Bauer-7-en-3beta-yl acetate: a major constituent of unusual samples of Brazilian propolis

The pentacyclic triterpenoid bauer-7-en-3beta-yl acetate was obtained from the chloroform extract of an unusual sample of propolis from southeast Brazil with the yield of 7%. The compound was identified by comparison of IR, MS and NMR analysis with published data.

Determination of chemical elements in africanized Apis mellifera (Hymenoptera: Apidae) honey samples from the State of Piauí, Brazil

Honey is a food used since the most remote times, appreciated for its characteristic flavor, considerable nutritional value and medicinal properties; however, little information exists about the presence of chemical elements in it. The objectives of this work were to determine the chemical elements present in 38 honey samples, collected directly from beekeepers from the State of Piauí, Brazil and to verify whether they presented any contamination. The chemical elements were determined by means of Total Reflection X-ray Fluorescence. The means of three replicates were: K (109.671 ± 17.487), Ca (14.471 ± 3.8797), Ti (0.112 ± 0.07), Cr (0.196 ± 0.11), Mn (0.493 ± 0.103), Fe (1.722 ± 0.446), Co (0.038), Ni (0.728 ± 0.706), Cu (0.179 ± 0.0471), Zn (0.967 ± 0.653), Se (not detected), Br (not detected), Rb (0.371 ± 0.097), Sr (0.145 ± 0.45), Ba (11.681), Hg (not detected), and Pb (0.863) µg g-1.

Comparison of GC and HPLC for quantification of organic acids in two jaboticaba (Myrciaria) fruit varieties

Gas chromatography (GC) with trimethylsilyl derivative formation was compared to high-performance liquid chromatography (HPLC) for quantification of organic acids (OAs) in two jaboticaba (Myrciaria) fruit (pulp and pericarp) varieties (Sabará and Açu Paulista). Succinic and citric acids were the major OAs found in all the samples analyzed. Besides being much more tedious, the results obtained with GC were significantly lower than HPLC (p<0.05) when the data (acids, variety, two parts and flowering days) were considered together. The presence of both acids was confirmed by gas chromatography-mass spectrometry (GC-MS).

Physicochemical composition of Apis mellifera honey samples from São Paulo State, Brazil

This research, developed with Apis mellifera honey samples from producers of São Paulo State, Brazil, has the objective of verifying how eucalyptus, wild flower, and orange honey samples would be clustered, based on physicochemical characteristics. All the orange honey samples and some wild flower ones formed distinct groups, thus confirming that the floral source interferes with honey characteristics. Eucalyptus and some of the wild flower honey samples were clustered together because of the great floral source variation in the latter ones. The characteristics that influence sample clustering are acidity and electric conductivity on the X axis, and total sugars and pH on the Y axis.

Cloud point extraction for the determination of copper in environmental samples by flame atomic absorption spectrometry

A simple cloud point extraction procedure is presented for the preconcentration of copper in various samples. After complexation by 4-hydroxy-2-mercapto-6-propylpyrimidine (PTU), copper ions are quantitatively extracted into the phase rich in Triton X-114 after centrifugation. Methanol acidified with 0.5 mol L-1 HNO3 was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). Analytical parameters including concentrations for PTU, Triton X-114 and HNO3, bath temperature, centrifugation rate and time were optimized. The influences of the matrix ions on the recoveries of copper ions were investigated. The detection limits (3SDb/m, n=4) of 1.6 ng mL-1 along with enrichment factors of 30 for Cu were achieved. The proposed procedure was applied to the analysis of environmental samples.

Determinação simultânea dos ácidos orgânicos tartárico, málico, ascórbico e cítrico em polpas de acerola, açaí e caju e avaliação da estabilidade em sucos de caju

The aim of the present study was determining the main organic acids in pulp and juices, as well as evaluating their stability, after opening the package, by liquid chromatography in a C18 column with isocratic elution and UV detection. In açaí pulp tartaric, malic and citric acids were found. Cashew samples presented all of the organic acids evaluated, besides high concentrations of ascorbic and malic acids. Acerola pulp had the highest ascorbic acid concentration. A small decrease in organic acid content during storage was observed. Malic and citric acids seem to be more stable than tartaric and ascorbic acids.

Analytical procedures for determining Pb and Sr isotopic compositions in water samples by ID-TIMS

Few articles deal with lead and strontium isotopic analysis of water samples. The aim of this study was to define the chemical procedures for Pb and Sr isotopic analyses of groundwater samples from an urban sedimentary aquifer. Thirty lead and fourteen strontium isotopic analyses were performed to test different analytical procedures. Pb and Sr isotopic ratios as well as Sr concentration did not vary using different chemical procedures. However, the Pb concentrations were very dependent on the different procedures. Therefore, the choice of the best analytical procedure was based on the Pb results, which indicated a higher reproducibility from samples that had been filtered and acidified before the evaporation, had their residues totally dissolved, and were purified by ion chromatography using the Biorad® column. Our results showed no changes in Pb ratios with the storage time.

The role of bound chlorine in the brightness reversion of bleached hardwood kraft pulp

Our previous paper showed fragmentary evidence that pulp brightness reversion may be negatively affected by its organically bound chlorine (OX) content. A thorough investigation on eucalyptus kraft pulp led to the conclusion that OX increases reversion of certain pulps but this trend is not universal. Alkaline bleaching stages decrease reversion regardless of pulp OX content. Pulps bleached with high temperature chlorine dioxide revert less than those bleached with conventional chlorine dioxide in sequences ending with a chlorine dioxide stage but similarly in sequences ending with a final peroxide stage. The use of secondary condensate for pulp washing decreases reversion.

Validation of an analytical methodology for the quantitative analysis of petroleum hydrocarbons in marine sediment samples

This work describes a validation of an analytical procedure for the analysis of petroleum hydrocarbons in marine sediment samples. The proposed protocol is able to measure n-alkanes and polycyclic aromatic hydrocarbons (PAH) in samples at concentrations as low as 30 ng/g, with a precision better than 15% for most of analytes. The extraction efficiency of fortified sediments varied from 65.1 to 105.6% and 59.7 to 97.8%, for n-alkanes and PAH in the ranges: C16 - C32 and fluoranthene - benzo(a)pyrene, respectively. The analytical protocol was applied to determine petroleum hydrocarbons in sediments collected from a marine coastal zone.

Characterization of the major nutritional components of Caryocar brasiliense fruit pulp by nmr spectroscopy

Pequi (Caryocar brasiliense Camb.), a typical fruit of Brazilian Cerrado, is well known in regional cookery and used in folk medicine to treat various illnesses. Mass spectrometry and chromatographic methods have identified the organic composition of pequi fruit pulp; however, NMR spectroscopy is used for the first time to characterize the nutritional components of organic and aqueous-ethanolic extracts. This spectroscopic technique determined the triacylglycerols in the pequi organic fraction, which is constituted mainly by oleate and palmitate esters, and detected the carbohydrate mixtures as the major components of aqueous and ethanolic fractions, respectively. In this study, presence of phenolic compounds was only evidenced in the ethanolic fraction.

Stability of antioxidants vitamins in bee pollen samples

This study evaluated the stability of vitamins C, E and β-carotene in six samples of bee pollen after their process, and in a one-year period of storage. After the pollen's process, there was a 67.1% increase for vitamin C (p <0.05), an 18.7% loss for vitamin E and 15.6% for β-carotene. Storage in freezer was the most efficient condition for the vitamins conservation; the loss in storage at room temperature (exposed or protected from light) was similar. Vitamin E appears to be better preserved during storage when compared to vitamin C and β-carotene.

Determination of aluminum in food samples after preconcentration as aluminon complex on microcrystalline naphthalene by spectrophotometry

A sensitive preconcentration procedure for spectrophotometeric determination of aluminum was developed. Aluminum as aluminon complex is adsorbed on microcrystalline naphthalene. The naphthalene containing the complex is dissolved in 3 mL of acetone and its absorbance is measured at 544 nm. The effect of various factors on the preconcentration of aluminum was investigated. The calibration graph was linear in the range of 1-60 mg L-1. The limit of detection was 0.52 mg L-1 and relative standard deviation for the determination of 5 mg L-1 was 2.65%. The proposed solid phase extraction procedure was applied to determination of aluminum in food samples.

Determination of traces of nitrate in water samples using spectrophotometric method after its preconcentration on microcrystalline naphthalene

Nitrate is quantitatively retained with 2,6-bis(4-methoxyphenyl)-4-phenyl pyrylium perchlorate (PPP) on microcrystalline naphthalene in the pH range of 6.5-9.0 from a large volume of aqueous solutions of various samples. The method was based on the complexation between PPP and nitrate and then, extraction of the resulted complex from aqueous solution by microcrystalline naphthalene. The solid mass consisting of the nitrate complex and naphthalene was then dissolved in dimethyl formamide (DMF) and absorption of the resulted solution was obtained at 328 nm. The linear calibration range for the determination of nitrate was 15-135 μg L-1 with the detection limit of 10 μg L-1.

Ion pair-dispersive liquid-liquid microextraction of trace amount of rhodium ion in water and road dust samples prior to flame atomic absorption spectrometry determination

A simple ion pair-dispersive liquid-liquid microextraction method was proposed for preconcentration trace amounts of rhodium. An ion association complex of RhCl4- and tetradecyldimetylbenzylamonium was extracted into cholorobenzene. The volume and the type of extractive and dispersive solvents, the extraction time and the pH of the aqueous solutions were optimized. The calibration curve was linear in the range of 0.6-500 ng mL-1 of rhodium. The limit of detection was 0.10 ng mL-1 in initial solution and preconcentration factor was 40. The proposed method was successfully applied to the extraction and determination of rhodium in road dust and water samples.

Dispersive liquid-liquid microextraction for the simultaneous separation of trace amounts of zinc and cadmium ions in water samples prior to flame atomic absorption spectrometry determination

In the proposed method, carbon tetrachloride and ethanol were used as extraction and dispersive solvents. Several factors that may be affected on the extraction process, such as extraction solvent, disperser solvent, the volume of extraction and disperser solvent, pH of the aqueous solution and extraction time were optimized. Under the optimal conditions, linearity was maintained between 1.0 ng mL-1 to 1.5 mg mL-1 for zinc and 1.0 ng mL-1 to 0.4 mg mL-1 for cadmium. The proposed method has been applied for determination of trace amount of zinc and cadmium in standard and water samples with satisfactory results.