LC-MS-MS Identification and Determination of the Flavone-C-Glucoside Vicenin-2 in Rat Plasma Samples Following Intraperitoneal Administration of Lychnophora Extract

The flavone C-glucoside, vicenin-2, in semi-purified extracts of the leaves of Lychnophora ericoides was quantified in rat plasma samples using a method based on reversed-phase high performance liquid chromatography coupled to tandem mass spectrometry. Vicenin-2 was analyzed on a LiChrospher (R) RP18 column using an isocratic mobile phase consisting of a mixture of methanol: water (30:70, v/v) plus 2.0% glacial acetic acid at a flow rate of 0.8 mL min(-1). Genistein was used as internal standard. The mass spectrometer was operated in positive ionization mode and analytes were quantified by multiple reaction monitoring at m/z 595 > 457 for vicenin-2 and m/z 271 > 153 for internal standard. Prior to the analysis, each rat plasma sample was acidified with 200 mu L of 50 mmol L(-1) acetic acid solution and extracted by solid-phase extraction using a C18 cartridge. The absolute recoveries were reproducible and the coefficients of variation values were lower than 5.2%. The method was linear over the 12.5 - 1500 ng mL(-1) concentration range and the quantification limit was 12.5 ng mL(-1). Within-day and between-day assay precision and accuracy were studied at three concentration levels (40, 400 and 800 ng mL(-1)) and were lower than 15%. The developed and validated method seems to be suitable for analysis of vicenin-2 in plasma samples obtained from rats that receive a single i.p. dose of 200 mg kg(-1) vicenin-2 extract.

DETERMINATION OF ENERGY VALUE OF HAMBURGERS AND MEATBALLS BY DIRECT CALORIMETRY AND FOOD ANALYSIS COMPOSITION. COMPARISON WITH NUTRITION INFORMATION DISPLAYED ON PACKAGES

The nutritional composition found in the laboratory and those present on labels of manufactured foods can differ significantly. The purpose of this study was to determine the nutritional composition of hamburgers and meatballs and compare them with your labels. The food analysis was performed following the Analytical Standards Institute`s Adolfo Lutz and energy content was determined by bomb calorimetry. Regarding the energy value, all the samples had values less than informed on the label. The content of lipids of hamburgers and meatballs ( except the beef) were lower than those reported on the label. The values of protein for the meatballs and chicken hamburger had lower values than those labels. Thus, the labels may overestimate as underestimate some nutritional values, leading to population erroneous information.

PCDDs in the water/sediment-seagrass-dugong (Dugong dugon) food chain on the Great Barrier Reef (Australia)

Polychlorinated dibenzo-p-dioxin (PCDD) and dibenzofuran (PCDF) concentrations were measured in sediment and seagrass from five locations in or adjacent to the Great Barrier Reef Marine Park. A full spectrum of Cl(5-8)DDs were present in all samples and, in particular, elevated levels of Cl8DD were found. PCDFs could not be quantified in any samples. The PCDD concentrations ranged over two orders of magnitude between sites, and there was a good correlation between sediment and seagrass levels. There were large quantities of sediment present on the seagrass (20-62% on a dry wt. basis), and it was concluded that this was a primary source of the PCDDs in the seagrass samples. The PCDD levels in the seagrass samples were compared with the levels in the tissue of three dugongs stranded in the same region. The relative accumulation of the 2,3,7,8-substituted PCDD congeners in the dugongs decreased by over two orders of magnitude with increasing degree of chlorination. This was attributed to the reduced absorption of the higher chlorinated congeners in the digestive tract, a behaviour that has been observed in other mammals such as domestic cows. (C) 2001 Elsevier Science Ltd. All rights reserved.

Comparison of fungal contamination between hospitals and companies food units

A descriptive study was developed to compare air and surfaces fungal contamination in ten hospitals’ food units and two food units from companies. Fifty air samples of 250 litres through impaction method were collected from hospitals’ food units and 41 swab samples from surfaces were also collected, using a 10 by 10 cm square stencil. Regarding the two companies, ten air samples and eight surface samples were collected. Air and surface samples were collected in food storage facilities, kitchen, food plating and canteen. Outdoor air was also collected since this is the place regarded as a reference. Simultaneously, temperature, relative humidity and meal numbers were registered. Concerning air from hospitals’ food units, 32 fungal species were identified, being the two most commonly isolated genera Penicillium sp.

Neutron activation analysis of wheat samples

The deficiency of essential micronutrients and excess of toxic metals in cereals, an important food items for human nutrition, can cause public health risk. Therefore, before their consumption and adoption of soil supplementation, concentrations of essential micronutrients and metals in cereals should be monitored. This study collected soil and two varieties of wheat samples–Triticum aestivum L. (Jordão/bread wheat), and Triticum durum L. (Marialva/durum wheat) from Elvas area, Portugal and analyzed concentrations of As, Cr, Co, Fe, K, Na, Rb and Zn using Instrumental Neutron Activation Analysis (INAA) to focus on the risk of adverse public health issues. The low variability and moderate concentrations of metals in soils indicated a lower significant effect of environmental input on metal concentrations in agricultural soils. The Cr and Fe concentrations in soils that ranged from 93–117 and 26,400–31,300 mg/kg, respectively, were relatively high, but Zn concentration was very low (below detection limit <22 mg/kg) indicating that soils should be supplemented with Zn during cultivation. The concentrations of metals in roots and straw of both varieties of wheat decreased in the order of K>Fe>Na>Zn>Cr>Rb>As>Co. Concentrations of As, Co and Cr in root, straw and spike of both varieties were higher than the permissible limits with exception of a few samples. The concentrations of Zn in root, straw and spike were relatively low (4–30 mg/kg) indicating the deficiency of an essential micronutrient Zn in wheat cultivated in Portugal. The elemental transfer from soil to plant decreases with increasing growth of the plant. The concentrations of various metals in different parts of wheat followed the order: Root>Straw>Spike. A few root, straw and spike samples showed enrichment of metals, but the majority of the samples showed no enrichment. Potassium is enriched in all samples of root, straw and spike for both varieties of wheat. Relatively to the seed used for cultivation, Jordão presented higher transfer coefficients than Marialva, in particular for Co, Fe, and Na. The Jordão and Marialva cultivars accumulated not statistically significant different concentrations of different metals. The advantages of using INAA are the multielementality, low detection limits and use of solid samples (no need of digestion).

Air fungal contamination in ten hospitals’ food units from Lisbon

A descriptive study was developed to monitor air fungal contamination in ten food units from hospitals. Fifty air samples of 250 litres were collected through impaction method. Samples were collected in food storage facilities, kitchen, food plating, canteen and also, outside premises, since this is the place regarded as reference. Simultaneously, environmental parameters were also monitored, including temperature and relative humidity through the equipment Babouc, LSI Sistems and according to the International Standard ISO 7726.

Electrochemical immunosensor for multiplexed detection of food-borne pathogens using nanocrystal bioconjugates and MWCNT screen-printed electrode

Bacterial food poisoning is an ever-present threat that can be prevented with proper care and handling of food products. A disposable electrochemical immunosensor for the simultaneous measurements of common food pathogenic bacteria namely Escherichia coli O157:H7 (E. coli), campylobacter and salmonella were developed. The immunosensor was fabricated by immobilizing the mixture of anti-E. coli, anticampylobacter and anti-salmonella antibodies with a ratio of 1:1:1 on the surface of the multiwall carbon nanotube-polyallylamine modified screen printed electrode (MWCNT-PAH/SPE). Bacteria suspension became attached to the immobilized antibodies when the immunosensor was incubated in liquid samples. The sandwich immunoassay was performed with three antibodies conjugated with specific nanocrystal ( -E. coli-CdS, -campylobacter-PbS and -salmonella-CuS) which has releasable metal ions for electrochemical measurements. The square wave anodic stripping voltammetry (SWASV) was employed to measure released metal ions from bound antibody nanocrystal conjugates. The calibration curves for three selected bacteria were found in the range of 1 × 103 – 5 × 105 cells mL−1 with the limit of detection (LOD) 400 cells mL−1 for salmonella, 400 cells mL−1 for campylobacter and 800 cells mL−1 for E. coli. The precision and sensitivity of this method show the feasibility of multiplexed determination of bacteria in milk samples.

Extraction of ochratoxin A in bread samples by the QuEChERS methodology

A QuEChERS method for the extraction of ochratoxin A (OTA) from bread samples was evaluated. A factorial design (23) was used to find the optimal QuEChERS parameters (extraction time, extraction solvent volume and sample mass). Extracts were analysed by LC with fluorescence detection. The optimal extraction conditions were: 5 g of sample, 15 mL of acetonitrile and 3 min of agitation. The extraction procedure was validated by systematic recovery experiments at three levels. The recoveries obtained ranged from 94.8% (at 1.0 μg kg -1) to 96.6% (at 3.0 μg kg -1). The limit of quantification of the method was 0.05 μg kg -1. The optimised procedure was applied to 20 samples of different bread types (‘‘Carcaça’’, ‘‘Broa de Milho’’, and ‘‘Broa de Avintes’’) highly consumed in Portugal. None of the samples exceeded the established European legal limit of 3 μg kg -1.

Survey of trace elements (Al, As, Cd, Cr, Co, Hg, Mn, Ni, Pb, Se, and Si) in retail samples of flavoured and bottled waters

Concentrations of eleven trace elements (Al, As, Cd, Cr, Co, Hg, Mn, Ni, Pb, Se, and Si) were measured in 39 (natural and flavoured) water samples. Determinations were performed using graphite furnace electrothermetry for almost all elements (Al, As, Cd, Cr, Co, Mn, Ni, Pb, and Si). For Se determination hydride generation was used, and cold vapour generation for Hg. These techniques were coupled to atomic absorption spectrophotometry. The trace element content of still or sparkling natural waters changed from brand to brand. Significant differences between natural still and natural sparkling waters (p<0.001) were only apparent for Mn. The Mann–Whitney U-test was used to search for significant differences between flavoured and natural waters. The concentration of each element was compared with the presence of flavours, preservatives, acidifying agents, fruit juice and/or sweeteners, according to the labelled composition. It was shown that flavoured waters generally increase the trace element content. The addition of preservatives and acidifying regulators had a significant influence on Mn, Co, As and Si contents (p<0.05). Fruit juice can also be correlated to the increase of Co and As. Sweeteners did not provide any significant difference in Mn, Co, Se and Si content.

Optimization of QuEChERS procedure coupled to GC-ECD for organochlorine pesticide determination in carrot samples

An optimised version of the Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) method for simultaneous determination of 14 organochlorine pesticides in carrots was developed using gas chromatography coupled with electron-capture detector (GC-ECD) and confirmation by gas chromatography tandem mass spectrometry (GC-MS/MS). A citrate-buffered version of QuEChERS was applied for the extraction of the organochlorine pesticides, and for the extract clean-up, primary secondary amine, octadecyl-bonded silica (C18), magnesium sulphate (MgSO4) and graphitized carbon black were used as sorbents. The GC-ECD determination of the target compounds was achieved in less than 20 min. The limits of detection were below the EUmaximum residue limits (MRLs) for carrots, 10–50 μg kg−1, while the limit of quantification did exceed 10 μg kg−1 for hexachlorobenzene (HCB). The introduction of a sonication step was shown to improve the recoveries. The overall average recoveries in carrots, at the four tested levels (60, 80, 100 and 140 μg kg−1), ranged from 66 to 111% with relative standard deviations in the range of 2– 15 % (n03) for all analytes, with the exception of HCB. The method has been applied to the analysis of 21 carrot samples from different Portuguese regions, and β-HCH was the pesticide most frequently found, with concentrations oscillating between less than the limit of quantification to 14.6 μg kg−1. Only one sample had a pesticide residue (β-HCH) above the MRL, 14.6 μg kg−1. This methodology combines the advantages of both QuEChERS and GC-ECD, producing a very rapid, sensitive and reliable procedure which can be applied in routine analytical laboratories.

Proposal of a short-form version of the Brazilian Food Insecurity Scale

OBJECTIVE To propose a short version of the Brazilian Food Insecurity Scale. METHODS Two samples were used to test the results obtained in the analyses in two distinct scenarios. One of the studies was composed of 230 low income families from Pelotas, RS, Southern Brazil, and the other was composed of 15,575 women, whose data were obtained from the 2006 National Survey on Demography and Health. Two models were tested, the first containing seven questions, and the second, the five questions that were considered the most relevant ones in the concordance analysis. The models were compared to the Brazilian Food Insecurity Scale, and the sensitivity, specificity and accuracy parameters were calculated, as well as the kappa agreement test. RESULTS Comparing the prevalence of food insecurity between the Brazilian Food Insecurity Scale and the two models, the differences were around 2 percentage points. In the sensitivity analysis, the short version of seven questions obtained 97.8% and 99.5% in the Pelotas sample and in the National Survey on Demography and Health sample, respectively, while specificity was 100% in both studies. The five-question model showed similar results (sensitivity of 95.7% and 99.5% in the Pelotas sample and in the National Survey on Demography and Health sample, respectively). In the Pelotas sample, the kappa test of the seven-question version totaled 97.0% and that of the five-question version, 95.0%. In the National Survey on Demography and Health sample, the two models presented a 99.0% kappa. CONCLUSIONS We suggest that the model with five questions should be used as the short version of the Brazilian Food Insecurity Scale, as its results were similar to the original scale with a lower number of questions. This version needs to be administered to other populations in Brazil in order to allow for the adequate assessment of the validity parameters.

Evaluating the use of in-store measures in retail food stores and restaurants in Brazil

ABSTRACTOBJECTIVE To assess inter-rater reliability, test-retest reliability, and construct validity of retail food store, open-air food market, and restaurant observation tools adapted to the Brazilian urban context.METHODS This study is part of a cross-sectional observation survey conducted in 13 districts across the city of Sao Paulo, Brazil in 2010-2011. Food store and restaurant observational tools were developed based on previously available tools, and then tested it. They included measures on the availability, variety, quality, pricing, and promotion of fruits and vegetables and ultra-processed foods. We used Kappa statistics and intra-class correlation coefficients to assess inter-rater and test-retest reliabilities in samples of 142 restaurants, 97 retail food stores (including open-air food markets), and of 62 restaurants and 45 retail food stores (including open-air food markets), respectively. Construct validity as the tool’s abilities to discriminate based on store types and different income contexts were assessed in the entire sample: 305 retail food stores, 8 fruits and vegetable markets, and 472 restaurants.RESULTS Inter-rater and test-retest reliability were generally high, with most Kappa values greater than 0.70 (range 0.49-1.00). Both tools discriminated between store types and neighborhoods with different median income. Fruits and vegetables were more likely to be found in middle to higher-income neighborhoods, while soda, fruit-flavored drink mixes, cookies, and chips were cheaper and more likely to be found in lower-income neighborhoods.CONCLUSIONS The measures were reliable and able to reveal significant differences across store types and different contexts. Although some items may require revision, results suggest that the tools may be used to reliably measure the food stores and restaurant food environment in urban settings of middle-income countries. Such studies can help .inform health promotion interventions and policies in these contexts.

Intestinal parasites in school food handlers in the city of Uberlândia, Minas Gerais, Brazil

In order to verify the presence of intestinal parasites in food handlers, stool samples were collected from 104 cooks and their helpers that were working in food preparation in 20 public elementary schools, in various areas of the city of Uberlândia, Minas Gerais, Brazil. The samples were collected during the months of November and December, 1988, in plastic flasks containing a 10% formaldehyde solution and processed by the Hoffmann, Pons & Janer method. The sediment was examined using triplicate slides. All individuals were females aged between 24 to 69 years. Intestinal parasites were found in 85.0% of the studied schools and 47.1% of the studied food handlers (cooks and helpers) were found to be positive. Among the 49 infected food handlers, 32 (65.3%) carried a single parasite and 17 (34.7%) carried two parasites. The following intestinal parasites were found: Giardia lamblia (21.1%), Entamoeba coli (21.1%), hookworms (9.6%), Ascaris lumbricoides (5.8%), Entamoeba histolytica (2.9%), Hymenolepis nana (1.9%), Strongyloides stercoralis (1.0%). These data emphasize the need for a rigid semi-annual control in all school food handlers, including diagnosis, specific treatment and orientation about the mechanisms of transmission of the intestinal parasites.

Freshwater arsenic detoxification through selenium-enriched food supplements. A proteomic approach

Dissertação apresentada para a obtenção do grau de doutor em Bioquímica pela Universidade Nova de Lisboa, Faculdade de Ciências e Tecnologia

Synthesis of biodiesel from wastes of food industry via direct transesterification with methanol/carbon dioxide mixtures

Dissertation presented at Faculdade de Ciências e Tecnologia from Universidade Nova de Lisboa to obtain the degree of Master in Chemical and Biochemical Engineering