Modelling of Soy Sauce Desalting by Electrodialysis

In this work, the main features of electrodialytic (ED) desalting of microfiltered samples of a traditional soy sauce under constant electric current in the range of 1.25 to 6.5 A were quite well reconstructed using a mathematical model based on the Nernst–Planck equation. Amino nitrogen migration was characterised by a small effective transport number (t _AN?=?0.070?±?0.01), resulting in an average loss in amino nitrogen of about 30% whatever the electric current tested. The sodium chloride transport number (t _B?=?0.969?±?0.05) and diffusion rate (L _B?≈?0), as well as the effective membrane surface area, essentially coincided with those previously established when dealing with concentrated model brines. On the contrary, there was a significant diversity in the water transport number (t _W?=?8.3?±?0.1) and diffusion rate [L _W?=?(6.9?±?0.2)?×?10^?5 mol m^?2 s^?1?bar^?1], as well as in the anion- and cation-exchange membrane resistances (R _a?=?R _c?≈?0.04 Ω). The experimental procedure and mathematical model described in this work may be recommended not only to optimise the ED desalination of soy sauce but also to generate a first-cut design for ED desalting of other natural seasonings.     

Simultaneous Determination of Antioxidants and Ultraviolet Absorbers by Ultra-Performance Liquid Chromatography in Food Simulants

An efficient analytical method for the quantitative determination of migration levels of antioxidants and UV absorbers in food contact materials by ultra-performance liquid chromatography has been developed. The analytical method showed good linearity, presenting regression coefficients (R ²?≥?0.9981) for all compounds. The limits of detection and quantification were between 0.03 and 0.32 mg L^?1 and between 0.08 and 1.06 mg L^?1 for 29 analytes, respectively. According to European Union Directive No. 10/2011, five food simulants were investigated: 3 % (w/v) acetic acid, 10 % (v/v) ethanol, 20 % (v/v) ethanol, 50 % (v/v) ethanol, and fatty food simulant (isooctane). Recoveries were in the range of 88.43?～?115.28 %, with relative standard deviations between 0.33?～?8.43 %. Migration levels of antioxidants and UV absorbers were determined. Irganox 1010, Irganox 1076, and Tinuvin 120 were found in the majority of the samples generally together with the phosphate Irgafos 168 and its oxidized product. These levels were lower than limits allowed by legislation.     

Use of a Core-Shell Column for the Development of a Green LC Method for Thiol Determination in Fresh Fruits Following Derivatization with Methyl Propiolate

A novel HPLC method has been established for the determination of thiols in fruit samples, introducing, for the first time, methyl propiolate as an advantageous precolumn derivatization reagent for cysteine (CYS), glutathione (GSH), and N-acetylcysteine (NAC). The formed derivatives were detected at 285 nm, following isocratic separation on a core-shell column (Ascentis Express C18, 50?×?2.1 mm i.d., 2.7 μm) with a mobile phase of 15 mmol L^?1 (ΝΗ₄)₂ΗPO₄/H₃PO₄ (pH?=?2.2)/methanol (92:8?v/v), containing 1 mmol L^?1 EDTA, at a flow rate of 0.2 mL min^?1. Derivatization parameters were optimized including pH and concentration of buffering medium, amount concentration of methyl propiolate, derivatization time, and temperature, by the univariate approach. Under optimal conditions, the developed analytical scheme offers a total analysis time of less than 10 min, limits of detection in the range 0.1–0.5 μmol L^?1, and satisfactory linearity up to 100 μmol L^?1 for all analytes. The method proved also to be equally selective and robust. Endogenous thiols were determined in melon, watermelon, and avocado, using the standards addition approach, after minimal sample preparation, with no use of organic solvents. The accuracy was evaluated by recovery experiments resulting in the range of 86.4–118.5 %.     

Simultaneous Detection of Azodicarbonamide and the Metabolic Product Semicarbazide in Flour by Capillary Electrophoresis

In the present work, capillary electrophoresis (CE) was used for the first time for the simultaneous analysis of azodicarbonamide (ADA) and semicarbazide (SEM), and the capillary electrophoresis separation conditions, extraction agents, and derivatization conditions were investigated. In 20 mmol L^?1 sodium tetraborate, 30 mmol L^?1 β-cyclodextrin (β-CD), 17 % isopropanol (v/v), and 25 mmol L^?1 sodium dodecyl sulfate (SDS) running buffer, ADA and SEM previously derivatized with 9-fluorenylmethyl chloroformate (FMOC) were separated in less than 25 min with good sensitivity. The linear ranges were 8.3?×?10^?4～6.6?×?10^?2 mmol L^?1 and 1.9?×?10^?3～3.4?×?10^?2 mmol L^?1, and detection limits (S/N?=?10) were 0.5 and 0.15 mg kg^?1 for ADA and SEM, respectively. The proposed method was successfully applied for the simultaneous analysis of ADA and SEM in five flour samples with satisfactory recovery data from 88.0 to 93.0 % for ADA and 98.0 to 106.0 % for SEM, indicating the valuable potential application of this method for food analysis.     

Antioxidant Activity and Determination of Phenolic Compounds from <Emphasis Type="Italic">Eugenia involucrata</Emphasis> DC. Fruits by UHPLC-MS/MS

Fruits have been the focus of several studies aimed at finding new antioxidant sources for protection against the damage caused by reactive species. In this study, the antioxidant activity and the presence of phenolic compounds in all parts (peel, pulp, and seeds) of Eugenia involucrata DC. fruits were evaluated. DPPH^·, ABTS^·+, and ORAC methods were used to determine the antioxidant activity, and an UHPLC-MS/MS method was developed for determining the phenolic compounds (gallic, chlorogenic, ferulic, p-coumaric and ellagic acids, quercetin, and myricetin). In the determination of both antioxidant activity and phenolic composition, the efficiency of solvents with different polarities—methanol/H₂O (80:20, v/v), ethanol/H₂O (80:20, v/v), methanol/acidified water with phosphoric acid pH 3.00 (80:20, v/v), and ethyl acetate—for the extraction of the phenolic compounds, was also evaluated. All parts of E. involucrata fruits showed antioxidant activity, in the range of 36.68 ± 1.44 to 873.87 ± 18.24 μmol TE g^?1, being the highest values found in the seeds and peel when more polar extraction solvents were used. Six, five, and three phenolic compounds were identified and quantified in the pulp, peel, and seeds, respectively, with the highest abundance as p-coumaric acid (14 ± 2 mg kg^?1) in the pulp, quercetin (47 ± 5 mg kg^?1) in the peel, and gallic acid (74 ± 4 mg kg^?1) in the seeds, also when more polar solvents were used. Although antioxidant activity methods suggested that the peel and seeds have more antioxidant potential, a wider variety of compounds were determined in the pulp.     

Determination of Polyphenol Content by Formation of Unstable Compound Using a Mini-Pump Multicommutation System

This article describes a multicommuted flow procedure for photometric determination of the polyphenol content in wines and teas, exploiting the formation of unstable intermediate products, by the reaction of sodium hypochloride with gallic acid. Because the lifetime of the formed compound is very short, a special flow cell was designed in order to enable mixing of sample and reagent solution within the flow cell, thus allowing signal monitoring, while compound formation proceeded. The flow system manifold comprised three solenoid mini-pumps to propel sample, reagent solution, and carrier fluid. The photometer consisted of a photodiode and a light emitting diode (LED) with maximum emission at 490 nm. Under the selected operational conditions, useful features including a linear response ranging from 62 to 1000 mg L^?1 gallic acid solution (R?=?0.9987), a detection limit of 21 mg L^?1 gallic acid, a sampling rate of 120 determinations per hour, a relative standard deviation of 1.9 % (n?=?20) for a typical solution containing 400 mg L^?1 gallic acid, and a waste generation of 1.0 mL per determination were also achieved. Medium recovery values of 96.2?±?10.4 and 101.9?±?7.3 % for wines and teas, respectively, were achieved.     

Speciation Determination of Selenium in Seafood by High-Performance Ion-Exchange Chromatography-Hydride Generation-Atomic Fluorescence Spectrometry

A high-performance ion-exchange chromatography coupled with hydride generation-atomic fluorescence spectrometry (HPIEC-HG-AFS) method was developed for simultaneous speciation of selenium in seafood. Three selenium species including of selenocystine (Se-Cys), selenome-thionine (Se-Met), and selenite Se(IV) were separated on an anion-exchange column (PRP-X100) with eluent of 30 mM NH₄H₂PO₄ and methanol (39:1, v/v) in 10 min at the flow rate of 1.0 mL min^?1. Variables affecting the HG-AFS detection of selenium species were optimized. The optimum conditions found were the following: reducing agent, 2.0 % of KBH₄, and 5.0 % of HCl; lamp current, 90 mA; photomultiplier tube voltage, 280 V; flow rate of carrier gas, 300 mL min^?1; and shielding gas, 800 mL min^?1. Under the optimized conditions, the good linearity of calibration curves (R ²?>?0.999) between signal of fluorescence and concentration of selenium species was obtained in the range of detection limits (DLs), 80 μg L^?1, and the DLs of Se-Cys, Se-Met, Se(IV) were 1.66, 0.990, 1.10 μg L^?1, respectively. The repeatability of the method, expressed as relative standard deviation, was less than 5.0 % (n?=?10), and the average recoveries for spiked test were from 87.3 to 103 % for three analytes in real seafood samples. The developed HPIEC-HG-AFS method was successfully applied for the speciation of selenium in seafood samples.     

Lemon (Citrus limon, Burm.f.) essential oil enhances the trans-epidermal release of lipid-(A, E) and water-(B6, C) soluble vitamins from topical emulsions in reconstructed human epidermis

Topical bioavailability of lipid‐ and water‐soluble vitamins is a critical issue for protecting or anti‐ageing formulations. Using 17‐day‐old SkinEthic^® reconstructed human epidermis, we investigated (at 34°C) the role of lemon EO in enhancing the penetration of α‐tocopherol (E) and retinyl acetate (A), pyridoxine (B₆) and ascorbic acid (C), released from O/W or W/O emulsions. D‐limonene, α‐pinene and p‐cymene (65.9, 2.2 and 0.5%w/w of the oil) had skin permeability coefficients Ps (10^?3 cm h^?1) of 0.56 ± 0.03 (or 0.73 ± 0.02), 0.72 ± 0.05 (or 0.98 ± 0.05) and 0.84 ± 0.04 (or 1.14 ± 0.04), respectively, when incorporated in a W/O (or O/W) emulsion. Vitamins B6, C and A had Ps values of (3.0 ± 0.4) × 10^?3, (7.9 ± 0.6) × 10^?3 and (0.37 ± 0.02) × 10^?5 cm h^?1, respectively, and their flux through the skin was enhanced by a factor of 4.1, 3.4 and 5.8, respectively, in the presence of lemon EO. The penetration of vitamin E was nine‐fold enhanced. Lemon EO produced only reversible modification of TEWL, and it is a safe and effective penetration enhancer for topical administration of lipid‐ and water‐soluble vitamins.     

Thermal transition and thermo-physical properties of potato (<Emphasis Type="Italic">Solanum tuberosum L</Emphasis>.) var. Russet brown

Potatoes are an important food in many regions of the world and are commonly used in a variety of food products. Thermal transition and thermo-physical properties of potatoes are important in order to design efficient food processes and select appropriate storage conditions. In this study, we determined the thermal transitions and thermophysical properties of raw and blanched/par-fried potato for a temperature range of ??32 to 21.1 °C. Using differential scanning calorimetry, we found an initial freezing point (T_f) at ??1.8?±?0.1 °C, an onset of melting (T_m^′) at ??9.9?±?0.2 °C and an unfreezable water content (X^′_w) for maximally freeze-concentrated raw potato at 0.21 kg water/kg potato. Corresponding values for blanched/par-fried potatoes were ??0.9?±?0.1 °C, ??11.0?±?0.2 °C and 0.18 kg water/kg potato. Results show that an increase in solids content decreased T_f of both raw and blanched potatoes. We modelled the relationship between them using the Chen model. The apparent specific heat (C_app) increased around T_f to 31.7?±?1.13 kJ/kg K for raw potato and 26.7?±?0.62 kJ/kg K for blanched/par-fried potato. For frozen raw potato at ??32 °C, thermal diffusivity (α) was 0.89?±?0.01?×?10?^?6 m²/s and thermal conductivity (k), 1.82?±?0.14 W/m K, respectively. These values were higher for frozen raw potato than for the unfrozen raw potato (0.15?±?0.01?×?10?^?6 m²/s and 0.56?±?0.08 W/m K, respectively at 21.1 °C). The apparent density (ρ) of frozen raw potato (992?±?4.00 kg/m³ at ??32 °C) was less than that for unfrozen raw potato (1053?±?4.00 kg/m³ at 21.1 °C), and a similar trend was obtained for blanched/par-fried potato (993?±?2.00 kg/m³ at ??32 °C and 1188?±?7.00 kg/m³ at 21.1 °C, respectively). This study established a correlation between thermo-physical properties and temperature. Findings may be used to inform the design and optimization of freezing processes and frozen storage for potato products.     

Inactivation of Escherichia coli Population on Fruit Surfaces Using Ultraviolet-C Light: Influence of Fruit Surface Characteristics

Ultraviolet-C (UV-C 254 nm) light is a possible alternative for chemical disinfection of fresh fruits. However, studies on the influence of surface characteristics on the kinetics of UV-C inactivation of microorganisms on fruits are limited. In this study, UV-C inactivation of generic Escherichia coli (ATCC 23716), a nonpathogenic surrogate strain for E. coli O157:H7, was inoculated onto the skin surface intact pear, pear with surface wounds, and the skin surface of intact peach. Disc shaped (0.057 m diameter?×?0.01 m height) fruit surface were exposed at room temperature to UV-C light ranging from 0 to 7.56?±?0.52 kJ/m² and microbial inactivation kinetics was determined. Maximum reductions of 3.70?±?0.125 log CFU/g were achieved for E. coli on intact pear surfaces (P?<?0.05), with lesser reduction on wounded pear (3.10?±?0.329 log CFU/g) and peach surfaces (2.91?±?0.284 log CFU/g) after 4 min UV-C exposure at 7.56 kJ/m² UV. The Weibull scale factor (α) values of UV-C inactivation for E. coli on an intact pear surface was 0.001?±?0.0007 min (0.235?±?0.001 kJ/m²), wounded pear surface, 0.003?±?0.001 min (0.240?±?0.002 kJ/m²) and peach surface, 0.004?±?0.0004 (0.241?±?0.0008 kJ/m²). The time required for a 90 % reduction in E. coli cell numbers or the reliable life time (t _R) calculated with the Weibull model for intact pear surfaces (0.019?±?0.009 min, 0.268?±?0.017 kJ/m²) was smaller than for wounded pear (0.062?±?0.013 min, 0.348?±?0.024 kJ/m²) and peach surfaces (0.074?±?0.012, 0.371?±?0.012 kJ/m²), suggesting that the wounds on pear surfaces and trichomes (100–1000 μm) on peach surfaces helped to shield and protect microorganisms from UV-C radiation. There was likely a more uniform distribution of bacterial cells onto pear surfaces due to its smaller surface roughness, spreading coefficient, and hydrophobic nature compared to peach. Fourier transform infrared spectroscopy indicate that bacterial membrane damage (phospholipids, protein secondary structures, and polysaccharides) and changes to DNA/RNA in E. coli resulted from UV-C treatment. UV-C can reduce E. coli populations on fresh fruit surfaces, but the efficacy of UV treatment is dependent upon the morphological and surface properties of the fruit and surface integrity.     

Determination of Quercetin, Gallic Acid, Resveratrol, Catechin and Malvidin in Brazilian Wines Elaborated in the Vale do São Francisco Using Liquid–Liquid Extraction Assisted by Ultrasound and GC-MS

In this work, a fast and simple methodology has been applied for the determination of gallic acid, resveratrol, catechin and malvidin in Brazilian wines by gas chromatography–mass spectrometry. The procedure included a stage of ultrasound-assisted liquid–liquid extraction and subsequent derivatization with N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) and GC-MS analysis. The limit of detection varied from 0.41 to 1.18 mg?L^?1 in all the analytes. The relative standard deviations calculated for 8.0 and 20 mg?L^?1 were 1.90 and 0.82 % for gallic acid, 3.08 and 1.22 % for catechin, 1.30 and 0.44 % for malvidin, 1.50 and 0.53 % for resveratrol, and 1.41 and 0.61 % for quercetin. The developed methodology was applied for the analysis of red wine samples collected in the São Francisco region, Bahia state, Brazil. Quercetin concentration varied from 2.4 to 3.0 mg?L^?1, gallic acid 21.4–56.3 mg?L^?1, resveratrol 1.5–5.9 mg?L^?1, malvidin 15.3–32.2 mg?L^?1, and catechin 11.71–18.2 mg?L^?1. The obtained concentrations are in agreement with those reported in the literature.     

Physicochemical Characterization of Lemongrass Essential Oil–Alginate Nanoemulsions: Effect of Ultrasound Processing Parameters

The formation of lemongrass oil (1 %?v/v) nanoemulsions in aqueous sodium alginate solution (1 %?w/v) containing Tween 80 (1 %?v/v) as nonionic surfactant was studied in terms of droplet size, electrical charge, viscosity, and whiteness index considering different ultrasonication times (0, 30, 60, 120, and 180 s) and amplitudes (30, 60, and 100 μm). The droplet size and size distribution of the emulsions decreased at increasing treatment time and amplitude. The minimum average droplet size observed in nanoemulsions was 4.31?±?0.18 nm with a narrow size distribution. The interface electrical charge of the coarse emulsion was ?18.0?±?2.9 mV, whereas in ultrasonicated nanoemulsions, it diminished up to ?55.8?±?6.4 mV when the sonication time was extended for 180 s. The viscosity of nanoemulsions also decreased at increasing treatment time and amplitude. Moreover, nanoemulsions became translucent after sonicating for 180 s at 30, 60, or 100 μm with whiteness indices of 28.61?±?0.17, 27.93?±?0.21, and 27.86?±?0.33, respectively. Therefore, it can be stated that ultrasound processing might be a feasible technology to produce highly translucent lemongrass oil–alginate nanoemulsions, with extremely small droplet sizes and high stability to be used as delivery systems of essential oils in food products. However, it is necessary to investigate the effect of ultrasound processing parameters on the antimicrobial potential of essential oils incorporated to nanoemulsions.     

Effects of Gellan-Based Edible Coating on the Quality of Fresh-Cut Pineapple During Cold Storage

The effects of gellan-based [gellan gum 0.56 % (w/v), glycerol 0.89 % (w/v) and sunflower oil 0.025 % (w/v)] edible coating on the respiration rate, physico-chemical properties and microbiological and sensory quality of fresh-cut pineapple during 16 days of storage (5?±?1 °C, 85?±?10 % RH) were evaluated. Uncoated fresh-cut pineapple was stored under the same condition and served as the control. For cross-linking reaction which was necessary for gel formation of gellan gum, a 2 % (w/v) calcium chloride solution that contained 1 % (w/v) ascorbic acid and 1 % (w/v) citric acid (as antibrowning agents) was used. The results obtained show that the respiration rate and weight loss of gellan-based coated samples were significantly (p?<?0.05) lower than those of the uncoated samples during 16 days of storage at 5 °C. In addition, coated samples significantly (p?<?0.05) maintained the firmness and colour of fresh-cut pineapple during low-temperature storage as compared to uncoated samples. The results obtained in this study also indicate that pH, titratable acidity and total soluble solids of coated and uncoated samples showed little changes during 16 days of storage at 5 °C. Gellan-based formulation did not show any antimicrobial effect, and no significant (p?>?0.05) differences were found among total plate counts and yeast and mould counts for coated and uncoated samples. Total plate counts and yeast and mould counts for coated and uncoated samples reached 10⁶ CFU/g (limit of shelf life acceptance for fruit-based products recommended by the Institute of Food Science and Technology in the UK) after 12 days of storage at 5 °C. In addition, the scores for all sensory characteristics at day 12 were significantly (p?<?0.05) higher in coated samples as compared to control. Therefore, the results obtained in this study indicate that gellan-based edible coating formulation has the potential to maintain the quality of fresh-cut pineapple during low-temperature storage for about 12 days.     

Use of Multivariate Optimization to Develop Methods for Direct Copper and Lead Determination in Breast Milk by Graphite Furnace Atomic Absorption Spectrometry

A direct method for lead and copper determination in breast milk by graphite furnace atomic absorption spectrometry, using aqueous calibration, was proposed in this study. Samples were diluted with hydroximethylaminomethane 80 %?v/v, pH 8. The dilution determination for Pb and Cu was 1:1 and 1:9, respectively. Fractional factorial (2^4?1) and central composite designs were used to optimize experimental conditions (pyrolysis and atomization temperatures, pyrolysis time, and modifier) using 10 μL samples introduced into a graphite furnace. The methods allowed for copper and lead determination under optimized conditions with an aqueous calibration curve between 0 and 180 μg L^?1 for Cu and 0 and 48 μg L^?1 for Pb. The detection limits were 0.92 μg L^?1 and 6.4 μg L^?1 for Pb and Cu, respectively. Intra and inter-assay studies revealed coefficients of variation of 5.0 and 6.3 %, and 6.4 and 5.5 % for Pb and Cu, respectively. Recovery studies at three concentration levels (three consecutive days, n?=?7/day) presented results between 107 and 109 % for Pb and 102 and 103 % for Cu. Good accuracy was obtained for both metals through recoveries studies using certified reference material (infant formula NIST® 1846). The method determined lead and copper in six samples and the concentrations ranged from 2.90 to 27.9 μg L^?1 for Pb and 384 to 1,212 μg L^?1 for Cu. While copper is an essential element, lead has no nutritional function and is cumulative at low concentrations. Therefore, safe, efficient, and validated methods should be available to determine its concentration in breast milk.     

Beer Clarification Using Ceramic Tubular Membranes

In this work, laboratory-made green beers were produced using a commercial hopped malt extract and used to study their cross-flow microfiltration (CFMF) performance in a bench-top plant, appropriately designed and equipped with ceramic tubular membrane modules with nominal pore size of 0.4, 0.8, or 1.2 μm, under different values of the initial green beer turbidity (H?≡?0.7–61.9 European Brewery Convention (EBC) unit), feed superficial velocity (v _S?≡?2–6 m s^?1), and transmembrane pressure difference (TMPD?≡?0.97–4.73 bar) under constant temperature (~10 °C). Whatever the membrane pore size and rough beer turbidity, the minimum quasi-steady-state value of the overall membrane resistance \( \left({\mathrm{R}}_{\mathrm{T}}^{*}\right) \) was obtained at TMPD of 3 to 4 bar and v _S?=?6 m s^?1. The 0.8-μm pore membrane was selected for the loss in the permeate density, and color was limited, while the volumetric permeation flux was high enough. Then, it was used to assess a double logarithmic trend between the quasi-steady-state permeation flux (J*) and beer turbidity with a limiting flux of 63?±?6 L m^?2 h^?1 for H?>?21 EBC units. Precentrifuged beer feeding resulted in 2.7- to 4.1-fold increase in J* with respect to the above limiting flux, provided that the haze level of rough beer had been reduced to 1.0 or 0.7 EBC unit, respectively. The cake filtration fouling mechanism was identified as the main reason for flux decline by analyzing mathematically the time course of both the experimental permeate volume and permeation flux data. By operating with the aforementioned clarified green beers at TMPD of 3.73 bar, v _S of 6 m s^?1, and periodic CO₂ backflushing, the average permeation flux (300–385 L m^?2 h^?1) resulted to be from three to five times higher than that (80–100 L m^?2 h^?1) at 0–2 °C claimed by the three commercial CFMF processes currently available.     

Differential Pulse Voltammetric Assay of Coffee Antioxidant Capacity with MWNT-Modified Electrode

Multi-walled carbon nanotube-modified glassy carbon electrode (GCE) has shown electrocatalytic activity toward electrochemical oxidation of hydroxycinnamic acids (chlorogenic, caffeic, p-coumaric and ferulic), i.e. decrease of the overpotential on 0.1–0.29 V and two- to threefold increase of oxidation currents in comparison with bare GCE under conditions of cyclic voltammetry. Oxidation of compounds under investigation is a diffusion-controlled process that is confirmed by linear dependence of peak currents on the v ^1/2 (R ²?=?0.9944–0.9998) and peak potentials on the logarithm of v (R ²?=?0.9805–0.9996). The differential pulse voltammetry has been applied for the hydroxycinnamic acid quantification. The calibration graphs linearity is continued in 2–5.5 order of concentrations. The approach developed has been utilized for coffee antioxidant capacity (AC) assay based on oxidation of hydroxycinnamic acids containing in coffee beans. Chlorogenic, caffeic and ferulic acids are the contributors to AC that was confirmed by standard addition method. The AC has been expressed in chlorogenic acid equivalents per 100 mL of coffee. AC of instant coffee is statistically insignificant lower than that for ground coffee (148?±?103 and 197?±?50 mg per 100 mL, p?>?0.05). Positive correlation has been observed between chlorogenic acid equivalent AC of coffee and ferric reducing power based on coulometric titration with electrogenerated hexacyanoferrate(III) ions (r?=?0.9602).     

Caffeine Content of Retail Market Coffee in Portugal

How much caffeine does one ingest when drinking a simple cup of coffee in Portugal? The study presented herein tried to answer this question through the assessment of caffeine content of commercially available espresso coffee samples, both caffeinated and decaffeinated, using a high-performance liquid chromatography assay. Caffeine was rapidly separated from the sample matrix using a RP-18 column (250?×?4 mm i.d., 5 μm). The flow rate was 1.0 mL/min and the mobile phase consisted of water acidified with 5% of orthophosphoric acid/methanol (35:65, v/v). Caffeine was detected directly at 273 nm. The assay was validated for linearity, lower limit of quantification and limit of detection, precision, accuracy, and stability. Seventeen different brands of caffeinated coffee and six of decaffeinated coffee were analyzed. As for capsule coffee, eight caffeinated and two decaffeinated blends were analyzed. The caffeine content of caffeinated coffee varied from 53.8?±?5.9 to 141.3?±?5.3 mg/cup, whereas for caffeinated capsule coffee caffeine concentrations ranged from 45.0?±?5.3 to 60.8?±?6.2 mg/cup. As for decaffeinated coffee, caffeine concentrations ranged from 0.96?±?0.04 to 3.9?±?0.1 mg/cup and for decaffeinated capsule coffee from 0.93?±?0.04 to 1.2?±?0.1 mg/cup.     

Determination of Benzalkonium Homologues and Didecyldimethylammonium in Powdered and Liquid Milk for Infants by Hydrophilic Interaction Liquid Chromatography–Mass Spectrometry

In this study, a hydrophilic interaction liquid chromatography–mass spectrometry (HILIC-MS/MS) method for the determination of benzalkonium (BAC) homologues and didecyldimethylammonium (DDAC) was developed. A satisfactory chromatographic separation of BAC homologues and DDAC was achieved using, as mobile phase, acetonitrile–aqueous 50 mM ammonium formate (pH 3.2) (93?+?7 v/v) at 0.3 mL min^?1. The elution order of BAC homologues was from benzyldimethylhexadecylammonium chloride (C₁₆-BAC) to benzyldimethyldecylammonium chloride (C₁₀-BAC), the exact opposite with respect to separation using reversed liquid chromatography. The instrumental method was successfully applied to powdered and liquid milk for infants (about 50 samples). From powdered milk samples, BAC and DDAC were extracted using 5 % formic acid in methanol for 60 min at 60 °C in an ultrasonic bath; after dilution with water and 5 % NH₄OH solution, a purification step using a weak cationic exchange column was performed. Satisfactory limit of detections (LODs) were achieved, below 1.0 μg kg^?1 and 0.05 μg L^?1 for powdered and liquid milk for infants, respectively. No sample was free of BAC homologues and DDAC, and in one powdered milk sample, the contamination level exceeded 500 μg kg^?1, the maximum level recommended by the Standing Committee on the Food Chain and Animal Health for food and feed.     

Validation of a HS-SPME-GC Method for Determining Higher Fatty Esters and Oak Lactones in White Rums

Higher fatty esters and oak lactones are the main components of white rum aroma and furthermore, they have an important sensorial impact in these distilled alcoholic beverages. A method for analyzing these volatile compounds was validated. It involves a separation and concentration step using headspace solid-phase microextraction (HS-SPME) and determination by capillary gas chromatography using flame ionization detection. The method showed a good within-day (RSD?<?3 %) and between-day precision (RSD?<?5 %). The calibration curves were linear at the tested ranges (R?>?0.99) and the limits of detection and quantification were 0.001–0.018 and 0.003–0.054 mg L^?1 (12 %?v/v alcohol), respectively. Good recoveries were obtained (98.6–100.3 %). The method is suitable for the quality control of higher fatty esters and oak lactones in white rums.     

Rapid Detection of Four Organophosphorous and Neonicotinoid Toxicants Using Bi-enzyme Tracer Competitive Enzyme-Linked Immunosorbent Assay

A bi-enzyme tracer direct competitive enzyme-linked immunosorbent assay (dc-ELISA) based on two generic antibodies was developed. The effects of several physicochemical factors, such as heterologous antigen–horseradish peroxidase (HRP), methanol concentration, ionic strength, and pH value, were optimized to obtain satisfactory sensitivity of the assay. Under the optimized conditions, the 50 % inhibition concentration (IC₅₀) value for parathion, parathion-methyl, imidaclothiz, and imidacloprid was 57.28?±?2.73, 169.82?±?5.64, 52.48?±?3.46, and 53.08?±?2.05 μg L^?1, with a limit of detection (LOD, IC₁₀) of 0.56, 3.16, 0.62, and 0.51 μg L^?1, respectively. There was no obvious cross-reactivity (CR) with most of the neonicotinoids and organophosphorus pesticides. The recoveries of parathion, parathion-methyl, imidaclothiz, and imidacloprid in environmental and agricultural samples, including river water, soil, and cabbage, ranged from 82.54 to 116.29 %. The relative standard deviation (RSD) ranged from 1.59 to 8.09 %. The ELISA results were confirmed by gas chromatography (GC) with a high correlation coefficient of 0.9882. These results showed that the bi-enzyme tracer competitive enzyme-linked immunosorbent assay could be used as a sensitive tool for monitoring parathion, parathion-methyl, imidaclothiz, and imidacloprid in environmental samples and agricultural products.