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101.
102.
Ultrasound‐assisted extraction method for the simultaneous determination of emerging contaminants in freshwater sediments
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Diana Nara Ribeiro de Sousa Guilherme Martins Grosseli Antonio Aparecido Mozeto Renato Lajarim Carneiro Pedro Sergio Fadini 《Journal of separation science》2015,38(19):3454-3460
Sediments are the fate of several emerging organic contaminants, such as pharmaceuticals, personal care products and hormones, and therefore an important subject in environmental monitoring studies. In the present work, a simple and sensitive method was developed, validated and applied for the simultaneous extraction of atenolol, caffeine, carbamazepine, diclofenac, ibuprofen, naproxen, propranolol, triclosan, estrone, 17‐β‐estradiol and 17‐α‐ethinylestradiol using ultrasound‐assisted extraction from freshwater sediment samples followed by solid‐phase extraction clean‐up and liquid chromatography with tandem mass spectrometry detection. The solvent type and extraction pH were evaluated to obtain the highest recoveries of the compounds. The best method shows absolute recoveries between 54.0 and 94.4% at 50 ng/g concentration. The method exhibits good precision with relative standard deviation ranging from 1.0–16%. The detection and quantification limits ranged from 0.006–0.067 and 0.016–0.336 ng/g, respectively. The developed method was successfully applied to freshwater sediment samples collected from different sites in Jundiaí River basin of São Paulo State, Brazil. The compounds atenolol, caffeine, propranolol and triclosan were detected in all the sampling sites with concentrations of 13.8, 41.0, 28.5 and 176 ng/g, respectively. 相似文献
103.
Gabriela Furlan Giordano Luis Carlos Silveira Vieira Angelo Luiz Gobbi Renato Sousa Lima Lauro Tatsuo Kubota 《Analytica chimica acta》2015
An integrated platform was developed for point-of-use determination of ethanol in sugar cane fermentation broths. Such analysis is important because ethanol reduces its fuel production efficiency by altering the alcoholic fermentation step when in excess. The custom-designed platform integrates gas diffusion separation with voltammetric detection in a single analysis module. The detector relied on a Ni(OH)2-modified electrode. It was stabilized by uniformly depositing cobalt and cadmium hydroxides as shown by XPS measurements. Such tests were in accordance with the hypothesis related to stabilization of the Ni(OH)2 structure by insertion of Co2+ and Cd2+ ions in this structure. The separation step, in turn, was based on a hydrophobic PTFE membrane, which separates the sample from receptor solution (electrolyte) where the electrodes were placed. Parameters of limit of detection and analytical sensitivity were estimated to be 0.2% v/v and 2.90 μA % (v/v)−1, respectively. Samples of fermentation broth were analyzed by both standard addition method and direct interpolation in saline medium based-analytical curve. In this case, the saline solution exhibited ionic strength similar to those of the samples intended to surpass the tonometry colligative effect of the samples over analyte concentration data by attributing the reduction in quantity of diffused ethanol vapor majorly to the electrolyte. The approach of analytical curve provided rapid, simple and accurate analysis, thus contributing for deployment of point-of-use technologies. All of the results were accurate with respect to those obtained by FTIR method at 95% confidence level. 相似文献
104.
105.
Luís G. Dias Cédric Sequeira Ana C.A. Veloso Mara E.B.C. Sousa António M. Peres 《Analytica chimica acta》2014
Overconsumption of sugar-sweetened beverages may increase the risk of health problems and so, the evaluation of their glycemic load and fructose-intolerance level is essential since it may allow establishing possible relations between physiologic effects of sugar-rich beverages and health. In this work, an electronic tongue was used to accurately classify beverages according to glycemic load (low, medium or high load) as well to their adequacy for people suffering from fructose malabsorption syndrome (tolerable or not): 100% of correct classifications (leave-one-out cross-validation) using linear discriminant models based on potentiomentric signals selected by a meta-heuristic simulated annealing algorithm. These results may be partially explained by the electronic tongue’s capability to mimic the human sweetness perception and total acid flavor of beverages, which can be related with glycemic load and fructose-intolerance index. Finally, the E-tongue was also applied to quantify, accurately, healthy and sensory indexes using multiple linear regression models (leave-one-out cross-validation: Radj > 0.99) in the following dynamic ranges: 4.7 < glycemic load ≤ 30; 0.4 < fructose intolerance index ≤ 1.5; 32 < sweetness perception < 155; 1.3 < total acid flavor, g L−1 < 8.3; and, 5.8 < well-balanced flavor ≤ 74. So, the proposed electronic tongue could be used as a practical, fast, low-cost and green tool for beverage’s healthy and sensory evaluation. 相似文献
106.
Thayana da C. Alves Mariele R. S. Gonçalves Francyne C. S. Correia Virgínia C. da Silva Paulo T. de Sousa Jr. Mário G. de Carvalho Raimundo Braz‐Filho Evandro L. Dall'Oglio 《Helvetica chimica acta》2014,97(11):1469-1474
From the hexane and MeOH extracts of Annona coriacea Mart . (Annonaceae) seeds, two novel acetogenins, coriapentocins A and B ( 1 and 2 , resp.) were isolated. The known acetogenin bullacin ( 3 ) was also isolated from the hexane extract. The structures of compounds 1 – 3 were elucidated by NMR and MS analysis, and relative configurations were established by comparison with literature data. 相似文献
107.
Everaldo F. Santos-FilhoJokderléa C. Sousa Natércia M.M. BezerraPaulo H. Menezes Roberta A. Oliveira 《Tetrahedron letters》2011,52(41):5288-5291
The homocoupling reaction between potassium aryl trifluoroborates containing different functionalities promoted by a catalytic amount of Pd(OAc)2 is described. The methodology uses water as a solvent under aerobic conditions to give the corresponding biaryl compounds in good yields. 相似文献
108.
G.D. Saraiva J.A. Lima Jr.F.F. de Sousa P.T.C. FreireJ. Mendes Filho A.G. Souza Filho 《Vibrational Spectroscopy》2011,55(1):101-106
Temperature dependent Raman study of l-ascorbic acid has been performed from 15 to 418 K. Changes in the wavenumber vs. temperature plots for some internal modes were interpreted as conformational molecular change and the discontinuity in the wavenumber vs. temperature plots along with the appearance of a new vibrational mode in the temperature range 200-270 K suggests that l-ascorbic acid undergoes a structural phase transition. For temperatures higher than 300 K, no relevant modification was observed on the Raman spectra thus indicating a stable structure at high temperatures. Additionally, a correlation between OH stretching wavenumber and the behavior of hydrogen bond is also made. 相似文献
109.
The use of therapeutics based on plasmid DNA (pDNA) relies on procedures that efficiently produce and purify the supercoiled (sc) plasmid isoform. Several chromatographic methods have been applied for the sc plasmid purification, but with most of them it is not possible to obtain the required purity degree and the majority of the supports used present low capacity to bind the plasmid molecules. However, the chromatographic monolithic supports are an interesting alternative to conventional supports due to their excellent mass transfer properties and their high binding capacity for pDNA. The separation of pDNA isoforms, using short non-grafted monolithic column with CarbonylDiImidazole (CDI) functional groups, is described in the current work. The effect of different flow rates on plasmid isoforms separation was also verified. Several breakthrough experiments were designed to study the effect of different parameters such as pDNA topology and concentration as well as flow rate on the monolithic support binding capacity. One of the most striking results is related to the specific recognition of the sc isoform by this CDI monolith, without flow rate dependence. Additionally, the binding capacity has been found to be significantly higher for sc plasmid, probably because of its compact structure, being also improved when using feedstock with increased plasmid concentrations and decreased linear velocity. In fact, this new monolithic support arises as a powerful instrument on the sc pDNA purification for further clinical applications. 相似文献
110.
Serrano A Sousa MM Hallett J Lopes JA Oliveira MC 《Analytical and bioanalytical chemistry》2011,401(2):735-743
A new analytical approach based on high-performance liquid chromatography with diode array detector (HPLC-DAD) and multivariate
data analysis was applied and assessed for analyzing the red dye extracted from cochineal insects, used in precious historical
textiles. The most widely used method of analysis involves quantification of specific minor compounds (markers), using HPLC-DAD.
However, variation in the cochineal markers concentration, use of aggressive dye extraction methods and poor resolution of
HPLC chromatograms can compromise the identification of the precise insect species used in the textiles. In this study, a
soft extraction method combined with a new dye recovery treatment was developed, capable of yielding HPLC chromatograms with
good resolution, for the first time, for historical cochineal-dyed textiles. After principal components analysis (PCA) and
mass spectrometry (MS), it was possible to identify the cochineal species used in these textiles, in contrast to the accepted
method of analysis. In order to compare both methodologies, 7 cochineal species and 63 historical cochineal insect specimens
were analyzed using the two approaches, and then compared with the results for 15 historical textiles in order to assess their
applicability to real complex samples. The methodology developed here was shown to provide more accurate and consistent information
than the traditional method. Almost all of the historical textiles were dyed with Porphyrophora sp. insects. These results emphasize the importance of adopting the proposed methodology for future research on cochineal
(and related red dyes). Mild extraction methods and HPLC-DAD/MSn analysis yield distinctive profiles, which, in combination with a PCA reference database, are a powerful tool for identifying
red insect dyes. 相似文献