Photocatalytic degradation of microcystin-LR in aqueous solutions

AbstractIn this work, the photocatalytic degradation of aqueous microcystin-LR was studied using TiO2 and ZnO as photocatalysts. The process was optimised and characterised at the bench scale (200mL); both semiconductors exhibited a high degradation capacity at reaction times of 1min (degradation greater than 95%). The transient species that were observed indicate that the degradation occurs via the multiple hydroxylation and elimination of the labile peptide residues of the molecule. When photocatalysis was applied in a continuous treatment system (20–50L), the photocatalytic process exhibited a high degradation efficiency, which resulted in residual microcystin-LR concentrations that were less than 1μgL−1 (C0=5μgL−1)

A validated method using RP-HPLC for quantification of reserpine in the Brazilian tree Rauvolfia sellowii Müll. Arg. (Apocynaceae)

This study describes a simple, fast and reproducible method using RP-HPLC-UV, in a gradient system, for quantification of reserpine in Rauvolfia sellowii stem bark. The analysis were carried out on a C18 column; mobile phase was water and acetonitrile, and separations were carried out in 10 min, flow rate of 1.0 mL min-1, 25 ºC and 268 nm. The validation data showed that the method was specific, accurate, precise and robust. Results were linear over a range of 0.625-40.0 μg mL-1, and the mean recovery was 95.1%. The amount of reserpine found in the dried stem bark was 0.01% (m/m)

DETERMINAÇÃO DE GENISTEÍNA E GENISTINA POR ESPECTROFOTOMETRIA DE UV-VISÍVEL EM EXTRATOS SECOS DE SOJA UTILIZADOS COMO MATÉRIA-PRIMA EM FARMÁCIAS DE MANIPULAÇÃO

As isoflavonas são predominantemente encontradas em leguminosas e mais abundantes na soja. Estas são fitoestrógenos que mimetizam a ação do estradiol, porém com menor intensidade e tem sido utilizadas principalmente na terapia de reposição hormonal. Genisteína, daidzeína e gliciteína são as agliconas mais abundantes nos extratos de soja, ocorrendo também como glicosídeos. Neste contexto, a genisteína é considerada a isoflavona com maior atividade estrogênica, sendo que sua quantidade pode variar devido à influência de diversos fatores. Portanto, sua determinação em extratos de soja é importante uma vez que o conteúdo individual de isoflavonas pode ter implicações na atividade biológica. No presente trabalho foi avaliado o teor de genisteína+genistina em dez amostras de extratos secos de soja utilizados como matéria-prima em farmácias de manipulação. O método utilizado foi o doseamento por UV-VIS após reação com cloreto de alumínio. Os resultados demonstraram que há uma considerável variação na concentração de genisteína+genistina entre os diferentes lotes de extrato seco e que 62,5% das amostras apresentaram teores aproximados dos valores declarados nos certificados de análises, demonstrando a necessidade de padronização de isoflavonas individuais nestas matérias-primas. O método utilizado se mostrou simples e rápido para a avaliação dos teores de genisteína+genistina de extratos secos de soja comercializados em farmácias de manipulação

ANÁLISES QUÍMICA E BROMATOLÓGICAS DE SEMENTES E DE ÓLEO FIXO DE MELANCIA (CITRULLUS LANATUS, CUCURBITACEAE)

A semente de melancia apresenta importância econômica para o Brasil, sendo produzida em grande escala anualmente, entretanto, o que é usado se resume à polpa, sendo a semente descartada ou usada apenas em chás. Visando evitar desperdício e suplementar a alimentação, esse estudo traz informações acerca das propriedades nutricionais e químicas da semente de melancia e de seu óleo fixo. Os processamentos da semente resultaram em importantes descobertas como uma alta taxa de fibras (40,47%) e proteína (17,26%) na farinha, além de grande concentração de ácido linoleico, que é conhecido por reduzir a massa corporal. Ainda, sugere-se que novas análises acerca do óleo sejam feitas

Search for alkaloids on callus culture of Passiflora alata

Preliminary work on Passiflora alata leaves failed to detect harmane alkaloids using LC. The aim of this work was to investigate the production of harmane alkaloids through the cell culture of P. alata, inducing its precursor (L-tryptophan). The leaf explants presented satisfactory results after disinfection, and the callus formation was initiated in MS media with adequate quantities of phytohormones. Sixty days after inoculation, calli were inoculated in the optimized semi-solid MS media, with and without the addition of L-tryptophan (50, 100, 200 mg/L) and kept in standard conditions for 90 days. Calli were collected on days 6, 16, 26, 36, and 90, followed by acid-base extraction, and analysed by LC. The results showed an absence of harmane, harmin, harmol, harmalol, and harmaline. With L-tryptophan feeding, two peaks were detected, collected and analysed through positive mode electrospray [ESI(+)-MS] and sequential analysis in tandem ESI(+)-MS/MS. The spectra obtained were very similar, with a repetition of the more intense ions, and consecutive loss of 68 Da units, attributed to the heterocycle pyrazole. It appeared that this transformation was not related to any enzymatic pathway previously described for the plant from L-tryptophan, and the biosynthesis of β-carboline alkaloids in callus culture of P. alata were not observed in this work.As folhas de varias espécies de Passiflora são utilizadas como ansioliticas e sedativas. Passiflora alata Curtis, Passifloraceae consta em três edições da farmacopéia brasileira, porem não há muitos estudos sobre sua composição química. No passado, enfatizava-se a ação conjunta de alcalóides e flavonóides. Em trabalho anterior, não foi detectada a presença de alcalóides harmanicos através de CLAE. Assim, decidiu-se investigar a produção dos mesmos através de cultivo celular, introduzindo seu precursor metabólico L-triptofano. Os explantes foliares apresentaram resultados satisfatorios para germinação apos assepsia, e a formação de calo foi iniciada em meio MS com quantidades adequadas de fitohormonios, previamente determinadas. Sessenta dias após a inoculação os calos foram repicados para meio semi-solido com e sem L-triptofano (50, 100, 200 mg/L), mantidos por 90 dias em condições padrão. Amostras foram coletadas com 6, 16, 26, 36, e 90 dias, realizada extração acido-base e o extrato analisado por CLAE. Os resultados mostraram a ausência de harmana, harmina, harmol, harmalol e harmalina. Dois picos presentes nas amostras com L-triptofano foram coletados e analisados através de espectrometria de massas, electrospray modo positiva [ESI(+)-MS] e analise em tandem ESI(+)-MS/MS. Os espectros correspondentes foram similares, mostrando a perda consecutiva de 68 Da, atribuídos ao pirazol. Este fato aponta para uma transformação não enzimática, não relacionada a uma biossintese previamente descrita para alcalóides β-carbolínicos.90191

Chemical composition, larvicidal and cytotoxic activity of Annona salzmannii (Annonaceae) seed oil

The seed oil of Annona salzmannii A. DC. was analyzed by GC-MS and 1 H qNMR, revealing a mixture of unsaturated (80.5%) and saturated (18.7%) fatty acids. Linoleic (45.3%) and oleic (33.5%) acid were the major unsaturated fatty acids identified, while palmitic acid (14.3%) was the major saturated fatty acid. The larvicidal effects of A. salzmannii seed oil were evaluated against third-instar larvae of Aedes aegypti (Linn.). The oil exhibited moderate larvicidal activity, with aLC50 of 569.77 ppm (95% CI = 408.11 to 825.88 ppm). However, when the cytotoxic effects of the oil were evaluated, no expressive antiproliferative effects were observed in tumor cell lines B16-F10 (mouse melanoma), HepG2 (human hepatocellular carcinoma), K562 (human chronic myelocytic leukemia), HL-60 (human promyelocytic leukemia), and non-tumor cell line PBMC (peripheral blood mononuclear cells), with IC50 values > 50 μg·mL-1. This is the first study to evaluate the chemical composition, larvicidal and cytotoxic activity of A. salzmannii seed oil

GRAPE JUICE QUALITY CONTROL BY MEANS OF 1

This work shows the application of ¹H NMR spectroscopy and chemometrics for quality control of grape juice. A wide range of quality assurance parameters were assessed by single ¹H NMR experiments acquired directly from juice. The investigation revealed that conditions and time of storage should be revised and indicated on all labels. The sterilization process of homemade grape juices was efficient, making it possible to store them for long periods without additives. Furthermore, chemometric analysis classified the best commercial grape juices to be similar to homemade grape juices, indicating that this approach can be used to determine the authenticity after adulteration

Applying liquid chromatography-tandem mass spectrometry to assess endodontic sealer microleakage

The objective of this study was to describe a new method for the quantitative analysis of a microleakage of endodontic filling materials. Forty extracted single-rooted teeth were randomly divided into three experimental groups. After root canal shaping, the experimental groups were filled using the lateral condensation technique with the Epiphany system (G1), with gutta-percha + Sealapex (G2), and with gutta-percha + AH Plus (G3). Each root was mounted on a modified leakage testing device, and caffeine solution was used as a tracer (2000 ng mL-1, pH 6.0), applied in the coronal direction towards the tooth apex, creating a hydrostatic pressure of 2.55 kPa. Presence of caffeine in the receiving solution was measured after 10, 30, and 60 days, using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). None of the groups presented microleakage at 10 days. At 30 days, G2 and G3 showed similar infiltration patterns (means: 16.0 and 13.9 ng mL-1, respectively), whereas G1 showed significantly higher values (mean: 105.2 ng mL-1). At 60 days, leakage values were 182.6 ng mL-1for G1, 139.0 ng mL-1 for G2, and 53.5 ng mL-1 for G3. AH Plus showed the best sealing ability and HPLC-MS/MS showed high sensitivity and specificity for tracer quantification