Fatty acids profile of pulp and nuts of brazilian fruits

Fruits and nuts from the North and Northeast regions of Brazil were collected to determine the fatty acid profile of their oils. The species studied were Brazil (Bertholletia excelsa H. B. K.), Mucaja (Couma rigida M.), Inaja (Maximiliana maripa D.), Jenipapo (Genipa Americana L.), and Buriti (Mauritia flexuosa L.) nuts. Fatty acid methyl esters were analyzed by gas chromatography with flame ionization detection (GC-FID). Brazil nut major fatty acid was 18:3n-3 (alpha-linolenic acid), and Buriti nut had approximately 23 times more 18: 3n-3 than the pulp. Mucaja nut presented high content of 12: 0 (lauric acid) and 16: 0 (palmitic acid), and Mucaja pulp showed significant levels of 18: 2n-6 (linoleic acid). Considering the PUFA (polyunsaturated fatty acid) sum values, almost all fruits and nuts analyzed presented very high levels of these compounds. Regarding n-6/n-3 ratio, only Brazil Nut, Buriti Nut, Inaja pulp, and Jenipapo pulp corresponded to the desired profile. These Brazilian fruits and nuts could be of potential interest due to their high nutritive value and lipid content.31495095

Use of multivariate statistical techniques to optimize the simultaneous separation of 13 phenolic compounds from extra-virgin olive oil by capillary electrophoresis

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Characterization of phenolic compounds in olive oil has not been achieved as yet, owing to the complexities of their chemical structures and analytical matrix. The aim of this work is to optimize and validate a method for simultaneous separation and quantification of 13 phenolic compounds from extra-virgin olive oil: tyrosol, hydroxytyrosol, oleuropein glycoside, ferrulic acid, p-coumaric acid, cinnamic acid, p-hydroxybenzoic acid, gallic acid, caffeic acid, luteolin, apigenin, vanillic acid and 3,4-dihydroxybenzoic acid. A statistical central composite design, response surface analysis and the simultaneous optimization method of Derringer and Suich were used to separate all the peaks. These multivariate procedures were efficient in determining the optimal separation condition, using five peak-pair resolutions and runtime as responses. The optimized method employed a fused-silica capillary of 50 mu m i.d. x 60 cm effective length with extended light path, 50 mmol L(-1) boric acid electrolyte, 10.2 pH, 25 degrees C, injection of 50 mbar for 25 s with application of reverse voltage (-30 kV for 5 s) before setting the running voltage (+30 kV) with detection at 210 nm and a run time of 12 min. Peak resolutions are found to be very sensitive to pH values outside the 10.15-10.25 range but acceptable electropherograms can be obtained for a wide range of boric acid concentrations within this pH interval. (c) 2010 Published by Elsevier B.V.834SI11811187Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)FAPESP [08/57548-0

Phytosterols and tocopherols content of pulps and nuts of Brazilian fruits

Fruits and nuts from the North and Northeast regions of Brazil were collected to determine their phytosterol and tocopherol content. The species studied were Cotia nut (Aptandra spruceana M.), Brazil nut (Bertholletia excelsa H.B.K.), Mucaja (Couma rigida M.), Red Acai (Euterpe oleracea M.), Inaja (Maximiliana maripa D.), Jenipapo (Genipa Americana L), Buriti (Mauritia flexuosa L) and Uxi (Endopleura uchi C.). Phytosterols were analyzed by GC-FID using beta-cholestanol as an internal standard, while tocopherols were determined by RP-HPLC-DAD. The pulps of Mucaja (26-236 mg 100 g(-1)), Inaja (119-285 mg 100 g(-1)) and Jenipapo (216 mg 100 g(-1)) showed the highest total phytosterol contents. Considering alpha-tocopherol equivalents, the pulps of Buriti (346.72 mu g g(-1)) and Uxi (200.92 mu g g(-1)) contained the highest vitamin E activity. Therefore, the results indicate that these fruits and nuts have great potential to be cultivated and marketed as alternative dietary sources for these bioactive compounds. (C) 2010 Elsevier Ltd. All rights reserved.4361603160

Optimization of capillary zone electrophoresis separation and on-line preconcentration of 16 phenolic compounds from wines produced in South America

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)A capillary zone electrophoresis method was optimized to simultaneously separate 16 phenolic compounds present in wines, as well as to evaluate sample on-line preconcentration for detectability improvement. The separated compounds were narirutin, (-)-epicatechin, (+)-catechin, rutin, kaempferol, myricetin, quercetin, morin, trans-resveratrol, cinnamic acid, ferulic acid, p-coumaric acid, vanillic acid, caffeic acid, gallic acid, and 3,4-dihydroxybenzoic acid. The optimized separation condition was 175 mmol L-1 boric acid at pH 9.0 and capillary of 50 mu m x 68 cm (60 cm effective length). The injection mode showing the greatest detectability (20 fold improvement) was hydrodynamic injection at 50 mbar for 30 s, followed by voltage inversion (-20 kV for 5 s) before the electrophoretic run. The method was validated and applied with success in a total of 23 samples of red, white, and rose wines. The developed method showed excellent applicability due to the simple extraction procedure and the low volume of reagents used, reducing expenses for reagents and technicians. (C) 2011 Elsevier Ltd. All rights reserved.451136144Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)FAPESP [04/10287-6

Chemometrics optimization of carbohydrate separations in six food matrices by micellar electrokinetic chromatography with anionic surfactant

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Multivariate statistical design modeling and the Derringer-Suich desirability function analysis were applied to micellar electrokinetic chromatography (MEKC) results with anionic surfactant to separate carbohydrates (CHOs) in different food matrices. This strategy has been studied with success to analyze compounds of difficult separation, but has not been explored for carbohydrates. Six procedures for the analysis of different sets of CHOs present in six food matrices were developed. The effects of pH, electrolyte and surfactant concentrations on the separation of the compounds were investigated using a central composite design requiring 17 experiments. The simultaneous optimization of the responses for separation of six sets of CHOs was performed employing empirical models for prediction of optimal resolution conditions in six matrices, condensed milk, orange juices, rice bran, red wine, roasted and ground coffee and breakfast cereal samples. The results indicate good separation for the samples, with appropriate detectability and selectivity, short analysis time, low reagent cost and little waste generation, demonstrating that the proposed technique is a viable alternative for carbohydrate analysis in foods. (C) 2011 Elsevier B.V. All rights reserved.851237244Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)FAPESP [07/56714-0

Doehlert design-desirability function multi-criteria optimal separation of 17 phenolic compounds from extra-virgin olive oil by capillary zone electrophoresis

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)In Brazil, the consumption of extra-virgin olive oil (EVOO) is increasing annually, but there are no experimental studies concerning the phenolic compound contents of commercial EVOO. The aim of this work was to optimise the separation of 17 phenolic compounds already detected in EVOO. A Doehlert matrix experimental design was used, evaluating the effects of pH and electrolyte concentration. Resolution, runtime and migration time relative standard deviation values were evaluated. Derringer's desirability function was used to simultaneously optimise all 37 responses. The 17 peaks were separated in 19 min using a fused-silica capillary (50 gm internal diameter, 72 cm of effective length) with an extended light path and 101.3 mmol L-1 of boric acid electrolyte (pH 9.15, 30 kV). The method was validated and applied to 15 EVOO samples found in Brazilian supermarkets. Published by Elsevier Ltd.146558568Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)FAPESP [08/57548-0

A fast and efficient method for the study of caffeine levels in energy drinks using micellar electrokinetic chromatography (MEKC)

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Energy drinks are becoming popular in Brazil and in the world due to their stimulant properties. Caffeine is present in energy drinks with the aim of stimulating the central nervous system and intensifying brain activity. On the other hand, the ingestion of high doses of caffeine can cause undesirable symptoms such as anxiety and tachycardia. Therefore, it is necessary to monitor the caffeine content added to energy drinks to guarantee that the levels in the final product are in accordance with the labeling and within the legislation limits. The goal of this work was to validate a fast, efficient, and low-cost method for the determination of caffeine in energy drinks by micellar electrokinetic chromatography (MEKC). A total of seven brands were analyzed, each in three lots. The electrolyte was prepared with 50 mmol.L-1 of sodium dodecyl sulfate (SDS) and 10 mmol.L-1 of sodium carbonate (pH 11.0). The mean concentration of caffeine ranged from 122.8 to 318.6 mg.L-1. None of the brands had caffeine levels above the maximum limit. Considering the interval of confidence (95%), 72% of the samples had less caffeine than the amount informed on the product label.322401404Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq

Optimisation of a CE method for caffeine analysis in decaffeinated coffee

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Multiple response simultaneous optimisation Was used to develop a micellar electrokinetic chromatography method for caffeine determination in decaffeinated coffees. Buffer composition and voltage were optimised using a central composite design. Six responses were evaluated and each set of response values was regressed on the factor levels of the experimental design using linear and quadratic models. The regression models, correlation coefficients and a principal component analysis (PCA) were used to determine the Optimum conditions. Successful results were obtained using a buffer containing 10 mmol L(-1) sodium carbonate and 50 mmol L(-1) sodium dodecylsulfate, 15 kV voltage, 25 degrees C temperature, 48 cm x 50 pm fused-silica capillary, hydrodynamic injection of 50 mBar during 7 s and detection at 206 nm. This optimised method was applied for caffeine analysis in 45 samples of commercial decaffeinated coffee. (C) 2009 Elsevier Ltd. All rights reserved.120411551161Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq

Comparison of capillary electrophoresis and high performance liquid chromatography methods for caffeine determination in decaffeinated coffee

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Decaffeinated coffee accounts for 10 percent of coffee sales in the world; it is preferred by consumers that do not wish or are sensitive to caffeine effects. This article presents an analytical comparison of capillary electrophoresis (CE) and high performance liquid chromatography (HPLC) methods for residual caffeine quantification in decaffeinated coffee in terms of validation parameters, costs, analysis time, composition and treatment of the residues generated, and caffeine quantification in 20 commercial samples. Both methods showed suitable validation parameters. Caffeine content did not differ statistically in the two different methods of analysis. The main advantage of the high performance liquid chromatography (HPLC) method was the 42-fold lower detection limit. Nevertheless, the capillary electrophoresis (CE) detection limit was 115-fold lower than the allowable limit by the Brazilian law. The capillary electrophoresis (CE) analyses were 30% faster, the reagent costs were 76.5-fold, and the volume of the residues generated was 33-fold lower. Therefore, the capillary electrophoresis (CE) method proved to be a valuable analytical tool for this type of analysis.331186191Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq