Comparison of methodologies for moisture determination on dried bee pollen samples

Bee pollen moisture value is one of the quality parameters for this product. Some countries such as Argentina, Brazil, Bulgaria, Poland and Switzerland have bee pollen regulations on quality parameters, but these are not clear regarding which method should be used for moisture determination. The aim of this paper was to compare six methods of moisture determination in dried bee pollen samples. The methods were: conventional oven at 100 °C, vacuum oven at 70 °C, desiccator with sulfuric acid, drying out process with infrared light at 85 °C, lyophilization and Karl Fisher's method. Based on the results, the best methods for moisture determination of bee pollen were the drying process with infrared and the lyophilization, since these have shown lower moisture values.

Determination of presence and quantification of cadmium, lead and copper in Nile tilapia (Oreochromis niloticus) fillets obtained from three cold storage plants in the state of Parana, Brazil

Pisciculture is an economic activity that is steadily growing in the state of Parana, Brazil, and Nile tilapia (Oreochromis niloticus) is one of the widely cultivated species in this state. Tilapia is not only a very nutritious food, but also an important indicator of environmental contamination. This study aimed to verify contamination by cadmium, copper and lead in tilapia fillets, and to compare the found values to international legislations. Were collected 135 samples of tilapia fillets, between July 2006 and May 2007, in three fish stores located in regions west and north of Paraná State. Samples of tilapia fillet were analyzed in relation to the presence of cadmiun, lead and copper, using atomic absorption spectrophotometry. Lead has not been detected in the analyses. Cadmium has been detected in three samples, on concentrations of 0.012 µg.g-1, 0.011 µg.g-1 and 0.014 µg.g-1. Copper has been detected in all fillets, and the average concentration of each cold storage plant was of 0.122 µg.g-1, 0.106 µg.g-1 and 0.153 µg.g-1. The concentrations found in this study are within the limits allowed by both the European and the Australian legislations.

Determination of pectin methylesterase activity in commercial pectinases and study of the inactivation kinetics through two potentiometric procedures

Pectinases are enzymes that degrade pectic substances and are widely used in juice and fruit beverages to improve the quality of the process. The objective of this study was to determine the optimum pH and temperature of two samples of commercial pectinases and propose an alternative procedure to determine the residual activity comparing the data with those of the traditional procedure. The pectin methylesterase (PME) activity in Pectinex 100 L Plus and Panzyn Clears was determined by potentiometry. The reaction consisted of 5.00 mg.mL-1 apple pectin, 0.100 mol.L-1 NaCl, and 50 µL enzyme to a total volume of 30 mL. The pectin reaction in the presence of PME in all experiments revealed a first order kinetics. The PME in the two enzyme preparations showed higher activity at pH 4.0 to 4.5 and temperature of 45 ºC. From the results of both procedures ΔV NaOH/Δt and ΔpH/Δt, it was concluded that the inactivation of PME occurred at 75 ºC. The results obtained from the ratio ΔpH/Δt showed good correlation with those obtained from the ratio ΔV NaOH/Δt. In the reaction accompanied by the ratio ΔpH/Δt, the release of H3O+ occurred in the real time reaction.

Determination of structural and mechanical properties, diffractometry, and thermal analysis of chitosan and hydroxypropylmethylcellulose (HPMC) films plasticized with sorbitol

In this work, the structural, mechanical, diffractometric, and thermal parameters of chitosan-hydroxypropylmethylcellulose (HPMC) films plasticized with sorbitol were studied. Solutions of HPMC (2% w/v) in water and chitosan (2% w/v) in 2% acetic acid solution were prepared. The concentration of sorbitol used was 10% (w/w) to both polymers. This solutions were mixed at different proportions (100/0; 70/30; 50/50; 30/70, and 0/100) of chitosan and HPMC, respectively, and 20 mL was cast in Petri dishes for further analysis of dried films. The miscibility of polymers was assessed by X-ray diffraction, scanning electronic microscopy (SEM), differential scanning calorimetry (DSC), and thermal gravimetric analysis (TGA). The results obtained indicate that the films are not fully miscible at a dry state despite the weak hydrogen bonding between the polymer functional groups.

Sugarcane starch: quantitative determination and characterization

Starch is found in sugarcane as a storage polysaccharide. Starch concentrations vary widely depending on the country, variety, developmental stage, and growth conditions. The purpose of this study was to determine the starch content in different varieties of sugarcane, between May and November 2007, and some characteristics of sugarcane starch such as structure and granules size; gelatinization temperature; starch solution filterability; and susceptibility to glucoamylase, pullulanase, and commercial bacterial and fungal α-amylase enzymes. Susceptibility to debranching amylolytic isoamylase enzyme from Flavobacterium sp. was also tested. Sugarcane starch had spherical shape with a diameter of 1-3 µm. Sugarcane starch formed complexes with iodine, which showed greater absorption in the range of 540 to 620 nm. Sugarcane starch showed higher susceptibility to glucoamylase compared to that of waxy maize, cassava, and potato starch. Sugarcane starch also showed susceptibility to debranching amylolytic pullulanases similar to that of waxy rice starch. It also showed susceptibility to α-amylase from Bacillus subtilis, Bacillus licheniformis, and Aspergillus oryzae similar to that of the other tested starches producing glucose, maltose, maltotriose, maltotetraose, maltopentose and limit α- dextrin.

Biosensor for determination of glucose in real samples of beverages

A biosensor was developed for spectrophotometric determination of glucose concentrations in real samples of orange juice energetic drinks, and sport drinks. The biosensor consisted of glucose oxidase (GOD) and horseradish peroxidase (HRP) immobilized onto polyaniline activated with glutaraldehyde (PANIG). Immobilization parameters were optimized for GOD, and maximum immobilization yield was 16% when 5.0 mg of PANIG and 8.9 U prepared in 0.1 mol.L-1 sodium phosphate buffer (pH 7.0) reacted for 60 minutes at 4 °C with gentle stirring. The linear operational range for glucose determination using optimized operational parameters was between 0.05 and 6.0 mg.mL-1 with a very good reproducibility of response. The results obtained in the biosensor were compared with those obtained using free enzymes (commercial kits) and then validated through statistical analysis using the Tukey test (95% confidence interval).

Cadmium determination in Lentinus edodes mushroom species

Many studies have drawn attention to the occurrence and concentration of toxic elements found in the fruiting body of mushrooms. Some edible mushroom species are known to accumulate high levels of inorganic contaminants, mainly cadmium, mercury, and lead. There are about 2,000 known edible mushroom species, but only 25 of them are cultivated and used as food. In Brazil, the most marketed and consumed mushroom species are Agaricus bisporus, known as Paris champignon, Lentinus edodes, or Shitake and Pleurotus sp, also called Shimeji or Hiratake. In this study, the concentration of cadmium was determined in Lentinus edodes mushrooms from different cities in São Paulo state and some samples imported from Japan and China. The analyses were performed by graphite furnace atomic absorption spectrometry after HNO3-H2O2 digestion. The results showed a lower concentration of Cd in the mushrooms cultivated in São Paulo (0.0079 to 0.023 mg.kg-1 in natura) than that of the mushrooms cultivated abroad (0.125 to 0.212 mg.kg-1 in natura). Although there is no tolerance limit for Cd in mushrooms in Brazil, the results show that Lentinus edodes mushrooms can be safely consumed.

Determination of acrolein, ethanol, volatile acidity, and copper in different samples of sugarcane spirits

Seventy-one samples of sugarcane spirits from small and average size stills produced in the northern and southern Minas Gerais (Brazil) were analyzed for acrolein using HPLC (High Performance Liquid Chromatography). Ethanol and copper concentrations and volatile acidity were also determined according to methods established by the Ministry of Agriculture, Livestock and Supply (MAPA). A total of 9.85% of the samples tested showed levels of acrolein above the legal limits, while the copper concentrations of 21.00% of the samples and the volatile acidity of 8.85% of the samples were higher than the limits established by the Brazilian legislation. The concentration of acrolein varied from 0 to 21.97 mg.100 mL-1 of ethanol. However, no significant difference at 5% of significance was observed between the samples produced in the northern and southern Minas Gerais. The method used for determination of acrolein in sugarcane spirits involved the formation of a derivative with 2,4-dinitrophenylhydrazine (2,4-DNPH) and subsequent analysis by HPLC.

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

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.

Development and optimization of a HPLC-RI method for the determination of major sugars in apple juice and evaluation of the effect of the ripening stage

The sugars in apple juice prove its authenticity and its sensory and nutritional properties. The aim of this study was to develop and validate a simple analytical method using high performance liquid chromatography with refractive index detection (HPLC-RI) to determinate and quantify the sugars sucrose, D-glucose, D-fructose, and D-sorbitol polyol in apple juices, as well as to analyze the juices from the Fuji suprema and Lis Gala cultivars at three ripening stages. The analytical performance parameters evaluated indicated that the method was specific for the compounds analyzed, and the linearity of the calibration curves of sugars showed high correlation coefficients (close to 1.0). The limits of detection and quantification are consistent with recommendations available in the literature for this type of matrix. Sample preparation is simple and generates small amount of residues. Over 70% of the sugars were determined in the juices of apples at the pre-ripe stage, with an increase during senescence. This method is applicable for the determination of sugars in juices and evaluation of apple ripening.

Mathematical modeling of microwave dried celery leaves and determination of the effective moisture diffusivities and activation energy

Celery (Apium graveolens L. var. secalinum Alef) leaves with 50±0.07 g weight and 91.75±0.15% humidity (~11.21 db) were dried using 8 different microwave power densities ranging between 1.8-20 W g-1, until the humidity fell down to 8.95±0.23% (~0.1 db). Microwave drying processes were completed between 5.5 and 77 min depending on the microwave power densities. In this study, measured values were compared with predicted values obtained from twenty thin layer drying theoretical, semi-empirical and empirical equations with a new thin layer drying equation. Within applied microwave power density; models whose coefficient and correlation (R²) values are highest were chosen as the best models. Weibull distribution model gave the most suitable predictions at all power density. At increasing microwave power densities, the effective moisture diffusivity values ranged from 1.595 10-10 to 6.377 10-12 m2 s-1. The activation energy was calculated using an exponential expression based on Arrhenius equation. The linear relationship between the drying rate constant and effective moisture diffusivity gave the best fit.

Forced-air, vacuum, and hydro precooling of cauliflower (Brassica oleracea L. var. botrytis cv. Freemont): part I. determination of precooling parameters

The aim of the present study was to precool cauliflower using forced-air, vacuum and high and low flow hydro cooling methods. The weight of the precooled cauliflower heads (5000±5 g) was measured before they were placed in standard plastic crates. Cauliflower heads, whose initial temperature was 23.5 ± 0.5 ºC, were cooled until the temperature reached at 1 ºC. During the precooling process, time-dependent temperature and energy consumption were measured, and during vacuum precooling, the decreasing pressure values were recorded, and a curve of time-dependent pressure decrease (vacuum) was built. The most suitable cooling method to precool cauliflower in terms of cooling time and energy consumption was vacuum, followed by the high and low flow hydro and forced-air precooling methods, respectively. The highest weight loss was observed in the vacuum precooling method, followed by the forced-air method. However, there was an increase in the weight of the cauliflower heads in the high and low flow hydro precooling method. The best colour and hardness values were found in the vacuum precooling method. Among all methods tested, the most suitable method to precool cauliflower in terms of cooling and quality parameters was the vacuum precooling method.

Forced-air, vacuum, and hydro precooling of cauliflower (Brassica oleracea L. var. botrytis cv. Freemont): Part II. Determination of quality parameters during storage

Cauliflower heads, which were precooled using four different methods including vacuum, forced-air, and high and low flow hydro precooling, were stored under controlled atmosphere and room conditions. Controlled atmosphere conditions (CA) were as follows: 1°C temperature, 90 ± 5% relative humidity, and 0:21 [(%CO2:%O2) – (0:21) control] atmosphere composition. Room conditions (RC) were: 22±1°C temperature and 55-60% humidity. Various quality parameters of the cauliflower heads were assessed during storage (days 0, 7, 14, 21, 28, and 35) under controlled atmosphere and room conditions (days 0, 5, and 10). During storage, weight loss, deterioration rate, overall sensory quality score, hardness, and colour (L, a, b, C and α) were evaluated. In the present study, the strength and quality parameters of cauliflower under CA and RC conditions were obtained. Vacuum precooling was found to be most suitable method before cauliflower was submitted to cold storage and sent to market. Furthermore, the storage of cauliflower without precooling resulted in a significant decrease in quality parameters.

Determination of some quality properties of marinated sea bream (Sparus Aurata L., 1758) during cold storage

In this study, it was aimed to determine the effect of sea bream (Sparus aurata) marinated some quality properties during cold storage. The fillets of fish were immersed into brine including 3.5% acetic acid 11% salt in the ratio of 1: 1.5 (fish: marinate brine) for marination process. After the process of ripening, samples were grouped into two and packed in plastic containers; one being plain (in sunflower oil) and the other being sauced (sauced prepared with sunflower oil). During storage, sensory, crude protein, lipid, dry matter and crude ash, TBA, TVB-N, TMA-N and peroxide analyses were done periodically. According to results of 200 days of storage, TVB-N values of sea bream marinates packaged as plain and sauced were 15.86/14.89 mg/100g, TBA 7.06/7.99 mg MA/kg, TMA-N 2.97/3.12, mg/100g, the value of peroxide was 7.23/7.45 meq/kg respectively. According to chemical and sensory analyses results obtained in the study; it was concluded that sea bream marinates packaged as plain and sauced can be stored in +4 °C for 200 days.

Development of a rapid method for the determination of antibiotic residues in honey using UPLC-ESI-MS/MS

Abstract An accurate, reliable and fast multianalyte/multiclass ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method was developed and validated for the simultaneous analysis of 23 pharmaceuticals, belonging to different classes amphenicols, sulfonamides, tetracyclines, in honey samples. The method developed consists of ultrasonic extraction followed by UPLC–ESI–MS/MS with electrospray ionization in both positive mode and negative mode. The influence of the extraction solvents and mobile phase composition on the sensitivity of the method, and the optimum conditions for sample weight and extraction temperature in terms of analyte recovery were extensively studied. The identification of antibiotics is fulfilled by simultaneous use of chromatographic separation using an Acquity BEH C18 (100 mm x 2.1 mm, 1.7 µm) analytical column with a gradient elution of mobile phases and tandem mass spectrometry with an electrospray ionization. Finally, the method developed was applied to the determination of target analytes in honey samples obtained from the local markets and several beekeepers in Muğla, Turkey. Ultrasonic-extraction of pharmaceuticals from honey samples is a well-established technique by UPLC–ESI–MS/MS, the uniqueness of this study lies in the simultaneous determination of a remarkable number of compounds belonging to 23 drug at the sub-nanogram per kilogram level.