuestos volátiles entre especies.


Subject(s)
Bromeliaceae/chemistry , Flowers/chemistry , Volatile Organic Compounds/analysis , Reference Values , Time Factors , Principal Component Analysis , Bromeliaceae/metabolism , Flowers/metabolism , Solid Phase Microextraction/methods , Gas Chromatography-Mass Spectrometry/methods
10.
Rev. cuba. plantas med ; 21(1)jan.-mar. 2016. ilus, tab
Article in Spanish | LILACS | ID: lil-781972

ABSTRACT

Introducción: las plantas aromáticas y medicinales son una fuente potencial de componentes antioxidantes. La Patagonia Argentina presenta un ambiente diverso en especies nativas, las cuales deberían ser estudiadas en mayor profundidad debido a su potencial farmacéutico, así como para contribuir a fomentar su conservación. Objetivos: estudiar la actividad antioxidante de infusiones, tinturas y aceites esenciales de las siguientes especies nativas de la Patagonia Argentina: Acantholippia seriphioides (A. Gray) Moldenke, Adesmia boronioides Hook. f., Buddleja globosa Hope, Fabiana imbricata Ruiz & Pav., Solidago chilensis Meyen. Identificar los componentes volátiles presentes en los aceites esenciales. Métodos: se obtuvieron infusiones y tinturas por la guía de las normas de la Farmacopea Argentina VI edición. Los aceites esenciales se obtuvieron por hidrodestilación con un aparato tipo Clevenger. El análisis de los componentes volátiles se realizó mediante cromatografía de gases-espectrometría de masas. Los ensayos de actividad antioxidante se realizaron por el método del difenil-picrilhidrazilo. Resultados: las especies presentaron el siguiente orden de actividad antioxidante: B. globosa > S. chilensis ≥ F. imbricata ≥ A . seriphioides > A. boronioides. Las infusiones de B. globosa, S. chilensis y A. seriphioides, presentaron una actividad antioxidante similar a Camellia sinensis (L.) Kuntze ("té verde") y superior a Ginkgo biloba (L.) Mant (especies reconocidas por su alto contenido de antioxidantes). La actividad encontrada para el aceite esencial de A. seriphioides se deba a sus contenidos en timol y carvacrol. En cuanto a la actividad de S. chilensis podría adjudicarse a su alto porcentaje de limoneno. Conclusiones: este trabajo es el primero que estudia la actividad antioxidante de plantas medicinales y aromáticas en la región noroeste de la Patagonia Argentina; los resultados obtenidos demuestran que las especies estudiadas de dicha región son una fuente rica en compuestos antioxidantes y de potencial valor como suplemento dietario(AU)


Introduction: medicinal and aromatic plants have potential as sources of antioxidant compounds. There is a great diversity of native species in Patagonia Argentina. It is worthy to study them because of its pharmaceutical potential and to help promote conservation. Objectives: to analyze antioxidant activities of herbal teas, tinctures and essential oils of native species from Patagonia Argentina: Acantholippia seriphioides (A. Gray) Moldenke, Adesmia boronioides Hook. f., Buddleja globosa Hope, Fabiana imbricata Ruiz & Pav., Solidago chilensis Meyen. Identify essential oils compounds. Methods: infusions and tinctures were obtained according to Pharmacopoeia Argentina VIth edition. The essential oils were obtained by hydrodistillation in a Clevenger apparatus. Volatiles compounds were analyzed by gas chromatography-mass spectrometry. Antioxidant activity assays were performed by difenil-picrilhidrazilo method. Results: antioxidant activity order was: B. globosa > S. chilensis ≥ F. imbricata ≥ A. seriphioides > A. boronioides. Infusions of B. globosa, S. chilensis and A. seriphioides presented an antioxidant activity similar to Camellia sinensis (L.) Kuntze ("green tea") and higher than Ginkgo biloba (L.) Mant. The A. seriphioides essential oil activity was probably obeyed to thymol and carvacrol presence. S. chilensis activity could be owing to its high limonene content. Conclusions: this study is the first report about antioxidant activity of medicinal and aromatic plants in the northwest region of Patagonia Argentina. The results showed that analyzed species are a rich source of antioxidant compounds and have potential value as a dietary supplement(AU)


Subject(s)
Humans , Fabiana imbricata/therapeutic use , Plant Preparations/therapeutic use , Solidago/drug effects , Buddleja/drug effects , Gas Chromatography-Mass Spectrometry/methods
11.
Bol. latinoam. Caribe plantas med. aromát ; 14(6): 442-448, Nov. 2015. tab
Article in English | LILACS | ID: biblio-907505

ABSTRACT

Phlomis species (Phlomis bucharica Regel and P. salicifolia Regel) have been traditionally used by Uzbek people as stimulant, tonic, diuretic, and in the treatment of ulcers, hemorrhoids, wounds and gynecological problems. In the present study, we characterized the chemical composition of non-polar extracts from P. bucharica and P. salicifolia by high resolution GLC-MS and evaluated their cytotoxicity. Concentrations of hexadecanoic acid in hexane and chloroform extracts were higher in P. bucharica than in P. salicifolia. 1,8- Cineol, camphor, borneol, alfa-terpinol, thymol, and isobornyl acetate were detected in P. bucharica but not in P. salicifolia. About 45 components were identified in P. bucharica and 40 in P. salicifolia. The chloroform extract from P. bucharica showed cytotoxicity in HeLa and HL-60 cells, with IC50 values of 26.07 and 29.42 ug/ml, respectively.


Las especies Phlomis (Phlomis bucharica Regel y P. salicifolia Regel) se han utilizado tradicionalmente por la gente de Uzbekistán como estimulante, tónico, diurético, y en el tratamiento de las úlceras, hemorroides, heridas y problemas ginecológicos. En el presente estudio, hemos caracterizado la composición química de los extractos no polares de P. bucharica y P. salicifolia por GLC-MS de alta resolución y se evaluó su citotoxicidad. Las concentraciones de ácido hexadecanoico en extractos de hexano y cloroformo fueron mayores en P. bucharica que en P. salicifolia. 1,8-cineol, alcanfor, borneol, se detectaron alfa-terpinol, timol, y acetato de isobornilo en P. bucharica pero no en P. salicifolia. Cerca de 45 componentes fueron identificados en P. bucharica y 40 en P. salicifolia. El extracto de cloroformo a partir de P. bucharica mostró citotoxicidad en células HL-60 y HeLa, con valores de CI 50 de 26,07 y 29,42 ug/ml, respectivamente.


Subject(s)
Oils, Volatile/chemistry , Oils, Volatile/pharmacology , Phlomis/chemistry , Plant Extracts/chemistry , Plant Extracts/pharmacology , Gas Chromatography-Mass Spectrometry/methods , Palmitic Acid/analysis , Terpenes/analysis
12.
Bol. latinoam. Caribe plantas med. aromát ; 14(5): 364-373, Sept. 2015. ilus
Article in Spanish | LILACS | ID: biblio-907499

ABSTRACT

Filmy ferns are a conspicuous epiphytic component of the temperate rain forest of southern Chile and the more abundant genus is Hymenophyllum represented by 19 species, they are a primitive fern family sharing their limited water lost control (poikilohydricity) with lower non-vascular plants, such as bryophytes and lichens. Because, carbohydrate accumulation is a desiccation tolerance mechanism proposed for desiccation-tolerant vascularized plants, the aim of this investigation was to propose a methodology for soluble carbohydrate analysis in native ferns. Preparative- TLC showed to be a simple and rapid technique for separating Hymenophyllum sugars. GC-MS analysis allowed identifying glucitol (2.0 percent), sucrose (2.0 percent), alpha or beta-melibiose (5.0 percent) and salidroside (4.4 percent) in H. cruentum carbohydrate profile from H. dentatum showed significant differences presenting only two sugars sucrose (1.4 percent) and alpha or beta-melibiose (3.2 percent). Furthermore, salidroside, an antioxidant compound, was identified only in H. cruentum. Our results suggest that H. cruentum, has higher preventive mechanisms than H. dentatum; that would allow delay the effects of desiccation (prevent a rapid dehydration) and thus survive to short periods of drought present in the study area. Due to the presence of salidroside in H. cruentum this species should be more resistant to oxidative stress that H. dentatum.


Los helechos película se pueden encontrar en el bosque templado lluvioso del sur de Chile, siendo el género más abundante Hymenophyllum representado con 19 especies. Son una familia de helechos primitivos que comparten la limitación de control de pérdida de agua (poiquilohidrícos) con plantas no vasculares, tales como briófitas y líquenes. Como el contenido de hidratos de carbono ha sido asociado a la protección de la planta durante la desecación, su análisis es una herramienta importante para dilucidar el mecanismo asociado a este fenómeno. El objetivo de esta investigación fue proponer una metodología fácil y rápida para el análisis de hidratos de carbono en helechos nativos. La CCF-preparativa permitió la separación de hidratos de carbono presentes en plantas del género Hymenophyllum. El análisis por GC-MS logró identificar glucitol (2,0 por ciento), sacarosa (2,0 por ciento), alfa o Beta-melibiosa (5.0 por ciento) y salidrosido (4,4 por ciento) en H. cruentum. El perfil de hidratos de carbono de H. dentatum mostró diferencias significativas, mostrando sólo dos compuestos sacarosa (1,4 por ciento) y alfa o beta- melibiosa (3.2 por ciento). Además, salidrosido, un compuesto antioxidante, sólo fue identificado en H. cruentum. Nuestros resultados sugieren que ante la menor tolerancia a la desecación observada previamente en H. cruentum, esta especie presenta mecanismos que le permitirían retardar los efectos de la desecación (prevención de una rápida pérdida de agua) y así sobrevivir a los periodos cortos de sequía presentes en la zona de estudio. Debido a La presencia de salidrosido en H. cruentum, esta especie debería ser más resistente al estrés oxidativo que H. dentatum.


Subject(s)
Carbohydrates/analysis , Ferns/chemistry , Gas Chromatography-Mass Spectrometry/methods
13.
Rev. cuba. farm ; 48(4)oct.-dic. 2014. ilus, tab
Article in Spanish | LILACS, CUMED | ID: lil-748771

ABSTRACT

INTRODUCCIÓN: la evaluación de hormonas en pacientes de endocrinología y bioquímica clínica, entre otros, se realiza actualmente por métodos de inmunoensayo con las desventajas inherentes a este tipo de análisis (ejemplo: reacciones cruzadas). Con la aplicación de la espectrometría de masas acoplada a cromatografía de gases es posible aumentar la sensibilidad y especificidad de los análisis. OBJETIVO: validar un ensayo que permita la cuantificación de 21 hormonas mediante la técnica de cromatografía de gases-espectrometría de masas con propósitos de pesquizaje. MÉTODOS: el ensayo se basó en una extracción en fase sólida con columnas DetectabuseTM y posterior extracción líquido-líquido a pH básico. Los derivados trimetilsilil se analizaron con un cromatógrafo de gases Hewlett-Packard 6890 acoplado a un espectrómetro de masas cuadrupolar serie 5973. La columna capilar fue HP Ultra-1 (17 m x 0,20 mm x 0,11 µm). La adquisición fue realizada en modo SIM (monitoreo selectivo de iones). RESULTADOS: los resultados del proceso de validación cumplieron con los criterios de aceptación de una manera adecuada correspondiente a un método con propósitos de pesquizaje. El método resultó ser específico para los 21 compuestos estudiados, lineal (r2= 0,900-0,996) y preciso (CV entre 1,4-9,6 por ciento). El rendimiento de extracción se mantuvo entre 69-117 por ciento. La robustez con variación de disolvente mostró recobrados entre 69-139 por ciento. CONCLUSIONES: los resultados demuestran que la técnica analítica desarrollada para la cuantificación de los 21 compuestos esteroidales en orina, es exacta, específica, lineal, precisa y robusta para su aplicación con propósitos de pesquizaje en estudios endocrinológicos clínicos(AU)


INTRODUCTION: the evaluation of hormones on endocrinology and clinical biochemistry patients, among others, is presently performed, using inmunoassays with its intrinsic disadvantages such as cross reactions. The application of gas chromatography coupled to mass spectrometry allows increasing the sensitivity and specificity of this analysis. OBJECTIVE: to validate an assay for quantitation of 21 hormones by the analytical technique of gas chromatography - mass spectrometry for screening purposes. METHODS: the assay followed a solid-phase extraction using DetectabuseTM columns and subsequently liquid-liquid extraction at basic pH. Trimethylsilyl derivatives were evaluated on Hewlett-Packard 6890 gas chromatograph coupled to serial 5973 quadrupolar mass spectrometer. The capillary column was HP Ultra-1 (17 m x 0.20 mm x 0.11 µm). Data was gathered following SIM mode (selective ion monitoring). RESULTS: the results of the validation process adequately fulfilled the acceptance criteria for screening purposes. The assay proved to be specific for all studied compounds, linear (r2= 0.900-0.996) and precise (VC 1.4-9.6 percent). The extraction yield was kept at 69-117 percent. The robustness assay with varying dissolvent showed extraction yields ranging 69-139 percent. CONCLUSIONS: results of the validation process show that the developed assay to simultaneously quantify 21 steroidal compounds in urine is exact, linear, precise, robust and specific for its application in clinical endocrine studies for screening purposes(AU)


Subject(s)
Humans , Male , Female , Validation Studies as Topic , Hormone Antagonists , Gas Chromatography-Mass Spectrometry/methods
14.
Bol. latinoam. Caribe plantas med. aromát ; 13(3): 285-296, mayo 2014. ilus, tab, graf
Article in English | LILACS | ID: lil-768855

ABSTRACT

In the present work an analytical methodology to micro scale based on the use of the HS-SPME/GC-MS to determine volatile compounds present in Clinopodium odorum (Griseb.) Harley (Lamiaceae)was optimized and settled differences and similarities with itsessential oil. A systematic description of the volatile components of flowers, stems, leaves and combined aerial parts (whole plant) was constructed via GC-MS analyses of HS-SPME adsorbed compounds and of essential oils obtained through hydrodistillation of the same tissues. Pulegone was the main component of both the HS-SPME analysis and essential oil analysis. In addition, piperitenone oxide andpiperitone oxide were the other main components in the essential oil whereas in the HS-SPME analysis cis-isopulegone and menthone prevailed. The HS-SPME method can achieve comparable results to those obtained by essential oil analysis, by using very fewer samples, ashorter extraction time and a much simpler procedure.


En el presente trabajo se ha optimizado una metodología analítica a micro-escala basada en HS-SPME/GC-MS para determinar los compuestos volátiles presentes en Clinopodium odorum (Griseb.) Harley (Lamiaceae), y se establecieron diferencias y similitudes con su aceite esencial. Se realizó una descripción sistemática de los componentes volátiles de flores, tallos, hojas y partes aéreas combinadas(planta entera) a partir de los análisis por GC-MS a través del sistema HS-SPME y de los aceites esenciales. Pulegona fue el componenteprincipal tanto del análisis por HS-SPME, como del aceite esencial. Además, el óxido de piperitenona y el óxido de piperitona eran los otroscomponentes principales en el aceite esencial mientras que en el análisis por HS-SPME, prevalecieron cis-isopulegona y mentona. El método de HS-SPME puede lograr resultados comparables a los obtenidos por el análisis de aceite esencial, mediante el uso de muestras de menor tamaño, un tiempo de extracción más corto y un procedimiento más simple.


Subject(s)
Oils, Volatile/chemistry , Gas Chromatography-Mass Spectrometry/methods , Distillation , Lamiaceae/chemistry , Menthol/analysis , Monoterpenes/analysis
15.
São Paulo; s.n; s.n; 2014. 174 p. tab, graf, ilus.
Thesis in Portuguese | LILACS | ID: biblio-847098

ABSTRACT

Os n-3 e n-6 são duas famílias de ácidos graxos poli-insaturados. Os ácidos graxos de cadeia longa como o ácido araquidônico (AA) e docosahexaenoico (DHA) apresentam importantes funções no desenvolvimento e funcionamento do cérebro. Os produtos de oxidação dos ácidos graxos poli-insaturados estão presentes ou aumentados ao longo do desenvolvimento de doenças neurodegenerativas. A caracterização de tais produtos é crítica para o estudo que busca entender o seu papel fisiopatológico no desenvolvimento de tais doenças. No presente trabalho, buscou-se o desenvolvimento de uma ferramenta analítica sensível e específica para a detecção e quantificação dos hidroperóxidos e hidróxidos do AA (HpETE e HETE), do seu precursor, o ácido linoleico (HpODE e HODE) e do DHA (HpDoHE e HDoHE). Estes hidroperóxidos foram sintetizados por fotooxidação e os hidróxidos correspondentes foram obtidos através da redução com o NaBH4. Os isômeros isolados foram caracterizados por LC-MS/MS. Os íons produto específicos de cada isômero foram escolhidos para a construção do método de monitoramento de reação selecionada (selected reaction monitoring - SRM) para a realização da análise quantitativa dos analitos de interesse. Cabe salientar que os dados obtidos poderão ser utilizados em bibliotecas de análise lipidômica e oxi-lipidômica pois serão essenciais para a identificação e quantificação dos analítos de interesse do presente estudo em diversas doenças. Utilizando o método padronizado, buscamos investigar o papel dos hidroperóxidos e hidróxidos do DHA, LA e AA em um modelo animal para a esclerose lateral amiotrófica (ELA), uma doença neurodegenerativa que acomete neurônios motores. Foi observado um aumento nos níveis de 13-HpODE, 9-HpODE e 12-HETE no córtex motor dos animais avaliados. Adicionalmente, foram observadas alterações nas taxas lipólica e lipogênica no tecido adiposo para os animais ELA em relação aos respectivos controles. Em conjunto, os dados apresentados no presente trabalho corroboram com os trabalhos da literatura que associam alteração dos níveis dos produtos de oxidação dos ácidos graxos poli-insaturados em doenças neurodegenerativas e o metabolismo energético alterado em ELA. Futuramente é necessária uma investigação mais ampla dos níveis dos hidroperóxidos e hidróxidos lipídicos em diferentes tecidos e do metabolismo lipídico, e os conhecimentos gerados poderão ser uma importante fonte de novas opções terapêuticas para os pacientes portadores de ELA


The n-3 and n-6 are two olyunsaturated fatty acids families. The long chain fatty acids such as arachidonic (AA) and docosahexaenoic acid (DHA) have important roles in the development and function of the brain. Polyunsaturated fatty acids (PUFAs) oxidation products are present or increased during the progression of neurodegenerative diseases. The characterization of DHA oxidation products is critical to understand their roles in the development of such diseases. In the present study, we sought to develop a sensitive and specific analytical tool for the detection and quantification of AA hydroperoxides and hydroxides (HPETE and HETE), its precursor linoleic acid (HPODE and HODE) and DHA (HpDoHE and HDoHE). These hydroperoxides were synthesized by photooxidation and the corresponding hydroxides were obtained by reduction with NaBH4. The isolated isomers were characterized by LC-MS/MS, and unique and specific fragment ions were chosen to construct a selected reaction monitoring (SRM) method for the targeted quantitative analysis. It should be emphasized that the data obtained - in the form of lipidomics and oxy-lipidomics libraries - may be used to assist in several diseases. Using the standardized method, we investigated the role of hydroperoxides and hydroxides of DHA, LA and AA in an animal model of amyotrophic lateral sclerosis (ALS), a neurodegenerative disease that affects motor neurons. Increased levels of 13-HPODE, 9-HPODE and 12-HETE were observed in the animals motor cortex. Additionally, results show changes in lipogenic and lipolytic rates in adipose tissue for ALS animals when compared to their respective controls. Altogether, the data presented herein corroborate with the literature by linking altered levels of PUFAs oxidation products in neurodegenerative diseases with altered energetic metabolism in ALS. In the future, a more extensive investigation of the hydroperoxide and hydroxide level in different tissues as well as the lipid metabolism must be done, which could lead to new therapeutic options for ALS patients


Subject(s)
Animals , Male , Female , Rats , Docosahexaenoic Acids/analysis , Neurodegenerative Diseases/prevention & control , Oxidation/analysis , Amyotrophic Lateral Sclerosis/pathology , Biomarkers, Pharmacological , Gas Chromatography-Mass Spectrometry/methods , Hydroxyeicosatetraenoic Acids/analysis , Photooxidation/methods
16.
Mem. Inst. Oswaldo Cruz ; 108(6): 778-784, set. 2013. graf
Article in English | LILACS | ID: lil-685498

ABSTRACT

The cuticular hydrocarbons of the Triatoma sordida subcomplex (Hemiptera: Reduviidae: Triatominae) were ana-lysed by gas chromatography and their structures identified by mass spectrometry. They comprised mostly n-alkanes and methyl-branched alkanes with one-four methyl substitutions. n-alkanes consisted of a homologous series from C21-C33 and represented 33-45% of the hydrocarbon fraction; n-C29 was the major component. Methyl-branched alkanes showed alkyl chains from C24-C43. High molecular weight dimethyl and trimethylalkanes (from C35-C39) represented most of the methyl-branched fraction. A few tetramethylalkanes were also detected, comprising mostly even-numbered chains. Several components such as odd-numbered 3-methylalkanes, dimethylalkanes and trimethylalkanes of C37 and C39 showed patterns of variation that allowed the differentiation of the species and populations studied. Triatoma guasayana and Triatoma patagonica showed the most distinct hydrocarbon patterns within the subcomplex. The T. sordida populations from Brazil and Argentina showed significantly different hydrocarbon profiles that posed concerns regarding the homogeneity of the species. Triatoma garciabesi had a more complex hydrocarbon pattern, but it shared some similarity with T. sordida. The quantitative and qualitative variations in the cuticular hydrocarbons may help to elucidate the relationships between species and populations of this insect group.


Subject(s)
Animals , Female , Male , Hydrocarbons/isolation & purification , Lipids/isolation & purification , Triatoma/chemistry , Analysis of Variance , Alkanes/analysis , Gas Chromatography-Mass Spectrometry/methods
17.
Indian J Exp Biol ; 2013 Mar; 51(3): 262-268
Article in English | IMSEAR | ID: sea-147591

ABSTRACT

Carbon (neutral) based renewable liquid biofuels are alternative to petroleum derived transport fuels that contribute to global warming and are of a limited availability. Microalgae based biofuels are considered as promising source of energy. Lyngbya sp. and Synechococcus sp. were studied for the possibility of biodiesel production in different media such as ASNIII, sea water enrichment medium and BG11. The sea water enrichment medium was found superior in enhancing the growth rate of these microalgae. Nitrogen depletion has less effect in total chlorophyll a content, at the same time the lipid content was increased in both Lyngbya sp. and Synechococcus sp. by 1.4 and 1.2 % respectively. Increase in salinity from 0.5-1.0 M also showed an increase in the lipid content to 2.0 and 0.8 % in these strains; but a salinity of 1.5 M has a total inhibitory effect in the growth. The total biomass yield was comparatively higher in tubular LED photobioreactor than the fluorescent flat plated photobioreactor. Lipid extraction was obtained maximum at 60 ºC in 1:10 sample: solvent ratio. GC-MS analysis of biodiesel showed high content of polyunsaturated fatty acids (PUFA; 4.86 %) than saturated fatty acid (SFA; 4.10 %). Biodiesel production was found maximum in Synechococcus sp. than Lyngbya sp. The viscosity of the biodiesel was closely related to conventional diesel. The results strongly suggest that marine microalgae could be used as a renewable energy source for biodiesel production.


Subject(s)
Biofuels , Biomass , Bioreactors , Carbon/chemistry , Chlorophyll/metabolism , Cyanobacteria/metabolism , Energy-Generating Resources/economics , Equipment Design , Esters/chemistry , Gas Chromatography-Mass Spectrometry/methods , Lipids/chemistry , Microalgae , Nitrogen/metabolism , Photochemistry/methods , Solvents/chemistry , Synechococcus/metabolism , Triglycerides/chemistry , Viscosity
19.
IJPR-Iranian Journal of Pharmaceutical Research. 2013; 12 (2): 295-302
in English | IMEMR | ID: emr-142649

ABSTRACT

A reliable, rapid and accurate method based on spiked calibration curves and direct sample introduction was developed for determination of 17 pesticide residues in rice by gas chromatography-mass spectrometry single quadrupole selected ion monitoring GC/MS-SQ-SIM. Sample preparation is based on extraction with acetonitrile without clean up. The use of spiked calibration curves for constructing the calibration curve substantially reduced adverse matrix-related effects. The average recovery of pesticides at 6 concentration levels was in range of 97.5-102.1%. The method was proved to be repeatable with RSDr in range of 0.7%-19.8%for all of the concentration levels. The limits of detection and limit of quantifications for all the pesticides were < 10 ng/g and < 25 ng/g, respectively. The developed method was applied for simultaneous determination of the selected pesticides in 23 rice samples collected from Tehran retail market in March 2009. Although many studies have been conducted regarding the determination of pesticides by using GC-MS, this is the first attempt in Iran using GC-MS-SIM technique that successfully can determine 17 pesticides with difference in physicochemical properties in rice


Subject(s)
Gas Chromatography-Mass Spectrometry/methods , Oryza/chemistry , Crops, Agricultural/chemistry , Pesticide Residues/isolation & purification
20.
Rev. bras. plantas med ; 15(2): 217-224, 2013. graf, tab
Article in English | LILACS | ID: lil-677029

ABSTRACT

Tilia species, among which is Tilia cordata Mill. (Tiliaceae), have been used in folk medicine as anxiolytic. The hydroethanolic extract was analyzed by using liquid chromatography with mass spectrometry HPLC-DAD-ESI-MS/MS in negative ion mode, and its chemical composition was compared to flavonoids reported as anxiolytics. The major flavonoids found were: quercetin-3,7-di-O-rhamnoside, kaempferol-3,7-di-O-rhamnoside and kaempferol 3-O-(6"-p-coumaroyl glucoside) or tiliroside. The anxiolytic activity of the genus Tilia has been attributed to the presence of quercetin and kaempferol derivatives, while the anxiolytic activity of T. americana var. Mexicana was attributed to tiliroside, which was also found among the major constituents of this species.


As espécies de Tilia, entre elas, a Tilia cordata Mill. (Tiliaceae) são utilizadas como ansiolíticas na medicina popular. O extrato hidroalcoólico foi analisado usando cromatografia líquida acoplada à espectrometria de massas HPLC-DAD-ESI/MS/MS no modo negativo e a sua composição química foi comparada com os flavonóides já reportados como ansiolíticos. Os principais flavonóides encontrados foram: quercetina-3,7-di-O-rhamnosideo, canferol-3,7-di-O-rhamnosideo, e canferol 3-O-(6"-p-cumaroil glucosideo) ou tilirosideo. A atividade ansiolítica do gênero Tília tem sido atribuída à presença de derivados de canferol e quercetina, enquanto que a atividade ansiolítica da T. americana var. Mexicana foi atribuída ao tilirosideo, o qual também foi encontrado entre os principais constituintes desta espécie.


Subject(s)
Anti-Anxiety Agents , Tilia europaea/analysis , Gas Chromatography-Mass Spectrometry/methods , Glycosides , Quercetin
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