Combining high intensity ultrasound and experimental design to improve carotenoid extraction efficiency from Buriti (Mauritia flexuosa).

Buriti (Mauritia flexuosa L.) is a significant source of carotenoids, but these compounds have been extracted using laborious and low-effective methods. The present work evaluated the high-intensity ultrasound combined with a chemometric approach to developing an optimal extraction method of carotenoids from buriti pulp. The multivariate optimization was carried out through two steps. First, a simplex-lattice mixture design was used to optimize the extractor solution finding higher extraction yield (903 ± 21 µg g-1) with the acetone:ethanol (75/25) mixture. After, sample mass (80 mg) and sonication time (30 min) were optimized applying central composite design (CCD) which provided a 14% improvement in the extraction method yield. So, the total carotenoid content (TCC) with optimal extraction conditions was 1026 ± 13 µg g-1which is almost twice the yield of methods known in the literature for buriti. The RP-HPLC-DAD analysis revealed that the carotenoids are gently extracted and ß-carotene is the major compound in the extracts. To confirm the accuracy, buriti samples spiked with ß-carotene standard and the developed method showed recovery >84% and precision <6.5%. Furthermore, the optimized ultrasound-assisted extraction (UAE) method was applied to other samples (tomato, guava, carrot, mango, acerola, papaya, and pumpkin) and presented a yield to 5.5-fold higher when compared to the reported methods indicating high robustness. Based on results, the UAE method developed has demonstrated feasibility and reliability for the study of carotenoids in buriti pulp as well as in other plant matrices with high biological relevance.

Feasibility of internal standardization in the direct and simultaneous determination of As, Cu and Pb in sugar-cane spirits by graphite furnace atomic absorption spectrometry.

Bismuth and Sb were evaluated as internal standards (IS) to minimize matrix effects on the direct and simultaneous determination of As, Cu, and Pb in cachaça by graphite furnace atomic absorption spectrometry using W-coated platform plus Pd-Mg(NO(3))(2) as modifier. For 20microL injected sample, calibration within the 0.5-10microg L(-1) As, 100-1000microg L(-1) Cu and 0.5-30microg L(-1) Pb intervals were established using the ratios As absorbance to Sb absorbance, Cu absorbance to Bi absorbance and Pb absorbance to Bi absorbance versus analytes concentration, respectively. Typical linear correlations of 0.998, 0.999 and 0.999 were, respectively, obtained. The proposed method was applied for direct determination of As, Cu and Pb in 10 commercial cachaça samples and results were in agreement with those obtained by inductively coupled plasma mass spectrometry at 95% confidence level. The found characteristic masses were 30pg As, 274pg Cu and 39pg Pb. The useful lifetime of the graphite tube was around 760 firings. Recoveries of As, Cu and Pb added to cachaça samples varied, respectively, from 98% to 109%, 97% to 108% and 98% to 104% with internal standards and from 48% to 54%, 53% to 92% and 62% to 97% without internal standards. The limits of detection were 0.13microg L(-1) As, 22microg L(-1) Cu and 0.05microg L(-1) Pb. The relative standard deviations (n=12) for a spiked sample containing 20microg L(-1) As, Pb and 500microg L(-1) Cu were 1.6%, 1.0%, and 1.8% with IS and 4.3%, 5.2%, and 5.5% without IS.

Evaluation of alternate lines of Fe for sequential multi-element determination of Cu, Fe, Mn and Zn in soil extracts by high-resolution continuum source flame atomic absorption spectrometry.

The usefulness of the secondary line at 252.744nm and the approach of side pixel registration were evaluated for the development of a method for sequential multi-element determination of Cu, Fe, Mn and Zn in soil extracts by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). The influence of side pixel registration on the sensitivity and linearity was investigated by measuring at wings (248.325, 248.323, 248.321, 248.329, and 248.332nm) of the main line for Fe at 248.327nm. For the secondary line at 252.744nm or side pixel registration at 248.325nm, main lines for Cu (324.754nm), Mn (279.482nm) and Zn (213.875nm), sample flow-rate of 5.0mLmin(-1) and calibration by matrix matching, analytical curves in the 0.2-1.0mgL(-1) Cu, 1.0-20.0mgL(-1) Fe, 0.2-2.0mgL(-1) Mn, 0.1-1.0mgL(-1) Zn ranges were obtained with linear correlations better than 0.998. The proposed method was applied to seven soil samples and two soil reference materials (IAC 277; IAC 280). Results were in agreement at a 95% confidence level (paired t-test) with reference values. Recoveries of analytes added to soil extracts containing 0.15 and 0.30mgL(-1) Cu, 7.0 and 14mgL(-1) Fe, 0.60 and 1.20mgL(-1) Mn, 0.07 and 0.15mgL(-1) Zn, varied within the 94-99, 92-98, 93-101, and 93-103% intervals, respectively. The relative standard deviations (n=12) were 2.7% (Cu), 1.4% (Fe - 252.744nm), 5.7% (Fe - 248.325nm), 3.2% (Mn) and 2.8% (Zn) for an extract containing 0.35mgL(-1) Cu, 14mgL(-1) Fe, 1.1mgL(-1) Mn and 0.12mgL(-1) Zn. Detection limits were 5.4microgL(-1) Cu, 55microgL(-1) Fe (252.744nm), 147microgL(-1) Fe (248.325nm), 3.0microgL(-1) Mn and 4.2microgL(-1) Zn.