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São Paulo; s.n; s.n; 2023. 131 p. tab, graf, ilus.
Thesis in Portuguese | LILACS | ID: biblio-1437606


myrsine coriacea (Sw.) R. Br. ex Roem. & Schult. (Primulaceae) conhecida popularmente como capororoquinha ou capororoca, é amplamente distribuída nas regiões sul e sudeste do Brasil. As espécies desse gênero apresentam um potencial antioxidante e anti-inflamatório, que pode ser acessado na busca de novos ativos para o tratamento de desordens pigmentares da pele. Desta forma, este trabalho teve como objetivos avaliar o potencial antitirosinase e antioxidante de extratos e frações de M. coriacea e identificar os possíveis compostos responsáveis por essas atividades. Foram realizados ensaios para avaliar o potencial antioxidante das amostras através do método do DPPH, enquanto a capacidade hipopigmentante das amostras foi avaliado pela inibição da enzima tirosinase. Como complemento, foram determinados os teores de compostos fenólicos totais e flavonoides através dos métodos colorimétricos empregando o reagente Folin-Ciocalteau e AlCl3. Adicionalmente, os extratos de M. coriacea tiveram avaliados seus potenciais citotóxicos utilizando diferentes linhagens tumorais humanas. O perfil fitoquímico de M. coriacea foi analisado por cromatografia a gás acoplada com espectrometria de massas (CG-EM) e cromatografia em camada delgada (CCD) com padrões. Nessas análises foram identificados 34 compostos, sendo o ácido palmítico e o palmitato de etila os compostos majoritários nas amostras de M. coriacea. O extrato bruto das folhas apresentou o maior teor de fenólicos totais, enquanto a fração de acetato de etila das folhas teve o maior teor de flavonoides. Contudo, o extrato bruto dos frutos apresentou a melhor atividade antioxidante de todas as amostras analisadas, apresentando também a melhor atividade antitirosinase. Dentre os compostos anotados, mandenol, ácido -linoleico e o linolenato de etila foram os compostos considerados como possíveis inibidores da tirosinase, com boa interação molecular com a enzima nas análises de ancoragem molecular in silico. Das amostras analisadas com relação a inibição de crescimento frente as células tumorais, a amostra da fração de clorofórmio das folhas foi a que apresentou potencial antitumoral frente as células de adenocarcinoma de cólon (HCT116)

myrsine coriacea (Sw.) R. Br. ex Roem. & Schult. (Primulaceae) popularly known as capororoquinha or capororoca, is widely distributed in southern and southeastern Brazil. Myrsine species have an antioxidant and anti-inflammatory potential, which can be accessed in the search for new actives for the treatment of skin pigmentation disorders. Thus, this work aimed to evaluate the antityrosinase and antioxidant potential from extracts and fractions of M. coriacea and to identify the probable compounds responsible for these activities. Assays were performed to evaluate the antioxidant potential of the samples using the DPPH method, while the hypopigmentation capacity of the samples was evaluated by the tyrosinase inhibition. As a complement, the amounts of total phenolic compounds and flavonoids were determined through colorimetric methods using the Folin-Ciocalteau reagent and AlCl3. Additionally, M. coriacea extracts had their cytotoxic potential evaluated using different human tumor cell lines. M. coriacea phytochemical profile was obtained by gas chromatography coupled with mass spectrometry (GC-MS) and thin layer chromatography (TLC) with standards. In these analyses, 34 compounds were identified, with palmitic acid and ethyl palmitate as the major compounds in M. coriacea samples. The leaf crude extract presented the highest total phenolics contents, while the leaf ethyl acetate fraction had the highest flavonoid amounts. However, the fruit crude extract showed the best antioxidant and antityrosinase activities of all analyzed samples. Among the annotated compounds, mandenol, -linoleic acid and ethyl linolenate were the compounds considered as putative tyrosinase inhibitors, presenting good molecular interaction with the enzyme active site in the in silico molecular docking analysis. The leaf chloroform fraction was the only sample that showed an antitumor potential against colon adenocarcinoma cells (HCT116)

Monophenol Monooxygenase/analysis , Primulaceae/metabolism , Myrsine/classification , Fruit/classification , Antioxidants/analysis , Mass Spectrometry/methods , Skin Pigmentation/immunology , Chromatography, Thin Layer/methods , Hypopigmentation/pathology
Braz. J. Pharm. Sci. (Online) ; 59: e21726, 2023. tab, graf
Article in English | LILACS | ID: biblio-1439500


Abstract Pterocarpus santalinoides is used in Nigerian ethnomedicine to treat diabetes mellitus. This study aimed to establish the antidiabetic property of the plant, and isolate and characterize its active principle. Dried and pulverized leaves (500 g) of P. santalinoides were extracted with 1.8 L of 80 % hydromethanol by cold maceration. The dried extract (10 g) was partitioned into n-hexane, ethyl acetate (EtOAc), n-butanol, and water. Antidiabetic activitiy-guided isolation by column chromatographic separation of the EtOAc soluble and purification of the sub-fractions by repeated preparative thin layer chromatography (pTLC) yielded a C-glycosyl flavonoid, identified as isovitexin. The chemical structure was elucidated based on high-resolution mass spectroscopy, 1D, and 2D nuclear magnetic resonance spectroscopic analyses. Alloxan-induced diabetic rat model was adopted for antidiabetic screening. The extract of P. santalinoides (100-200 mg/kg), fraction F4 (50 mg/kg), sub-fraction F4.3 (10 mg/kg), and the semi-purified compound F4.3.2 (5 mg/kg) significantly (p<0.05) reduced the fasting blood glucose of alloxan-induced diabetic rats, causing 48.4, 69.4, 57.7 and 64.5 % antidiabetic activity respectively, compared with > 68 % recorded in glibenclamide (2 mg/kg) control. These results reveal that isovitexin is the antidiabetic principle in P. santalinoides

Animals , Male , Rats , Plant Extracts/analysis , Pterocarpus/adverse effects , Hypoglycemic Agents/analysis , Mass Spectrometry/methods , Flavonoids/pharmacology , Magnetic Resonance Spectroscopy/methods , Chromatography, Thin Layer/methods , Diabetes Mellitus/pathology , Acetates/pharmacology
Braz. J. Pharm. Sci. (Online) ; 58: e18860, 2022. tab, graf
Article in English | LILACS | ID: biblio-1364415


Abstract There is no biodistribution or imaging data on 99mtechnetium (Tc)-hexamethyl propylamine oxime (HMPAO)-labeled platelets in the literature. The current study aimed to present updated information about the clinical procedures for preparation and use of labeled platelets. Following two-step centrifugation at 1500 and 2500 rpm, the platelets were extracted from whole blood into platelet-rich plasma (PRP) above the buffy coat and then from PRP into a platelet pellet at the bottom of the tube. The 99mTc-HMPAO-labeled platelets were inspected for purity, viability, release of 99mTc from platelets, and sterility. Also, microscopic examination and thin layer chromatography (TLC) were performed. Biodistribution was assessed following necropsy in BALB/c mice and through imaging of New Zealand rabbits. The separation ratio was estimated at 98%, and radiochemical purity was measured to be 80%. The labeling efficiency was above 30% in more than half of the assays (range: 17-43%). The release of 99mTc from platelets was 9% per hour at 37ºC. After 24 hours, stability was estimated at 54% in the human serum. The target organs of mice included the spleen and liver. In rabbits, the imaging results indicated liver as the target organ. Thyroid uptake was negligible up to 90 minutes. Based on the findings, extraction of platelets and labeling them with 99mTc-HMPAO is a feasible and safe approach in routine practice.

Humans , Animals , Male , Mice , Quality Control , Blood Platelets/classification , Technetium Tc 99m Exametazime , Methods , Spleen , Chromatography, Thin Layer/methods , Efficiency/classification , Platelet-Rich Plasma , Liver
Braz. J. Pharm. Sci. (Online) ; 56: e18094, 2020. tab, graf
Article in English | LILACS | ID: biblio-1285510


Ursodeoxycholic acid (UDCA), a secondary bile acid (BA), has been used as a drug to treat various liver diseases. UDCA is synthesised from cholic or chenodeoxycholic acid (CA/CDCA), two primary BAs frequently used as the starting materials. Nowadays, swine, cattle, and poultry bile are the main sources of those BAs. However, other commercial animals could be promising sources as well. We identified two livestock, two poultries, and eight fishes that are commercially cultivated in Indonesia. Four free BAs including CA, CDCA, deoxycholic acid (DCA), and lithocholic acid (LA) were identified for their occurrences using thin-layer chromatography and high-performance liquid chromatography. CA was detected in cow, duck, red tilapia, gourami, the common carp, and grouper, whereas CDCA was only detected in two poultries and the common carp. The occurrence of DCA was common and abundant in most tested animals. In contrast, the presence of LA was found to be very low in all samples. The biliary bile of tilapia has been found to contain a high abundance of free CA (43% of the total bile). A simple extraction was able to purify CA from biliary bile of tilapia. This is a new promising and competitive source of CA.

Animals , Male , Female , Bile/drug effects , Chromatography, High Pressure Liquid/methods , Chromatography, Thin Layer/methods , Indonesia/ethnology , Animals , Ursodeoxycholic Acid , Ursodeoxycholic Acid/antagonists & inhibitors , Bile Acids and Salts/therapeutic use , Chenodeoxycholic Acid , Tilapia/classification , Cholic Acid/agonists , Deoxycholic Acid , Lithocholic Acid
Rev. cuba. plantas med ; 22(1)ene.-mar. 2017. ilus, tab
Article in Spanish | LILACS, CUMED | ID: biblio-901502


Introducción: Curcuma longa L. es una planta de la familia Zingiberaceae distribuida en las regiones tropicales y subtropicales, utilizada en la industria alimentaria, en medicina y en cosmética. Su colorante principal es la curcumina, un polifenol con múltiples efectos medicinales. Objetivos: obtener, caracterizar químicamente y evaluar la actividad biológica de tres curcuminoides de C. longa, cultivada en el Quindío-Colombia. Métodos: se purificaron tres curcuminoides (curcumina (C), demetoxicurcumina (DMC) y bisdemetoxicurcumina (BDMC) desde el rizoma de la planta, en estado seco, por cromatografía en columna y se caracterizaron por punto de fusión, espectroscopía infrarroja (IR), espectroscopía UV-vis y espectrometría de masas. Se evaluó la actividad antimicrobiana en bacterias y hongos por el método modificado de pozos de agar, la citotoxicidad sobre células BHK-21 por el método de bromuro de 3-(4,5- dimetiltiazol-2-ilo)-2,5-difeniltetrazol (MTT) y la toxicidad sobre Artemia salina. Finalmente se determinó el efecto de los curcuminoides en células BHK-21 infectadas con dengue virus 2. Resultados: la curcumina presentó mayor punto de fusión (177,3 ºC-183,2 ºC). El espectro IR reveló los grupos funcionales característicos y el UV-vis indicó máximos de absorción para curcumina, demetoxicurcumina y bisdemetoxicurcumina de 419, 418 y 414 nm en cloroformo, respectivamente. El espectro de masas mostró m/z para C: 368, DMC: 338 y BDMC: 308. Se encontró actividad antimicrobiana frente a Staphylococcus aureus y Staphylococcus epidermidis, se determinó que BDMC presentó menor toxicidad y se evidenció mayor efecto inhibitorio sobre viriones infectivos de dengue con curcumina a 20 y 30 M. Conclusiones: la caracterización de los compuestos confirma su composición como polifenoles, lo cual se relaciona a la actividad biológica de éstos, encontrándose principalmente que la curcumina altera la infección por virus dengue en cultivo celular. Esta investigación confirma la importancia de los principios activos de plantas con amplio espectro farmacológico como C. longa(AU)

Introduction: Curcuma longa L. is a plant from the family Zingiberaceae distributed in tropical and subtropical regions and used in the food industry, in medicine and in cosmetics. Its main coloring substance is curcumin, a polyphenol with many medicinal properties. Objectives: Obtain, characterize chemically and evaluate the biological activity of three curcuminoids from C. longa grown in Quindío, Colombia. Methods: Three curcuminoids (curcumin (C), demethoxycurcumin (DMC) and bisdemethoxycurcumin BDMC) from the rhizome of the plant were purified in a dry state by column chromatography and characterized by fusion point, infrared (IR) spectroscopy, UV-vis spectroscopy and mass spectrometry. Antimicrobial activity against bacteria and fungi was evaluated by the modified agar well method, cytotoxicity to BHK-21 cells by the 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) method, and toxicity against Artemia salina. Finally, determination was made of the effect of the curcuminoids in BHK-21 cells infected with dengue virus 2. Results: Curcumin had the highest fusion point (177.3 ºC-183.2 ºC). IR spectroscopy revealed the characteristic functional groups and UV-vis spectroscopy showed maximum absorption values for curcumin, demethoxycurcumin and bisdemethoxycurcumin of 419, 418 and 414 nm in chloroform, respectively. Mass spectrometry found that m/z values were C: 368, DMC: 338 and BDMC: 308. Antimicrobial activity was observed against Staphylococcus aureus and Staphylococcus epidermidis. BDMC was found to have lower toxicity. A greater inhibitory effect against infective dengue virions was observed with curcumin at 20 y 30 µM. Conclusions: Characterization of the compounds confirms their polyphenolic composition, which manifests in their biological activity, mainly the capacity of curcumin to alter infection by dengue virus in cell cultures. The study corroborated the importance of the active principles of plants with a wide pharmacological spectrum, such as C. longa(AU)

Humans , Curcuma/drug effects , Products with Antimicrobial Action , Virion , Chromatography, Thin Layer/methods , Colombia
Rev. cuba. plantas med ; 22(1)ene.-mar. 2017. ilus, tab
Article in Spanish | LILACS, CUMED | ID: biblio-901503


Introducción: Solanum dolichosepalum Bitter, llamada comúnmente frutillo, es tradicionalmente usada en Colombia como antibacteriano, antiinflamatorio, cicatrizante y en enfermedades renales. La escasa información en bases de datos sobre la planta en estudio no permitió referenciar un mayor número de artículos actuales. Objetivo: evaluar la actividad antibacteriana de extractos obtenidos del fruto de S. dolichosepalum y realizar un estudio fitoquímico preliminar. Método: la actividad antimicrobiana fue evaluada a partir de cuatro fracciones (F) obtenidas del extracto etanólico de los frutos secos deS. dolichosepalum frente a cepas de Escherichia coli, Staphylococcus aureus y Pseudomona aeruginosa por el método de Kirby-Bauer. La primera fracción se sometió a cromatografía en columna y a sus fracciones se les evaluó la concentración inhibitoria mínima (MIC) por el método de microdilución. Los metabolitos responsables de la actividad antimicrobiana se identificaron por cromatografía de capa delgada en placas de sílica gel (MERCK) y lámpara ultravioleta (365nm). Se realizó finalmente un estudio fitoquímico del extracto etanólico de los frutos para evaluar la presencia de metabolitos bioactivos. Resultados: las pruebas fitoquímicas del extracto etanólico revelaron la presencia de alcaloides, esteroides y/o triterpenoides libres, taninos, saponinas, flavonoides y glucósidos cardiotónicos. De las cuatro fracciones obtenidas a partir de este extracto, las fracciones F1 y F2 tuvieron MIC de 31,25 y 15,62 mg/mL, respectivamente frente a E. coli y de 500 y 31,25 mg/mL frente a S. aureus. F3 y F4 no presentaron inhibición y ninguna fracción tuvo actividad frente a P. aeruginosa. Las fracciones obtenidas por cromatografía en columna a partir de F1 se denominaron F1A, F1B, F1C y F1D; la fracción F 1B mostró la mayor actividad antimicrobiana, con MICs de 35 y 17,5 mg/mL frente a S. aureus y E. coli respectivamente. Conclusiones: los resultados obtenidos confirman el uso tradicional delS. dolichosepalum como antibacteriana, con actividad frente a E. coli y S. aureus(AU)

Introduction: Solanum dolichosepalum Bitter, commonly known as frutillo, has been traditionally used in Colombia as antibacterial, antiinflammatory and cicatrizant, and to treat renal disease. Due to the scant information about the study plant contained in databases, it was not possible to reference a larger number of current papers. Objective: Evaluate the antibacterial activity of extracts obtained from the fruit of S. dolichosepalum and conduct a preliminary phytochemical study. Method: The Kirby-Bauer method was applied to four fractions (F) obtained from the ethanolic extract of dry fruits of S. dolichosepalum to evaluate antimicrobial activity against strains ofEscherichia coli, Staphylococcus aureus and Pseudomona aeruginosa. The first fraction underwent column chromatography and its fractions were tested for minimum inhibitory concentration (MIC) using the microdilution method. Metabolites responsible for antimicrobial activity were identified by thin layer chromatography on silica gel plates (MERCK) with an ultraviolet lamp (365 nm). Finally, a phytochemical study was conducted of the ethanolic extract of the fruits to determine the presence of bioactive metabolites.Results: Phytochemical testing of the ethanolic extract revealed the presence of alkaloids, steroids and/or free triterpenoids, tannins, saponins, flavonoids and cardiotonic glucosides. Of the four fractions obtained from the extract, fractions F1 and F2 had an MIC of 31.25 and 15.62 mg/mL, respectively, against E. coli, and 500 and 31.25 mg/mL against S. aureus. F3 and F4 did not show any inhibition, and no fraction displayed any activity against P. aeruginosa. The fractions obtained by column chromatography from F1 were named F1A, F1B, F1C and F1D. Fraction F1B showed the highest antimicrobial activity, with MICs of 35 and 17.5 mg/mL against S. aureus and E. coli, respectively. Conclusions: The results obtained confirm the validity of the traditional use ofS. dolichosepalum as antibacterial, with activity against E. coli and S. aureus(AU)

Humans , Male , Female , /therapeutic use , Solanum , Phytotherapy , Chromatography, Thin Layer/methods , Colombia
Rev. cuba. plantas med ; 22(1)ene.-mar. 2017. ilus, tab
Article in Spanish | LILACS, CUMED | ID: biblio-901508


Introducción: la composición química de las especies vegetales está sujeta a cambios, dependiendo, entre otros factores, de la localización geográfica. Moringa oleífera Lam., que crece en Machala, Ecuador, puede diferir de especies de otras regiones geográficas. Objetivo: realizar un estudio farmacognóstico preliminar del tallo y raíz (corteza y pulpa) de la planta M. oleífera cultivada en las áreas de la Unidad Académica de Ciencias Agropecuarias, de la Universidad Técnica de Machala. Métodos: se desarrolla el control de la calidad de la droga cruda según la metodología establecida por la Organización Mundial de la Salud, mediante determinación de la humedad residual, el porciento de cenizas y el porciento de sustancias solubles en el tallo y la raíz. Se cuantificaron algunos metales mediante espectrometría de emisión óptica con plasma acoplado inductivamente. El estudio químico preliminar se efectuó a través de ensayos de tamizaje fitoquímico y mediante cromatografía en capa delgada. Resultados: la humedad residual para ambos órganos y los valores de cenizas obtenidos para la raíz se encuentran dentro de los límites establecidos. Las cenizas totales para el tallo resultaron elevadas. La determinación de metales descartó la presencia de metales tóxicos en los órganos estudiados. Los valores de sustancias solubles indicaron mayor poder extractivo para el agua. La evaluación mediante tamizaje fitoquímico sugirió triterpenos y esteroides, azúcares reductores, alcaloides, flavonoides, aminoácidos y saponinas, en los extractos de la raíz. En el tallo se detectaron, además, catequinas, mucílagos y compuestos fenólicos, no así flavonoides. La cromatografía en capa delgada sugirió la existencia de alcaloides derivados de la fenilmetilamina. Conclusiones: el estudio permitió establecer parámetros de calidad de la droga cruda para la especie estudiada; sugerir, en principio, semejanzas en composición química de la planta analizada con otras de orígenes geográficos diferentes, y comprobar la ausencia de metales tóxicos en los órganos estudiados(AU)

Introduction: The chemical composition of plant species is subject to changes which depend, among other factors, on their geographic location. The Moringa oleifera Lam. growing in Machala, Ecuador, may differ from species from other geographic regions. Objective: Conduct a preliminary pharmacognostic study of the stem and root (bark and pulp) of the plant M. oleifera grown in areas from the Agricultural Sciences Academic Unit of the Technical University of Machala. Methods: Quality control was performed of the crude drug following the methodology set up by the World Health Organization to determine residual humidity, percentage of ashes and percentage of soluble substances in the stem and the root. Several metals were quantified by inductively coupled plasma atomic emission spectroscopy. The preliminary chemical study was conducted by phytochemical screening testing and thin layer chromatography. Results: Both the residual humidity for both organs and the ash values obtained for the root are within the limits established. Total ashes for the stem were high. Metal determination discarded the presence of toxic metals in the organs studied. Values for soluble substances awarded a greater extraction capacity to water. Phytochemical screening pointed to the presence of triterpenes and steroids, reducing sugars, alkaloids, flavonoids, amino acids and saponins in root extracts. The stem was found to also contain catechins, mucilages and phenolic compounds, but not flavonoids. Thin layer chromatography pointed to the presence of alkaloids derived from phenyl methylamine. Conclusions: The study made it possible to set up crude drug quality parameters for the study species, make preliminary suggestions about similarities between the chemical composition of the plant analyzed and other plants of different geographic origin, and verify the absence of toxic metals in the organs studied(AU)

Humans , Pharmacognosy , Benzylamines/antagonists & inhibitors , Chromatography, Thin Layer/methods , Moringa oleifera/toxicity , Ecuador/ethnology
São Paulo; s.n; s.n; 2017. 93 p. tab, graf, ilus.
Thesis in Portuguese | LILACS | ID: biblio-875303


Mono e diacilgliceróis são produtos empregados na indústria alimentícia, farmacêutica, cosmética e química como emulsificantes e melhoradores de viscosidade de produtos alimentícios, cosméticos e farmacêuticos. No entanto, a forma mais usual de obtê-los é por síntese química, o que acaba rendendo produtos finais caros e com atributos de qualidade, rendimento e de aplicabilidade tecnológica inferiores aos esperados. A busca por formas de obtenção mais racionais, eficientes e com melhor padrão de qualidade destes produtos foi o objetivo principal do trabalho, por meio de hidrólise parcial enzimática, que necessita de condições de reação mais brandas. Foram avaliadas a hidrólise enzimática descontína, empregando como substrato a trioleína técnica, e a hidrólise enzimática descontínua-alimentada, usando como substrato o óleo de girassol médio oléico. Foi utilizada, em ambos processsos, a lipase imobilizada sn-1,3 específica Lipozyme RM IM (de Rhizomucor miehei). A caracterização dos padrões e dos substrados, bem como o acompanhamento da formação dos produtos da hidrólise enzimática foram feitos por determinação da porcentagem de hidrólise, cromatografia em camada delgada (TLC), dos perfis das curvas de fusão e cristalização por calorimetria diferencial de varredura (DSC), cromatografia gasosa (CG) e cromatografia de exclusão de tamanho de alto desempenho (HPSEC). Os parâmetros de hidrólise descontínua foram o tempo de reação, a temperatura e a concentração inicial de substrato. Os parâmetros de hidrólise descontínua-alimentada foram tempo de enchimento e intervalo de alimentação de substrato. Para as respostas analíticas de porcentagem de hidrólise e de composição de frações lipídicas foi aplicado um modelo de regressão múltipla com base em metodologia de superfície de resposta. Os resultados experimentais observados nas reações de hidrólise enzimática descontínua de trioleína técnica mostraram de 24,7 a 34,2% de mono e diacilgliceróis (para 5% de óleo na emulsão) e de 21,4 a 33,6% de mono e diacilgliceróis (para 20% de óleo na emulsão). Os resultados experimentais observados nas reações de hidrólise enzimática descontínua-alimentada de óleo de girassol médio oléico (para 15% de óleo na emulsão), mostraram de 7,9 a 31,8% de mono e diacilgliceróis. Os modelos de superfície de resposta foram considerados significativos e preditivos. As hidrólises obtidas no formato descontínuo e descontínuo-alimentado permitiram efetivamente a obtenção de frações de mono/ diacilgliceróis com vários graus de eficiência de conversão e com corretas identificação e quantificação das frações de lipídios procuradas. As correlações feitas entre porcentagem de hidrólise e entalpias de cristalização e fusão, corroboradas com os resultados qualitativos e/ou quantitativos diretos obtidos na cromatografia de camada delgada (TLC) e de HPSEC, demonstraram que estes atributos podem positivamente indicar a ocorrência efetiva de reação de hidrólise, além de auferir uma escala de desempenho de reação alinhada com o previsto na literatura, à medida que são aumentadas a temperatura, o tempo de hidrólise e a porcentagem inicial de substrato oleoso, sob regime descontínuo, e que puderam ser melhoradas, de forma inovadora, sob parâmetros de tempo total de alimentação e de intervalo de alimentação, sob regime descontínuo-alimentado. A hidrólise parcial enzimática de triacilgliceróis utilizando lipase imobilizada sn-1,3 específica pode ser considerada uma alternativa às vias químicas para a produção de misturas de mono e diacilgliceróis para utilização como aditivos químicos.

Mono and diacylglycerols are products used in the food, pharmaceutical, cosmetic and chemical industries as emulsifiers and viscosity improvers for food products, cosmetics and pharmaceuticals. However, the most usual forms of obtaining them are by chemical synthesis, which ends up yielding expensive final products with attributes of quality, yield and technological applicability lower than expected. The search for more rational, efficient and better quality standards of these products was the aim of the work, through partial enzymatic hydrolysis, which requires milder reaction conditions. Discontinuous enzymatic hydrolysis was evaluated using technical triolein as substrate and discontinuous-fed enzymatic hydrolysis using as the substrate the mid oleic sunflower oil. In both processes, immobilized lipase sn-1,3 specific Lipozyme RM IM (from Rhizomucor miehei) was used. The characterization of the patterns and substrates, as well as the monitoring of the formation of the products from the enzymatic hydrolysis were made by determining the percentage of hydrolysis, thin layer chromatography (TLC), profiles of the melting and crystallization curves by differential scanning calorimetry ( DSC), gas chromatography (GC) and high performance size exclusion chromatography (HPSEC). The parameters of discontinuous hydrolysis were the reaction time, the temperature and the initial substrate concentration. The parameters of discontinuous-fed hydrolysis were filling time and substrate feed interval. For the analytical responses of hydrolysis percentage and composition of lipid fractions a multiple regression model was applied based on response surface methodology. The experimental results observed in the reactions of discontinuous enzymatic hydrolysis of technical triolein indicated amounts of mono- and diacylglycerols from 24.7 to 34.2% (for 5% of oil in the emulsion) and from 21.4 to 33.6% for mono and diacylglycerols with 20% oil in the emulsion. The experimental results observed in the reactions of discontinuous-fed enzymatic hydrolysis of mid oleic sunflower oil (for 15% oil in the emulsion), showed from 7.9 to 31.8% of mono and diacylglycerols. Response surface models were considered significant and viii predictive. The hydrolysis obtained in the discontinuous and discontinuous-fed form allowed to obtain fractions of mono / diacylglycerols with various degrees of conversion efficiency and with correct identification and quantification of the lipid fractions sought. The correlations between the percentage of hydrolysis and enthalpies of crystallization and fusion, corroborated with the qualitative and / or quantitative direct results obtained in thin layer chromatography (TLC) and HPSEC, showed that these attributes can positively indicate the effective occurrence of reaction of Hydrolysis, in addition to achieving a reaction performance scale in line with the literature, as the temperature rate, the hydrolysis time and the initial percentage of oily substrate are increased under a discontinuous regime and can be improved, in a innovative form, under parameters of total filling time and feeding interval, under a fed-batch regime. The partial enzymatic hydrolysis of triacylglycerols using specific sn-1,3-specific immobilized lipase may be considered an alternative to the chemical pathways for the production of mono- and diacylglycerol blends for use as chemical additives.

Diglycerides/analysis , Hydrolysis , Calorimetry, Differential Scanning , Oils , Chromatography, Thin Layer/methods , Monoglycerides/classification , Lipase
Rev. cuba. plantas med ; 21(4)oct.-dic. 2016. tab
Article in Spanish | LILACS, CUMED | ID: biblio-960654


Introducción: el género Piper perteneciente a la familia Piperaceae es de gran importancia económica debido a sus aplicaciones a nivel alimenticio, industrial y medicinal. Especies de este género son conocidas popularmente como cordoncillos y se caracterizan porque presentan un amplio espectro de actividades biológicas, entre las que se encuentra el efecto neuroprotector, que está asociado al tratamiento de enfermedades neurodegenerativas como el Alzheimer. En Colombia existen muchas especies a las cuales no se les han desarrollado estudios investigativos, tal es el caso de Piper pesaresanum C. DC. Objetivo: caracterizar química y biológicamente el extracto etanólico de hojas de P. pesaresanum mediante un estudio fitoquímico biodirigido y evaluar la actividad inhibitoria sobre acetilcolinesterasa. Métodos: a partir del extracto etanólico de hojas maduras de P. pesarenasum se realizó un estudio químico biodirigido para aislar e identificar las sustancias responsables de la actividad inhibitoria sobre acetilcolinesterasa. La evaluación de la actividad inhibitoria sobre acetilcolinesterasa se realizó por autografía directa empleando el método de Ellman. Adicionalmente se realizó un tamizaje fitoquímico preliminar mediante pruebas de coloración y precipitación llevadas a cabo en vía húmeda y cromatografía en capa delgada. Resultados: el análisis fitoquímico preliminar sugiere la presencia de terpenos, esteroides, fenoles y cumarinas. La evaluación de la actividad inhibitoria sobre acetilcolinesterasa permitió evidenciar zonas claras de inhibición en las fracciones de éter de petróleo (EP) y cloroformo (CHCl3). El estudio fitoquímico biodirigido condujo al aislamiento e identificación por primera vez para la especie del ácido 4-metoxi-3,5-di(3'-metil-2'-butenil) benzoico. Conclusiones: el estudio químico y de actividad biológica llevado a cabo en la especie P. pesaresanum permitió identificar al ácido 4-metoxi-3,5-di(3'-metil-2'-butenil) benzoico como uno de los compuestos responsables de la actividad inhibitoria sobre acetilcolinesteras(AU)

Introduction: The genus Piper, from the Piperaceae family, has great economic importance, due to its uses on a nutritional, industrial and medicinal level. The species in this genus are commonly known as peppers, and are characterized by a broad range of biological activities, including a neuroprotective effect associated with the treatment of neurodegenerative conditions such as Alzheimer's disease. Many of the species growing in Colombia have not been studied. Such is the case with Piper pesaresanum C. DC. Objective: Carry out a chemical and biological characterization of the ethanolic extract of P. pesaresanum leaves by means of a bioguided phytochemical study and evaluate inhibitory activity on acetylcholinesterase. Methods: A bioguided chemical study was conducted of the ethanolic extract of P. pesarenasum mature leaves to isolate and identify the substances responsible for inhibitory activity on acetylcholinesterase. Evaluation of inhibitory activity on acetylcholinesterase was based on direct autography using the Ellman method. Preliminary phytochemical screening was also performed by means of wet color and precipitation tests, and thin-layer chromatography. Results: Preliminary phytochemical analysis suggests the presence of terpenes, steroids, phenols and coumarins. Evaluation of inhibitory activity on acetylcholinesterase revealed clear-cut inhibition areas in petroleum ether (PE) and chloroform (CHCl3) fractions. The bioguided phytochemical study led to isolation and identification of 4-methoxy-3.5-di(3'-methyl-2'-butenyl) benzoic acid for the first time in the study species. Conclusions: Chemical study and evaluation of the biological activity of the species P. pesaresanum led to identification of 4-methoxy-3.5-di(3'-methyl-2'-butenyl) benzoic acid as one of the compounds responsible for inhibitory activity on acetylcholinesterase(AU)

Humans , Piperaceae/drug effects , Plant Preparations/therapeutic use , Alzheimer Disease/drug therapy , Acetylcholinesterase , Chromatography, Thin Layer/methods , Colombia
Rev. cuba. plantas med ; 21(4)oct.-dic. 2016. ilus, tab
Article in Spanish | LILACS, CUMED | ID: biblio-960653


Introducción: la especie Esenbeckia litoralis Donn.Sm. (Rutaceae) es también conocida como Loro o Loro grande, ha sido empleado en la medicina tradicional para el tratamiento de mordeduras de serpientes, dolor de garganta y lesiones ocasionadas por picaduras de insectos. Esta variedad de actividades son causadas por acción de los compuestos que la constituyen, como lignanos, terpenos, alcaloides, cumarinas y polifenoles que representan un alto potencial farmacológico para esta especie. Objetivo: realizar el estudio fitoquímico y evaluación de la actividad antioxidante de la especie E. litoralis. Métodos: los extractos vegetales de hojas corteza y madera se obtuvieron empleando etanol al 96 por ciento, y posteriormente fueron fraccionados usando técnicas cromatográficas como Cromatografía en Capa Delgada (CCD), Cromatografía en Columna (CC) y Cromatografía en Capa Delgada Preparativa (CCDP). Los compuestos se identificaron mediante el análisis de datos espectroscópicos con el empleo de técnicas instrumentales como: Infrarrojo (IR), Resonancia Magnética Nuclear Protónica y de Carbono trece (RMN-1H y 13C), Espectrometría de Masas (EM) y difracción de rayos x (DRX). La actividad antioxidante se evaluó a través de los métodos radical catiónico ABTS•+, radical libre DPPH• y Potencial de Actividad de Reducción Férrica (FRAP). Resultados: de esta especie se aislaron e identificaron cinco compuestos: cuatro alcaloides y un flavonoide. Los extractos en acetato de etilo de hojas y corteza mostraron una significativa actividad frente a los radicales ABTS•+ con un IC50 de 5,65 y 7,65 µg/mL respectivamente. Conclusiones: de los distintos extractos se aislaron cinco compuestos: 1-hidroxi-3-metoxi-N-metilacridona (1), maculosidina (2) maculina (3), dictamina (4) y gardenina B (5). El extracto en acetato de etilo de hojas y corteza presentaron una significativa actividad antioxidante frente al radical ABTS con un IC50 de 5,65 y 7,65 mg/L, respectivamente(AU)

Introduction: The species Esenbeckia litoralis Donn. Sm. (Rutaceae), also known as loro or loro grande, has been used in traditional medicine to treat snakebites, sore throats and lesions caused by insect bites. The compounds contained in the plant, among them lignans, terpenes, alkaloids, coumarins and polyphenols, are responsible for such a broad variety of activities, granting it great pharmacological potential. Objective: Conduct a phytochemical study and evaluation of the antioxidant activity of the species E. litoralis. Methods: Plant extracts from leaves, stem and wood were obtained using 96 percent ethanol, and then fractioned with chromatographic techniques such as thin-layer chromatography (TLC), column chromatography (CC) and preparative thin-layer chromatography (PTLC). The compounds were identified by spectroscopic data analysis using instrumental techniques such as infrared (IR) spectroscopy, proton and Carbon-13 nuclear magnetic resonance (NMR-1H and 13C), mass spectrometry (MS) and X-ray diffraction (XRD). Antioxidant activity was evaluated with the methods ABTSo+ radical cation, DPPHo free radical and ferric reducing ability power (FRAP). Results: Five compounds were isolated from the species: four alkaloids and one flavonoid. Ethyl acetate extracts from leaves and stem displayed significant activity against ABTSo+ radicals, with a CI50 of 5.65 and 7.65 µg/ml, respectively. Conclusions: Five compounds were isolated from the various extracts: 1-hydroxy-3-methoxy-N-methylacridone (1), maculosidin (2), maculin (3), dictamin (4) and gardenin B (5). The leaf and stem extract in ethyl acetate displayed significant antioxidant activity against the ABTS radical, with a CI50 of 5.65 and 7.65 mg/l, respectively(AU)

Humans , Rutaceae/drug effects , Plant Preparations/therapeutic use , Antioxidants/therapeutic use , Chromatography, Thin Layer/methods , Phytochemicals
Bol. micol. (Valparaiso En linea) ; 31(2): 1-8, dic. 2016. tab
Article in Spanish | LILACS | ID: biblio-868811


Antecedentes: la fitoterapia es una de las más antiguas prácticas utilizadas por la humanidad. Hasta mediados del siglo XIX, cuando se introdujeron los medicamentos, la formulación de estos generalmente era basada en plantas medicinales. Objetivos: Determinar la micobiota y los niveles de aflatoxinas originadas de Aspergillus sección Flavi aislados de las 50 muestras de medicamentos fitoterápicos comercializados actualmente en la ciudad de São Paulo, Brasil. Métodos: Cincuenta (50) muestras de medicamentos fitoterápicos en la forma de hojas (té-25) y cápsulas (25) fueron colectadas de agosto de 2000 a julio de 2001. Los hongos filamentosos aislados fueron identificados al nivel de género de acuerdo con las características morfológicas y criterios taxonómicos. El análisis de aflatoxinas fue realizada por cromatografía de capa fina (TLC). Resultados: El análisis microbiológico mostró que 41 (82 por ciento) de los medicamentos fitoterápicos presentaron un crecimiento fúngico sobre las 100 UFC/g. Un total de 106 especies de seis diferentes géneros fueron aislados (Aspergillus, Penicillium, Mucor, Rhizopus y Alternaria). El género Aspergillus fue el predominante (60.5 por ciento) seguido por Penicillium (20,0 por ciento). Aspergillus niger (30 por ciento) A. flavus (22 por ciento), A. fumigatus (6,5 por ciento) y A. parasiticus fueron las especies de Aspergillus identificadas. Se observó que 13 (56,5 por ciento), de los 23 A. flavus aislados y dos aislados de A. parasiticus produjeron aflatoxinas. Conclusiones: La contaminación observada en la mayoría de los productos y el alto nivel de cepas productoras de aflatoxinas justifica un análisis más cuidadoso de los medicamentos fitoterápicos comercializados y la aplicación de leyes más rigurosas son necesarias para garantizar la calidad de los productos.

Background: phytotherapy is one of the most ancient practices used by humanity. In Antiquity until the middle of the XIX century, when chemotherapeutic drugs were introduced, formulation of medicines was usually based on medicinal plants. Objective: To determine mycobiota and levels of Aspergillus section Flavi aflatoxins isolated from 50 samples of phytotherapeutic remedies currently commercialized in São Paulo, Brazil. Methods: Fifty (50) samples of phytotherapeutic remedies in the form of leaves (teas-25) and powders (capsules-25) were collected from August 2000 to July 2001. Filamentous fungi isolates were identified at the genera level in accordance with morphological characteristics and taxonomic criteria. Aflatoxins were performed by Thin-layer chromatography (TLC). Results: The microbiological analysis showed that 41 (82 percent) of phytotherapeutic remedies presented a fungal growth over 100 CFU/g. A total of 106 species of six different genera were isolated (Aspergillus, Penicillium, Mucor, Rhizopus and Alternaria). The genus Aspergillus was the predominant (60.5 percent) followed by Penicillium genus (20.0 percent). Aspergillus niger (30 percent) A. flavus (22 percent), A. fumigatus (6.5 percent) and A. parasiticus were the species of Aspergillus identified. It was observed that 13 (56.5 percent) of 23 A. flavus isolates and two A. parasiticus isolates produced aflatoxins. Conclusions: The contamination observed in most products and the high level of aflatoxigenic strains justify the concern regarding the execution of more careful analyzes of the commercialized phytotherapeutic remedies and the application of more rigorous laws that may warrant the quality of these products.

Aflatoxins , Aspergillus flavus/isolation & purification , Aspergillus flavus/growth & development , Aspergillus flavus/pathogenicity , Mycotoxins , Plants, Medicinal/microbiology , Brazil , Chromatography, Thin Layer/methods , Fungi/classification , Fungi/pathogenicity , Mycobiome , Phytotherapeutic Drugs , Quality Control
Rev. cuba. plantas med ; 21(3)jul.-set. 2016. tab
Article in Spanish | LILACS, CUMED | ID: biblio-845110


Introducción: Bejaria resinosa Mutis ex L. es una especie vegetal conocida en Colombia como pegamosco; es empleada por diferentes comunidades para atrapar insectos y para el tratamiento de dolencias respiratorias; además, es una especie que cuenta con escasos estudios desde el punto de vista químico y biológico. Objetivos: contribuir al estudio fitoquímico de las hojas, flores y frutos de B. resinosa (Ericaceae) y evaluar su actividad antiinflamatoria. Métodos: hojas, flores y frutos por separado fueron extraídos por maceración en frío con éter de petróleo y etanol 96 por ciento; estos extractos se fraccionaron por partición líquido/líquido y métodos cromatográficos; su actividad antiinflamatoria se evaluó utilizando el modelo murino de edema auricular inducido por 13-acetato de 12-tetradecanoilforbol (TPA). La elucidación estructural de los compuestos aislados se llevó a cabo mediante las técnicas de CG-EM y RMN (experimentos 1H, 13C, COSY, J-MOD, HSQC y HMBC). Resultados: la separación de los extractos y fracciones por cromatografías en columna, en capa delgada y preparativa, permitieron obtener una mezcla de compuestos tipo triterpeno compuesta por germanicol, -amirina y -amirina y el aislamiento de lupeol, salicilato de metilo, 3,5,7,3´,4´ pentahidroxiflavona (quercetina), 3,5-dihidroxi-6,7,8-trimetoxiflavona y 3,5,7,3´,4´ pentahidroxiflavanol. Se encontró que la fracción que contiene la mezcla de triterpenos y la quercetina fueron las que presentaron un efecto antiinflamatorio mayor al 65 por ciento. Conclusiones: el estudio fitoquímico de la especie vegetal B. resinosa permitió establecer similitud en cuanto a la composición química de los diferentes órganos ya que se encontraron metabolitos secundarios comunes para hojas flores y frutos como la mezcla de triterpenos, lupeol y quercetina; además se logró establecer que la mezcla de triterpenos y la quercetina son fuertes agentes antiinflamatorios, pues redujeron significativamente el edema causado por el TPA en la oreja del ratón con porcentajes de inhibición cercanos a los presentados por el fármaco de referencia, indometacina(AU)

Introduction: Bejaria resinosa Mutis ex L. is a plant species known as pegamosco in Colombia. It is used by several communities to catch insects and to treat respiratory disorders. Few chemical and biological studies have been conducted about this species. Objectives: Contribute to the phytochemical study of leaves, flowers and fruits of B. resinosa (Ericaceae) and evaluate its anti-inflammatory activity. Methods: Leaves, flowers and fruits were extracted separately by cold maceration with petroleum ether and 96 percent ethanol. The extracts obtained were fractioned using liquid / liquid partition and chromatographic methods. Their anti-inflammatory activity was evaluated with the mouse model of ear edema induced by 12-tetradecanoyl phorbol 13-acetate (TPA). Structural characterization of the compounds isolated was based on GC-MS and NMR techniques (experiments 1H, 13C, COSY, J-MOD, HSQC and HMBC). Results: Separation of extracts and fractions by thin-layer and preparative column chromatography made it possible to obtain a mixture of triterpene compounds made up of germanicol, α-amyrin and ß-amyrin, and isolate lupeol, methyl salicylate, 3,5,7,3´,4´ pentahydroxyflavone (quercetin), 3,5-dihydroxy-6,7,8-trimetoxyflavona and 3,5,7,3´,4´-pentahydroxyflavanol. It was found that the fraction containing the mixture of triterpenes and quercetin had an anti-inflammatory effect above 65 percent. Conclusions: The phytochemical study of the plant species B. resinosa revealed similarities between the chemical composition of the different organs, since common secondary metabolites were found in leaves, flowers and fruits, such as the mixture of triterpenes, lupeol and quercetin. It was also established that the mixture of triterpenes and quercetin is a strong anti-inflammatory agent, for it significantly reduced the mouse ear edema caused by TPA with inhibition percentages close to those of the drug of reference indometacin(AU)

Humans , Chromatography, Thin Layer/methods , Ericaceae , Plant Preparations/therapeutic use , Anti-Inflammatory Agents/therapeutic use , Colombia
Rev. cuba. farm ; 50(1)ene.-mar. 2016.
Article in Spanish | LILACS, CUMED | ID: biblio-844874


El sobrepeso y la obesidad son considerados un problema de salud pública a nivel mundial y a la postre, esa condición incentiva que millones de personas consuman productos para perder o controlar el peso. Dentro de este significativo mercado se puede encontrar una gran cantidad y variedad de productos que se comercializan con la denominación de origen natural. En la última década, se presenta que muchos de ellos son adulterados con sustancias sintéticas para potencializar su efecto. Una de las drogas sintéticas que se utiliza con ese propósito es la sibutramina, aun cuando fue retirada del mercado a nivel mundial en el año 2010 debido a sus graves efectos secundarios. En este trabajo se describen algunos ejemplos de casos importantes de adulteración de productos naturales en el orbe y las metodologías analíticas que se pueden utilizar en la determinación de su adulteración con sibutramina; luego de revisar y seleccionar artículos científicos de los últimos años y acceder a través de bases de datos Proquest, Scient Direct, Springer, EBSCO y otras del Sistema de Bibliotecas e Información de la Universidad de Costa Rica. Se encontró una variedad de técnicas y metodologías analíticas que permiten identificar y cuantificar la presencia de sibutramina en productos utilizados para bajar de peso(AU)

Overweight and obesity are considered as a public health problem worldwide and ultimately, this condition encourages millions of people to buy products for losing or controlling weight. In this significant market, it is possible to find a large number and great variety of products sold under the natural origin denomination. In the last decade, it has been found that many of them have been adulterated with synthetic substances to potentiate their effect. A synthetic drug that is used for this purpose is sibutramine, even though it was withdrawn from the worldwide market in 2010 because of its serious side effects. This paper described some significant examples of adulteration of natural products in the world and the analytical methodologies that can be used in determining the adulteration of these goods with sibutramine after reviewing and selecting scientific papers in recent years and access through databases Proquest, Scient Direct, Springer, EBSCO and others of the System of Libraries and Information at the University of Costa Rica. A range of techniques and analytical methods to identify and quantify sibutramine in slimming products was found(AU)

Humans , Biological Products/therapeutic use , Overweight/epidemiology , Obesity/drug therapy , Chromatography, Thin Layer/methods , Costa Rica , Reference Drugs
Rev. cuba. farm ; 49(4)oct.-dic. 2015. ilus
Article in Spanish | LILACS, CUMED | ID: lil-780750


Introducción: las hojas de Pteris vittata L (helecho) son utilizadas por la población para el tratamiento de la candidiasis y en enfermedades producidas por bacterias en la piel. Objetivo: identificar preliminarmente las familias de metabolitos secundarios presentes en las hojas de la planta y evaluar su posible actividad antimicrobiana. Métodos: se recolectaron las hojas de Pteris vittata L. El material vegetal fue lavado, desinfectado, secado y seguidamente se procedió a su pulverización. Este polvo se utilizó en la elaboración de los diferentes extractos y tintura. La tintura obtenida se concentró y se fraccionó sucesivamente con n-hexano, cloroformo y acetato de etilo. A estos extractos se les realizó el tamizaje fitoquímico, ensayos microbiológicos y cromatografía de capa fina. Resultados: las pruebas in vitro efectuadas a los extractos obtenidos a partir de la tintura 20 por ciento, demostraron que éstos presentan actividad antimicrobiana frente a Escherichia coli, Staphylococcus aureus, destacándose los resultados obtenidos frente a Candida sp para los extractos de acetato de etilo y clorofórmico. En estas fracciones están presentes en mayor proporción alcaloides y quinonas, que podrían ser los responsables de esta actividad, lo cual se corrobora con la identificación de estos metabolitos secundarios mediante la cromatografía de capa fina y el tamizaje fitoquímico realizado. Conclusiones: el estudio combinado mediante la cromatografía de capa fina y el tamizaje fitoquímico de los extractos hexánico, acetato de etilo y clorofórmico permite inferir que la actividad antimicrobiana puede deberse a la presencia de quinonas y alcaloides(AU)

Introduction: Pteris vittata L. leaves (fern) are used by people on the candidiasis treatment and some skin illnesses caused by bacteria. Objective: to identify preliminarily the secondary metabolites present in the leaves of the plant and to evaluate their possible antimicrobial activity. Methods: Pteris vittata L. leaves were collected. The plant material was washed, disinfected, dried and pulverized. The powder obtained was used to make the various extracts and the tincture. The latter was concentrated and successively fractionated with n-hexane, chloroform, and ethyl acetate. The extracts underwent phytochemical screening, microbiological assays and thin-layer chromatography. Results: in vitro tests performed in the obtained extracts from the 20 percent tincture proved that they have antimicrobial activity against Escherichia coli and Staphylococcus aureus, emphasizing the accomplished results against Candida of the ethyl and chloroform acetate extracts. Alkaloids and quinones, which are found in large proportion in the extracts, would be responsible of the above- mentioned antibacterial activity. This was corroborated by the identification of these secondary metabolites through thin-layer chromatography and phytochemical screening. Conclusions: the combined study through thin-layer chromatography and phytochemical screening of the ethyl and chloroform acetate extracts showed that the antimicrobial activity could be possible due to the alkaloids and quinones presence(AU)

Humans , Candidiasis/therapy , Pteris , Dermatologic Agents/therapeutic use , Phytotherapy , Chromatography, Thin Layer/methods
Braz. j. med. biol. res ; 48(10): 902-907, Oct. 2015. tab, ilus
Article in English | LILACS | ID: lil-761597


Knowledge of the radiochemical purity of radiopharmaceuticals is mandatory and can be evaluated by several methods and techniques. Planar chromatography is the technique normally employed in nuclear medicine since it is simple, rapid and usually of low cost. There is no standard system for the chromatographic technique, but price, separation efficiency and short time for execution must be considered. We have studied an alternative system using common chromatographic stationary phase and alcohol or alcohol:chloroform mixtures as the mobile phase, using the lipophilic radiopharmaceutical [99mTc(MIBI)6]+ as a model. Whatman 1 modified phase paper and absolute ethanol, Whatman 1 paper and methanol:chloroform (25:75), Whatman 3MM paper and ethanol:chloroform (25:75), and the more expensive ITLC-SG and 1-propanol:chloroform (10:90) were suitable systems for the direct determination of radiochemical purity of [99mTc(MIBI)6]+ since impurities such as99mTc-reduced-hydrolyzed (RH),99mTcO4- and [99mTc(cysteine)2]-complex were completely separated from the radiopharmaceutical, which moved toward the front of chromatographic systems while impurities were retained at the origin. The time required for analysis was 4 to 15 min, which is appropriate for nuclear medicine routines.

Chromatography, Paper/methods , Chromatography, Thin Layer/methods , Radiopharmaceuticals/analysis , /analysis , Alcohols , Chloroform , Chromatography, Paper/economics , Chromatography, Thin Layer/economics , Chromatography/economics , Chromatography/methods , Quality Control , Radiopharmaceuticals/classification
Acta toxicol. argent ; 23(2): 89-94, set. 2015.
Article in Portuguese | LILACS | ID: biblio-908895


Aflatoxinas são metabólitos secundários de fungos com grande potencial carcinogênico, produzidos principalmente por Apergillus flavus e Aspergillus parasiticus. Em vista da ampla variedade de alimentos em que se encontram essas micotoxinas, o presente estudo teve como objetivo determinar condições de cultivo para o Aspergillus parasiticus e produção das quatro principais aflatoxinas (AFB1, AFB2, AFG1 e AFG2) considerando diferentes substratos conhecidos pela contaminação por estas micotoxinas, entre eles arroz branco, arroz cateto, amendoim, milho e farinha de trigo integral, e diferentes valores de umidade e pH. Ao analisar por cromatrografia em camada delgada os extratos dos diferentes substratos, verificou-se a produção de aflatoxinas em todos os alimentos, porém na cromatografia líquida de alta eficiência foi possível perceber a maior produção de aflatoxinas no arroz cateto e na farinha de trigo integral. Para a continuidade do trabalho, utilizou-se o arroz cateto e então preparou- se diferentes meios sólidos com valores de pH entre 3,5 e 7,5 e umidade entre 42 % e 62 %. Ao analisar por CLAE, todas as amostras apresentaram produção de AF, porém as amostras com o maior valor de água agregada (62%) apresentaram maior produção enquanto a variação de pH não apresentou influência nesta produção.

Aflatoxins are secondary metabolites of fungi with great carcinogenic potencial, mainly produced by Aspergillus flavus and Aspergillus parasiticus. In order of the wide variety of foods where mycotoxins are found in, this study aimed to determine growth conditions for Aspergillus parasiticus and production of four major aflatoxins (AFB1, AFB2, AFG1 and AFG2) considering different substrates known for contamination by these aflatoxins, including white rice, cathetus rice, peanuts, maize and whole wheat flour, and different pH and humidity values. When extracts of different substrates were analyzed by thin layer chromatography, it has been verified the production of aflatoxins in all foods; however, when high performance liquid chromatography (HPLC) analysis was performed, the greater production of aflatoxins was observed in cathetus rice and whole-wheat flour. Cathetus rice was then selected to continue the study and different solid medium with pH values between 3.5 and 7.5 and humidity percentages between 42 % and 62 % were prepared. When analyzed by HPLC, all samples showed production of aflatoxins, but the samples with higher humidity value (62%) showed greatest production while the pH changes had no effect on this production.

Aflatoxins/toxicity , Aspergillus/pathogenicity , Arachis/microbiology , Chromatography, High Pressure Liquid/methods , Chromatography, Thin Layer/methods , Oryza/microbiology , Triticum/microbiology , Zea mays/microbiology
Article in English | IMSEAR | ID: sea-162094


Introduction: On Sudden death of a medical student (20 year old girl) of National Institute of Medical Science autopsy materials along with site of injection were sent to F.S.L. It was informed during investigation that the girl took tetanus vaccine before death. In crime scene investigation Forensic Team observed that it was a case of gross negligence of dispensing wrong injection. Material: Tests were performed on viscera material viz., liver, spleen, kidney, lungs, brain, skin and blood etc. Mystery of suspected death was solved when a new GC-MS application was designed to get the unknown drug and various fragments of extracted material were studied. Method: A new method was developed on gas-chromatography-mass spectrophotometer and TL.C using various solvent systems is explained. Results: Metabolite fragments of vecuronium bromide a muscle relaxant were surprisingly observed in Viscera material, Blood sample and Skin piece from Leftt cubital fossa from this young girl, whose death is questioned. Conclusion: Structural elucidations of fragments provide a new approach to toxicokinetics. Th e explanation of fragments obtained were structurally compared with other neuromuscular blocking groups like atracurium and succinyl choline Th e presence of bromide attached cholest-5-en-Br, hydroxylated cholest-5-en-ol as hydroxylated product, acetylated fragments as cholest-5-enacetate and piperidone-2-one present in visceral samples indicates structural part obtained from vecuronium bromide drug. Th ese metabolites studies makes the case studies highly informative. Beside this new method of extractions, TLC systems and colouring reagents are also explained.

Chromatography, Thin Layer/methods , Death , Female , Humans , Kinetics/methods , Mass Spectrometry/methods , Toxicity Tests/methods , Vecuronium Bromide/analysis , Vecuronium Bromide/metabolism , Vecuronium Bromide/toxicity , Viscera/analysis , Young Adult
Rev. cuba. farm ; 48(4)oct.-dic. 2014. ilus
Article in Spanish | LILACS, CUMED | ID: lil-748772


INTRODUCCIÓN: la Empresa Productora Roberto Escudero Díaz, llevó a cabo la reformulación de la crema de nitrato de miconazol al 2 por ciento, por incumplimiento de algunas especificaciones de calidad y contaminaciones microbiológicas de varios lotes industriales, por lo que hubo que realizar cambios mayores a la composición de la formulación registrada. OBJETIVO: determinar la estabilidad de la nueva formulación de nitrato de miconazol crema al 2 por ciento, para determinar su período de validez. MÉTODOS: se realizaron los estudios según las regulaciones vigentes. Se emplearon tres lotes elaborados a escala piloto, envasados en tubos comprimibles de aluminio por 25 g. Se emplearon como métodos analíticos una técnica por cromatografía líquida de alta resolución y una por cromatografía en capa delgada previamente validadas para estos propósitos. Se consideraron dos temperaturas de almacenamiento: 30 ± 2 ºC (vida de estante) y 40 ± 2 ºC (estabilidad acelerada). Se determinaron los parámetros: propiedades organolépticas, pH, área de extensibilidad, valoración, contenido de sustancias relacionadas y/o productos de degradación, y además se evaluó la calidad de la formulación desde el punto de vista microbiológico. RESULTADOS: desde el punto de vista químico, los lotes evaluados mostraron contenidos superiores al 98 por ciento de analito y niveles muy bajos de sustancias relacionadas, independientemente del lote y la temperatura de almacenamiento. No se detectaron manchas adicionales por cromatografía en capa delgada atribuibles a posibles productos de degradación. La extensibilidad mostró un decrecimiento normal debido a la estructuración progresiva del sistema, y el pH también disminuyó discretamente pero dentro de los límites propuestos. Además se comprobó la elevada estabilidad microbiológica del medicamento a los 12 meses. CONCLUSIONES: la crema es estable química, física y microbiológicamente a temperatura ambiente durante 12 meses, por lo que se propone este tiempo como período de validez provisional(AU)

INTRODUCTION: Roberto Escudero Diaz drug producing company is carrying out the reformulation of 2 percent miconazole nitrate cream due to non-compliance with some quality specifications and the microbiological contamination of several industrial batches, so it was required to make major changes in the registered formulation composition. OBJECTIVE: to determine the stability of the new 2 percent miconazol nitrate cream formulation to verify its validity period. METHODS: the studies followed the regulations in force. Three pilot-scaled batches, packed in 25 g aluminum tubes, were used. The analytical methods were high resolution liquid chromatography technique and thin layer chromatography, being both methods previously validated for these purposes. The selected storage temperatures were 30 ± 2 °C (shelf life) and 40 ± 2 ºC (accelerated stability). The estimated parameters included organoleptic properties, pH, extensibility area, titration, content of related substances and/or degradation products in addition to evaluating the quality of formulation from the microbiological viewpoint. RESULTS: from the chemical viewpoint, the evaluated batches showed contents over 98 percent of analyte and very low levels of related substances, regardless of batch and the storage temperature. The thin layer chromatography did not detect any additional stain attributed to possible degradation products. The extensibility showed normal decrease resulting from progressive structuring of the system and the pH also lowered within the set limits. The microbiological stability of the drug was proved to be high after 12 months. CONCLUSIONS: the cream was chemically, physically and microbiologically stable at room temperature for 12 months, so this is the term suggested as the temporary validity period(AU

Humans , Male , Female , Chromatography, High Pressure Liquid/methods , Chromatography, Thin Layer/methods , Skin Cream/therapeutic use , Miconazole/therapeutic use
Rev. cuba. plantas med ; 18(4): 513-521, oct.-dic. 2013.
Article in Spanish | LILACS | ID: lil-695046


Introducción: la corteza del fuste de Cedrela adorata L (cedro) es utilizada por la población para el tratamiento del asma, como vermífuga, antibacteriana, febrífuga y en cocimiento para dolores cuando se sufren caídas o golpes. Objetivo: identificar los metabolitos secundarios presentes en esta parte de la planta y evaluar su posible actividad antibacteriana. Métodos: se recolectó la corteza del fuste de Cedrela adorata. El material vegetal fue lavado, desinfectado, secado y seguidamente se procedió a su pulverización. Este polvo se utilizó en la elaboración de los diferentes extractos y tintura. La tintura obtenida se concentró y se fraccionó sucesivamente con n-hexano, cloroformo, acetato de etilo y agua. A estos extractos se les realizó el tamizaje fitoquímico, ensayos microbiológicos y cromatografía de capa fina. Resultados: las pruebas in vitro efectuadas a los extractos obtenidos a partir de la tintura 20 por ciento, demostraron que estos presentan actividad antibacteriana frente a Escherichia coli, Pseudomonas aeruginosa, Staphylococcus aureus, Shigella sp., Salmonella enterica y Enterobacter aerogene; destacándose los resultados obtenidos frente al Staphylococcus aureus, para el extracto hexánico de cedro. En estos extractos están presentes en mayor proporción alcaloides, triterpenos o esteroles, y quinonas, que son los responsables de esta actividad, lo cual se logró corroborar con la identificación de estos metabolitos secundarios mediante la cromatografía de capa fina y el tamizaje fitoquímico realizados. Conclusiones: mediante la cromatografía de capa fina y el tamizaje fitoquímico de los extractos se identificaron alcaloides, triterpenos o esteroles, y quinonas, que pueden ser los responsables de la actividad antibacteriana

Introduction: the stem bark of Cedrela adorata L (cedar) is used by the population to treat asthma, as vermifuge, antibacterial and febrifuge, and in the form of decoction to relieve the pain caused by falls or bumps. Objective: identify the secondary metabolites present in this part of the plant and evaluate their potential antibacterial activity. Methods: stem bark from Cedrela adorata was collected. The plant material was washed, disinfected, dried and pulverized. The powder obtained was used to make the various extracts and the tincture. The latter was concentrated and successively fractionated with n-hexane, chloroform, ethyl acetate and water. The extracts underwent phytochemical screening, microbiological assays and thin-layer chromatography. Results: in vitro tests of the extracts obtained from the 20 percent tincture showed antibacterial activity against Escherichia coli, Pseudomonas aeruginosa, Staphylococcus aureus, Shigella sp., Salmonella enterica and Enterobacter aerogen. Antibacterial activity of the hexanic cedar extract against Staphylococcus aureus was noteworthy. Alkaloids, triterpenes or sterols, and quinones, which are found in a large proportion in the extracts, are responsible for the above-mentioned antibacterial activity. Identification of these secondary metabolites was confirmed through thin-layer chromatography and phytochemical screening. Conclusions: the alkaloids, triterpenes or sterols, and quinones potentially responsible for antibacterial activity were identified through thin-later chromatography and phytochemical screening

Anti-Bacterial Agents/therapeutic use , Cedrela , Mass Screening/methods , Chromatography, Thin Layer/methods
Rev. cuba. farm ; 47(3): 300-314, jul.-sep. 2013.
Article in Spanish | LILACS | ID: lil-691239


Objetivo: evaluar los métodos cromatográficos para la estabilidad química del nitrato de miconazol en una nueva crema al 2 por ciento. Métodos: en primer lugar se aplicaron diferentes condiciones degradativas al nitrato de miconazol materia prima a fin de obtener los posibles productos de degradación del fármaco y evaluarlos por un método diseñado por cromatografía en capa delgada, el cual se validó para identificar productos de degradación en la crema. Se evaluó el desempeño del método oficial informado en la Farmacopea Británica 2010 por cromatografía líquida de alta resolución para la valoración del nitrato de miconazol en la crema, analizando su selectividad frente a los posibles productos de degradación. Ambos métodos cromatográficos fueron aplicados al análisis de muestras de crema procedentes de los tres lotes pilotos sometidos a estrés térmico durante 30 días. Resultados: ambos métodos mostraron elevada selectividad frente a los excipientes y los productos de degradación del fármaco. Se obtuvo degradación del nitrato de miconazol frente a hidrólisis ácida, termólisis y fotólisis y el límite de detección fue de 1 µg para cromatografía en capa delgada. No se mostró degradación del analito según los resultados cualitativos y cuantitativos en ninguno de los tres lotes analizados. Conclusiones: los métodos utilizados son válidos para el objetivo con el cual se proponen, por lo que pueden emplearse en el estudio de estabilidad química de las cremas de nitrato de miconazol al 2 por ciento

Objective: to assess the chromatographic methods for the chemical stability of a new 2 percent miconazol nitrate cream. Methods: various degradation conditions were firstly used in the raw material miconazole nitrate in order to obtain the possible degradation products of this drug and to evaluate them by thin layer chromatography-based method, which was validated to identify the degradation products in the new cream. The performance of the official method based on high resolution liquid chromatography and reported in British Pharmacopeia 2010 was evaluated, and its selectivity against the possible degradation products were also analyzed. Both chromatographic methods were applied to the analysis of cream samples from the three pilot batches under heat stress for 30 days. Results: the two methods showed high selectivity against excipients and degradation products of the drug. Miconazol nitrate was degraded against acid hydrolysis, thermolysis and photolysis, being the detection limit of 1 µg for the thin layer chromatography. No degradation of the analyte was observed in any of the three analyzed batches according to the qualitative and quantitative results. Conclusions: these methods are valid for the submitted objective, so they may be used in the chemical stability study of 2 percent miconazol nitrate creams

Humans , Chromatography, High Pressure Liquid/methods , Chromatography, Thin Layer/methods , Drug Stability , Miconazole/chemistry , Nitrates/chemistry