Comparison of Simple and Rapid Extraction Procedures for the Determination of Pesticide Residues in Fruit Juices by Fast Gas Chromatography–Mass Spectrometry

Three sample treatment methods, based on QuEChERS, solid-phase extraction (SPE) and solid-phase microextraction (SPME), were compared and evaluated in order to obtain the best conditions to determine pesticide residues in fruit juice by fast gas chromatography–mass spectrometry (single quadrupole GC-MS). Analysis were performed under selected ion monitoring, acquiring the three most abundant and/or specific ions for each analyte and using their relative intensity ratios as a confirmatory parameter. The 3 methodologies (QuEChERS, SPE and SPME) were validated taking 15 selected pesticides as model compounds, using commercial apple juice. QuEChERS procedure was based on the AOAC Official Method 2007.01, using acetonitrile (containing 1 % acetic acid) as extraction solvent and primary–secondary amine during the dispersive solid-phase extraction. Oasis hydrophilic–lipophilic balance cartridges were used for SPE, and polyacrylate fibers were used for direct immersion SPME procedure. Three isotopically labeled standards were added to the samples before extraction and used as surrogate standards. Validation parameters as recoveries, limits of detection, and limits of quantification (LOQ), as well as matrix effects and sample throughput, were obtained and compared for the three extraction procedures. QuEChERS was considered faster and led to the best quantitative results. In this way, validation was extended to up to 56 pesticides by applying QuEChERS in multi-fruit juice samples, obtaining LOQs ranging from 2 to 20 μg/L for most compounds. Accuracy and precision were evaluated by means of recovery experiments at two concentration levels (10 and 100 μg/L), obtaining recoveries between 70 and 120 % in most cases and relative standard deviations below 15 %. Finally, the QuEChERS method was applied to the analysis of commercial juices, including mango–apple, pineapple, grapefruit and orange.     

Correlations of sensory parameters with physicochemical characteristics of Argentinean honeys by multivariate statistical techniques

Honey acceptability is mainly determined by its colour, crystallisation degree and aroma. In the present work, the sensory characteristics and physicochemical parameters of Argentinean honeys from different ecoregions were analysed. Moisture content, Pfund colour, diastase activity, hydroxymethylfurfural content, electrical conductivity, sugar profile and volatile compounds were analytically determined in honey samples, while sensory characteristics (crystal size, fluency score, sweetness, persistence, granularity, crystallisation, colour intensity and aroma) were evaluated by a trained panel. Significant correlations were found between honey crystallisation degree and hydroxymethylfurfural content and diastase activity (P ≤ 0.05). It could be confirmed that honey crystallisation interferes with the visual perception of colour. Floral, fresh fruit, ripe fruit, balsamic and wood aromas could be successfully linked to honey volatile profile (P ≤ 0.05). These results demonstrate that the parameters that could best guarantee the consumers’ preference can be successfully associated with the chemical composition of honey by multivariate statistical analysis.     

Innovative Quality Improvement by Continuous Microwave Processing of a Faba Beans Pesto Sauce

Nowadays, consumers demand healthy, safe, and ready-to-eat horticultural products because of their lifestyle. In this regard, new legume-based food product development with eco-innovative technologies seems to be an interesting market. The effect on quality of an innovative pesto sauce, made of fresh faba bean seeds, of an alternative continuous microwave treatment pasteurization (MW, 11 kW; 30 s) regarding a conventional pasteurization (85 °C; 5 min) throughout 20 days at 5 °C was studied. Non-heated blended samples were used as control. The microbial quality was satisfactory in all treatments. MW treatment improved the sensorial quality of pesto sauce and decreased condensed tannins. Additionally, MW-treated samples showed the best texture, consistency, and color, preserving its chlorophyll and carotenoid content. On the other hand, thermal treatments showed a decrease in total phenolic compounds (TPC) and antioxidant capacity (TEAC) after heating, regarding control samples; however, TPC and TEAC remained quite constant throughout the storage.     

Chemometric Analysis of <Superscript>1</Superscript>H NMR Fingerprints of <Emphasis Type="Italic">Coffea arabica</Emphasis> Green Bean Extracts Cultivated under Different Planting Densities

High planting density has been used to increase coffee production but there are few studies related to the variations it provokes in metabolite compositions. The use of ¹H NMR data associated with chemometric techniques allows the determination of metabolic fingerprints and verification of metabolic changes when coffee is subjected to high planting densities. The aim of this work is to investigate ¹H NMR spectral data of green bean extracts of Coffea arabica cv. IAPAR 59 grown in a square pattern at two planting densities, 6000 and 10,000 plants ha^?1. Thirty extracts were obtained using a simplex centroid design with four solvents (ethanol, acetone, dichloromethane, and hexane). The lyophilized extracts were dissolved in DMSO-d₆ to obtain the ¹H NMR spectra. The spectral data were analyzed with principal component (PCA) and cluster analyses (CA). Significant differences between ethanolic and non-ethanolic extracts were found by PCA. Only the ethanolic mean spectrum showed characteristic chemical shifts of sugars and trigonelline. Acetone extracts were separated by cluster analysis.     

Comparison of crumb microstructure from pound cakes baked in a microwave or conventional oven

Imaging, light microscopy and scanning electron microscopy were used to compare the microstructure of crumbs from pound cakes baked in a microwave or conventional oven. The microwave baking conditions for pound cake (240 W, 5 min) were established in previous research, conventional baked pound cakes were obtained using a swing oven at 180 °C for 40 min. Statistical differences in total cell, cell/cm² and mean cell area (P?0.05) were observed in the image analysis. Cells from microwaved pound cake crumbs were 20% larger. However, factor shape was 0.81 for both microwave and conventionally baked crumbs, and crumbs from both oven types were similar in appearance. Light microscopy revealed birefringence in crumbs from both types of pound cakes. Scanning electron microscopy revealed that the conventionally baked product had a greater amount of protein matrix however; the matrix structure of the crumb was comparable between microwave-baked and conventionally baked pound cakes. In conclusion, our results suggest that the unique aspects of pound cake dough, including its high content of fat, sugar and moisture, make it well suited to microwave baking.     

Antimicrobial and antibiofilm activities of procyanidins extracted from laurel wood against a selection of foodborne microorganisms

This study aimed to evaluate the antimicrobial and antibiofilm activities of two procyanidins isolated from an ethyl acetate extract of laurel wood against a selection of foodborne pathogens. The analysis of the extract by HPLC–DAD/ESI–MS allowed us to detect the presence of two procyanidins, which were selectively isolated and identified by chromatographic and spectroscopic means as cinnamtannin B‐1 ( 1 ) and procyanidin B‐2 ( 2 ). Procyanidins 1 and 2 exhibited two biological activities: inhibition of bacterial growth at high concentrations and prevention of biofilm formation at lower concentrations. Synergistic effect was also detected when both compounds were tested in combination against Listeria monocytogenes. Significant effects were also detected on disruption of preformed biofilm. The ability of procyanidins to inhibit microbial growth and biofilm formation and to synergistically work with each other may stimulate a market as natural food preservatives, and/or natural sanitisers for processing equipment where foodborne pathogens reside.     

Germin-like protein Cit s 1 and profilin Cit s 2 are major allergens in orange (Citrus sinensis) fruits

Oranges are clinically relevant allergenic foods. To date, orange allergens have not been characterized in detail. The study is aimed at analyzing the sensitization profile in orange-sensitized subjects with and without clinical allergy, and to identify orange allergens. Fifty-six sensitized subjects with self-reported reactions to orange were grouped into reactors (anaphylaxis or multiple episodes of immediate reactions and/or positive challenge tests) and non-reactors (negative open food challenge tests). Allergens were characterized by IgE immunoblotting, N-terminal sequencing, IgE-inhibition assays, and mediator release assays were performed to determine the allergenic potency of orange profilin. Of 56 subjects, 23 were classified as orange allergic showing mainly an oral allergy syndrome. Of 23 subjects classified as orange allergic, 22 were sensitized to profilin, Cit s 2. In patients with mono-sensitization to profilin in vitro histamine releases up to 75% from basophils were induced using orange extract and purified plant profilins. Of the allergic patients 78% were sensitized to germin-like protein, Cit s 1. Both allergens showed retained IgE reactivity in heat-processed orange juice. Interestingly, subjects with and without clinical allergy showed a comparable sensitization profile. Profilin and germin-like proteins are major orange allergens. The potential clinical relevance of orange profilin was indicated by its strong capacity to release histamine from basophils. However, a predominant sensitization to both allergens in subjects without symptoms also indicates a high frequency of clinically insignificant sensitization.     

HS-SPME/GC-MS Method to Characterise the Flavour of Italian Pasta: Potential Application to Assess the Quality of the Products

Food flavour, consisting of a large number of volatile compounds, has great influence on consumer acceptability and, when safety and nutritional value are guaranteed, sensory parameters become the discriminating factor in the product quality assessment which determines the differentiation on the market. The present work combines head space-solid phase micro-extraction and gas chromatography mass spectrometry techniques to analyse the volatile fraction of Italian durum wheat pasta. The aim was the optimization of an analytical method suitable to show possible differences in pasta flavour richness and identify compounds that could be used as food quality markers. Twenty-three odorants were identified and confirmed by comparing their mass spectra with those of 27 standard substances. The optimum conditions for extraction temperature and time, respectively, resulted from 70 °C and 90 min; the best recoveries were achieved with 10.5 g of sample. The developed method was applied for the relative quantitative analysis of different priced pasta to verify the technique capability to highlight possible quality differences.