Degradação Fotocatalítica De Pesticida Organofosforado De Efluente Agrícola Por Tio2 Imobilizado Sob Radiação Solar

This paper describes solar heterogeneous photocatalysis using immobilized TiO2 applied in the treatment of agricultural waste resulting from the application of commercial formulations of methyl parathion. The disappearance of the insecticide, as well as the formation of its metabolite, was monitored by high-performance liquid chromatographytandem mass spectrometry (LC-MS/MS), while mineralization efficiency was monitored by measurements of total organic carbon (TOC). Toxicity studies were performed using the microcrustacean Artemia salina. The TOC removal efficiency by photocatalytic process was 48.5%. After 45 minutes of treatment, the removal efficiency of methyl parathion was 90%, being completely mineralized at the end of treatment. The formation and removal of the metabolite methyl paraoxon was observed during the photocatalytic process. The photocatalytic treatment resulted in increased microcrustacean mobility, indicating a reduction of acute toxicity. © 2016, Institute for Environmental Research in Hydrographic Basins (IPABHi). All rights reserved.11477878

Methods Of Extraction And/or Concentration Of Compounds Found In Biological Fluids For Subsequent Chromatographic Determination [métodos De Extração E/ou Concentração De Compostos Encontrados Em Fluidos Biológicos Para Posterior Determinação Cromatográfica]

When organic compounds present in biological fluids are analysed by chromatographic methods, it is generally necessary to carry out a prior sample preparation due the high complexity of this type of sample, especially when the compounds to be determinated are found in very low concentrations. This article describes some of the principal methods for sample preparation in analyses of substances present in biological fluids. The methods include liquid-liquid extraction, solid phase extraction, supercritical fluid extraction and extraction using solid and liquid membranes. The advantages and disadvantages of these methods are discussed.2416876Drummer, O.H., (1999) J. Chromatogr. B., 733, p. 27Polettini, A., (1999) J. Chromatogr. 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Antitumoral, Antioxidant And Antimicrobial Molecules From Combretum Rupicola

This investigation describes the anticancer, antioxidant and antimicrobial properties of the extracts of Combretum rupicola, a native plant from Northeast of Brazil. Methanolic, ethyl acetate and chloroform extracts from leaves of C. rupicola were evaluated in relation to their potential in inhibiting the cell growth and cytotoxic properties against nine human cancer cell lines (MCF-7, NCI-ADR/RES, OVCAR-3, PC-3, HT-29, NCIH460, 786-O, UACC-62, K-562). In addition, antioxidant activity of these extracts was measured using DPPH as radical scavenging assay and the antimicrobial activities against nine pathogens were tested by agar diffusion method. Preliminary results showed that the this plant demonstrates to have moderate activity against bacteria but, on the other side, the extracts showed significant anticancer activitiesagainst four cell lines and the most significant activity was observed against MCF-7 (65.9 μg mL-1), highest inhibitory concentration IC50 0.22 μg mL-1 for antioxidant activity. These founds are the first scientific reports on secondary metabolites with biological activities of C. rupicola, suggesting the potential of this botanic species for pharmaceutical industry.41B422B428Butler, M.S., The role of natural product chemistry in drug Discovery (2004) J of Nat Prod, 67 (12), pp. 2141-2153Ripa, F.A., Nahar, L., Haque, M., Islam, M.M., Antibacterial, Cytotoxic and Antioxidant Activity of Crude Extract of Marsilea Quadrifolia (2009) Eur J of Scien Res, 33 (1), pp. 123-129Santos, S.N., Oliveira, L.K.X., Melo, I.S., Velozo, E.S., Roque, M.R.A., Antifungal activity of bacterial strains from the rhizosphere of Stachytarpheta crassifólia (2011) Afri J of Biot, 10 (25), pp. 4996-5000Pettit, G.R., Singh, S.B., Niven, M.L., Hamel, E., Schmidt, J.M., Isolation, Structure, and Synthesis of Combretastatins A-1 and B- 1, Potent New Inhibitors of Microtubule Assembly, Derived from Combretum caffrum (1987) J of Nat Prod, 50 (1), pp. 119-131Tan, F.X., Shi, S.H., Zhong, Y., Gong, X., Wang, Y.G., Phylogenetic relationships of Combretoideae (Combretaceae) inferred from plastid, nuclear gene and spacer sequences (2002) J of Plant Res, 115, pp. 475-481Fyhrquist, P., Mwasumbi, L., Haeggstrom, C.A., Vuorela, H., Hiltunen, R., Vuorela, P., Microscopic diagnosis of tumors of the central nervous system by phase contrast microscopy (2002) J of Ethnoph, 79, pp. 169-177McGaw, L.J., Rabe, T., Sparg, S.G., Jager, A.K., Eloff, J.N., Van Staden, J., An investigation on the biological activity of Combretum species (2001) J of Ethnoph, 75, pp. 45-50Ridley, H.N., Notes on the Botany of Fernando Noronha (1890) Botany, 27 (181), pp. 1-95Eloff, J.N., Katerere, D.R., McGaw, L.J., The biological activity and chemistry of the southern African Combretaceae (2008) J of Ethnoph, 119, pp. 686-699Grammer, A., Antibiotic sensitivity and Assay test (1976) Collins CH and Lyne PM, Eds. 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Density Of Planting And Age Of Phillanthus Amarus - Genotype Unicamp/ Cpqba-14 On The Productivity Of Phyllanthin [densidade De Plantio E Idade De Colheita De Quebra-pedra [phyllanthus Amarus (schumach. & Thonning) Genótipo Unicamp-cpqba 14] Na Produtividade De Filantina]

The effect of planting density and age of Phyllanthus amarus- genotype CPQBA-14, on the content and productivity of phyllanthin were evaluated. The experimental design was randomized blocks in factorial scheme 4 × 6, with five replicates, consisting of 4 treatments of planting density (400.000 pl ha-1; 200.000 pl ha-1; 100.000 pl ha-1 and 66667.68 pl ha-1) with six ages of plants (30, 45, 60, 75, 90 and 105 days after transplanting (DAT)). Data were subjected to analysis of variance and regression (P>0.005). For phyllanthin content independent and significant effects of harvest and planting density were observed. The phyllanthin contents increased with plant age, peaking at 105 DAT, with a content of 11.52 g kg-1. The estimated population density that provided the high phyllanthin contents (8.66 g kg-1) was at 299.860 pl ha-1. The productivity of phyllanthin showed significant interaction between planting density and plants ages. It was observed during the plant growth, the treatments with 200 and 400.000 pl ha -1 had the highest yield of phyllanthin (39.3 and 37.8 kg ha-1) with 95.17 and 97.12 DAT, respectively. We conclude that the proper spacing for best spatial arrangement of the cultivation is 299.860 pl ha-1 for the yield of 3974.19 kg (dry weight leaf) × 0.00866 kg (phyllanthin contents) = 34.416 kg ha-1 of phyllanthin with harvest scheduled at 97 DAT.SPECIAL ISSUE633641Barbosa Filho, J.M., Lignanas, neolignanas e seus análogos (2000) Farmacognosia: Da planta ao medicamento, pp. 481-498. , In: SIMÕES, C.M. OSCHENKEL, E.P., GOSMANN, G., MELLO, J.C.P.MENTZ, L.A.PETROVICK, P. R, Porto Alegre: Ed. UFRGS/UFSC, 3°edFernandes, L.A., Furtini Neto, A.D., Fonseca, F.C., Ribeiro Do Vale, F., Crescimento inicial, níveis críticos de fósforo e frações fosfatadas em espécies florestais (2000) Pesquisa Agropecuária Brasileira, Brasília, 35 (6), pp. 1191-1198Herbert, R.B., (1989) The biosynthesis of secondary metabolites, p. 231. , 2a EdGobbo-Neto, L., Lopes, N.P., Plantas medicinais: Fatores de influência no conteúdo de metabólitos secundários (2007) Química Nova, 30 (2), pp. 374-381Gotlieb, O., Kaplan, M.A.C., de Borin, M.R.M.B., (1996) Biodiversidade: Um enfoque químico-biológico, p. 268. , Rio de Janeiro: Editora UFRJMann, J., (1994) Chemical aspects of biosynthesis, p. 44. , New York: Oxford Science publicationsMarschner, H., (1995) Mineral nutrition of higher plants, p. 850. , London: Academic PressMarchese, J.A., (1999) Produção e detecção de artemisinina em plantas de Artemisia annua L, p. 97. , submetidas a estresses abióticos., (Dissertação de mestrado em Ciências Biológicas). Instituto de Biologia, UNICAMP, Campinas-SPMarchese, J.A., Figueira, G.M., O uso de tecnologias pré e pós-colheita e boas práticas agrícolas na produção de plantas medicinais e aromáticas (2005) Revista Brasileira de Plantas Medicinais, Botucatu-SP, 7 (3), pp. 86-96Mehrotra, R., Rawat, S., Kulshreshtha, D.K., Goyal, P., Patnaik, G.K., Dhawan, B.N., In vitro effect of Phyllanthus amarus on hepattis B virus (1991) Indian Journal of Medicinal Researches, 93, pp. 71-73Murugaiyah, V., Chan, K.T., Determination of four lignans in Phyllanthus niruri L. by a simple highperformance liquid chromatography method with fluorescence detection (2007) Journal of Chromatography Archives, 11 (54), pp. 198-204Notka, F., Meier, G.R., Wagner, R., Inhibtion of wildtype human immunodeficiency virus and reverse transcriptas or-resistant variants by Phyllanthus amarus (2003) Antiviral research, 53, pp. 175-186Raí, V., Khatoon, S., Bisht, S.S., Menhotra, S., Effect of cadmium on growth, ultramorphology of leaf and secondary metabolites of Phyllanthus amarus Shum & Thonn (2005) Chemosphere, 61, pp. 1644-1650van Raij, B., Andrade, J.C., Cantarella, H., Quaggio, J.A., (2001) Análise química para avaliação da fertilidade de solos tropicais, p. 285. , (Ed.), Campinas: Instituto AgronômicoSalomé, J.R., (2007) Análise fitoquimica dos principios ativos, filantina, hipofilantina e nirantina da quebra-pedra (Phyllanthus amarus Shumach & Thonn) sob condições de deficit hídrico, p. 93. , Dissertação (Mestrado em Fisiologia e Bioquímica de Plantas)-Escola Superior de Agricultura "Luiz de Queiroz". Universidade de São Paulo, Piracicaba, SPSilva, M.J., Sales, M.F., O gênero Phyllanthus L. (Phyllantheae-Euphorbiaceae Juss.) no bioma Caatinga do estado de Pernambuco-Brasil (2004) Rodriguésia, 55 (84), pp. 101-126Syamsundar, K.V., Singh, B., Thakur, R.S., Hussain, A., Kiso, A., Hikino, H., Antiepatotoxic principles of Phyllanthus niruri Herb (1985) Journal of Ethnopharmacology, 14, pp. 41-44Taiz, L., Zeiger, E., (2004) Fisiologia Vegetal, p. 719. , SANTARÉM, E.R. (Tradução), 3. ed, Porto Alegre: ArtmedTeratomo, J.R.S., Oliveira, R.F., Santos, S., Rehder, V.L.G., Avaliação dos teores das lignanas filantina, hipofilantina e niratina em quebra-pedra (Phyllanthus amarus Schumach. & Thonn.) sob diferentes condições de deficiência hídrica (2008) Revista Brasileira de Plantas Medicinais, 10 (4), pp. 67-7

Liquid-liquid extraction combined with high performance liquid chromatography-diode array-ultra-violet for simultaneous determination of antineoplastic drugs in plasma

A liquid-liquid extraction (LLE) combined with high-performance liquid chromatography-diode array detection method for simultaneous analysis of four chemically and structurally different antineoplastic drugs (cyclophosphamide, doxorubicin, 5-fluorouracil and ifosfamide) was developed. The assay was performed by isocratic elution, with a C18 column (5 µm, 250 x 4.6 mm) and mobile phase constituted by water pH 4.0- acetonitrile-methanol (68:19:13, v/v/v), which allowed satisfactory separation of the compounds of interest. LLE, with ethyl acetate, was used for sample clean-up with recoveries ranging from 60 to 98%. The linear ranges were from 0.5 to 100 µg mL-1, for doxorubicin and 1 to 100 µg mL-1, for the other compounds. The relative standard deviations ranged from 5.5 to 17.7%. This method is a fast and simple alternative that can be used, simultaneously, for the determination of the four drugs in plasma, with a range enabling quantification of the drugs in pharmacokinetics, bioequivalence and therapeutic drug-monitoring studies.<br>Um método de extração líquido-líquido (ELL) combinado com cromatografia líquida de alta eficiência-detector de arranjo de diodos foi desenvolvido para análise simultânea de quatro fármacos antineoplásicos quimicamente e estruturalmente diferentes (ciclofosfamida, doxorrubicina, fluoruracila e ifosfamida). O estudo foi realizado sob condições isocráticas, com coluna C18 (5µm, 250 x 4.6 mm) e fase móvel constituída por água pH 4.0-acetonitrila-metanol (68:19:13, v/v/v), que permitiu separação satisfatória dos analitos de interesse. A ELL, com acetato de etila, foi utilizada para limpeza da amostra, com recuperação variando de 60 a 98%. As faixas foram lineares de 0,5 a 100 µg mL-1 para doxorrubicina e 1 a 100 µg mL-1 para os outros compostos. O desvio padrão relativo variou de 5,5 a 17,7%. Este método é uma alternativa rápida e simples que pode ser usado, simultaneamente, para a determinação dos quatro fármacos em plasma, com uma faixa que permite quantificá-los em estudos de farmacocinética, bioequivalência e monitorização terapêutica

Single gas chromatography method with nitrogen phosphorus detector for urinary cotinine determination in passive and active smokers

Nicotine is a major addictive compound in cigarettes and is rapidly and extensively metabolized to several metabolites in humans, including urinary cotinine, considered a biomarker due to its high concentration compared to other metabolites. The aim of this study was to develop a single method for determination of urinary cotinine, in active and passive smokers, by gas chromatography with a nitrogen phosphorus detector (GC-NPD). Urine (5.0 mL) was extracted with 1.0 mL of sodium hydroxide 5 mol L-1, 5.0 mL of chloroform, and lidocaine used as the internal standard. Injection volume was 1 &#956;L in GC-NPD. Limit of quantification was 10 ng mL-1. Linearity was evaluated in the ranges 10-1000 ng mL-1 and 500-6000 ng mL-1, with determination coefficients of 0.9986 and 0.9952, respectively. Intra- and inter-assay standard relative deviations were lower than 14.2 %, while inaccuracy (bias) was less than +11.9%. The efficiency of extraction was greater than 88.5%. Ruggedness was verified, according to Youden's test. Means of cotinine concentrations observed were 2,980 ng mL-1 for active smokers and 132 ng mL-1, for passive smokers. The results revealed that satisfactory chromatographic separation between the analyte and interferents was obtained with a ZB-1 column. This method is reliable, precise, linear and presented ruggedness in the range evaluated. The results suggest that it can be applied in routine analysis for passive and active smokers, since it is able to quantify a wide range of cotinine concentrations in urine.<br>A nicotina é uma substância presente no cigarro capaz de causar dependência, sendo biotransformada em vários metabólitos nos seres humanos, dentre eles a cotinina urinária, que é considerada um indicador biológico de exposição à nicotina, devido a suas altas concentrações, comparado a outras matrizes. Assim, o objetivo deste estudo foi desenvolver um único método para determinação de cotinina urinária, em amostras de urina de fumantes ativos e passivos, através de cromatografia em fase gasosa com detector de nitrogênio- fósforo (CG-DNF). Para o preparo de amostras foram utilizados 5 mL de urina, 1 mL de hidróxido de sódio 5 mol L-1, 5 mL de clorofórmio, tendo como padrão interno a lidocaína. Na faixa de concentrações de 10-1000 ng mL-1 e 500- 6000 ng mL-1, o coeficiente de determinação foi 0,9986 e 0,9952, respectivamente e, o limite de quantificação foi 10 ng mL-1. A precisão intra- e interensaio apresentou desvio padrão relativo (%) menor que 14,2% e a inexatidão foi menor que +11,9%, com uma eficiência de extração de 88,5%. O método apresentou robustez, de acordo com o teste de Youden. As concentrações médias de cotinina observadas foram 2980 ng mL-1, para fumantes ativos e 132 ng mL-1, para fumantes passivos. Os resultados sugerem que o método é confiável, preciso, linear e apresentou robustez, na faixa avaliada, podendo ser aplicado na rotina para análises de amostras de fumantes ativos e passivos, pois é capaz de quantificar uma ampla faixa de concentrações de cotinina urinária