A Case Study on Optimization of Biomass Flow During Single-Screw Extrusion Cooking Using Genetic Algorithm (GA) and Response Surface Method (RSM)

In the present study, response surface method (RSM) and genetic algorithm (GA) were used to study the effects of process variables like screw speed, rpm (x ₁), L/D ratio (x ₂), barrel temperature (°C; x ₃), and feed mix moisture content (%; x ₄), on flow rate of biomass during single-screw extrusion cooking. A second-order regression equation was developed for flow rate in terms of the process variables. The significance of the process variables based on Pareto chart indicated that screw speed and feed mix moisture content had the most influence followed by L/D ratio and barrel temperature on the flow rate. RSM analysis indicated that a screw speed?>?80 rpm, L/D ratio?>?12, barrel temperature?>?80 °C, and feed mix moisture content?>?20% resulted in maximum flow rate. Increase in screw speed and L/D ratio increased the drag flow and also the path of traverse of the feed mix inside the extruder resulting in more shear. The presence of lipids of about 35% in the biomass feed mix might have induced a lubrication effect and has significantly influenced the flow rate. The second-order regression equations were further used as the objective function for optimization using genetic algorithm. A population of 100 and iterations of 100 have successfully led to convergence the optimum. The maximum and minimum flow rates obtained using GA were 13.19?×?10^?7 m³/s (x ₁?=?139.08 rpm, x ₂?=?15.90, x ₃?=?99.56 °C, and x ₄?=?59.72%) and 0.53?×?10^?7 m³/s (x ₁?=?59.65 rpm, x ₂?=?11.93, x ₃?=?68.98 °C, and x ₄?=?20.04%).     

Freezing Efficiency and Quality Attributes as Affected by Voids in Plant Tissues During Ultrasound-Assisted Immersion Freezing

Voids, filled with air, in plant tissues, can attenuate ultrasound, resulting in weakening the effectiveness of ultrasound during immersion freezing. The effect of voids on ultrasound-assisted immersion freezing (UF) in selected plant tissues, apple, radish, and potato was investigated in the present study. The freezing time and quality attributes of firmness, drip loss, total calcium content, and total phenolic content were investigated in apple, radish, and potato samples treated by normal immersion freezing (IF) and UF. The results showed that the more the percentage voids in the plant tissues, the lower the effectiveness of the ultrasound treatment. The total freezing time reduction (%) due to UF was a power function of the volume of voids (%): y?=?0.018x^?1.057 (R²?=?0.994). Ultrasound at 0.62 W/cm² (28 kHz) resulted in the best firmness and lowest drip loss in potato, while no significant (p?>?0.05) differences in quality attributes were observed between IF and UF in apple samples. These findings indicated that UF was more effective in freezing fruit or vegetables with a highly dense structure.     

A mathematical model for moisture movement during continous and intermittent drying of <Emphasis Type="Italic">Eucalyptus saligna</Emphasis>

A modified diffusion-based mathematical model is proposed to describe the moisture movement during continuous and intermittent drying of Eucalyptus saligna. This model includes the temperature change, the surface drying coefficient (β _n ) and 2 diffusion coefficients [from green to FSP (D _f ) and from FSP to dry condition (D _o )] as important parameters. The final model expression obtained was M?=?exp (??25 β _n ² D _t /l²) with the β _n used was 1.5807 kg m^?2 s^?1, the D _f was 2.26?×?10^?11 m² s^?1, and the D _o was 5.85?×?10^?12 m² s^?1. The range of temperature change between heating and non-heating phases in the intermittent drying regimes was from 24.9 to 31.8 °C. The R² values obtained when the model was fitted into the drying data of different intermittent regimes ranged from 71.5 to 85.9%. The R² value was 87.4% when the model was fitted into continuous trial data. The high values of R² indicate that the model can be used to understand the moisture reduction both in intermittent and continuous regimes.     

Smart NMR Method of Measurement of Moisture Content of Vegetables During Microwave Vacuum Drying

Microwave drying is usually combined with vacuum environment in conjunction with hot air flow to draw the moisture rapidly. The moisture content of the vegetables undergoing drying is hard to measure online. This research designed a microwave vacuum drying (MVD)-low-field nuclear magnetic resonance (NMR) smart device and investigated the feasibility of NMR method for online measurement of state of moisture during MVD. The relation between the signal amplitude (A ₂) and the true moisture content (M ₁) of six kinds of vegetables (mushroom, carrot, potato, lotus, edamame, vegetable corn) was fitted to estimate if NMR can measure the M ₁ of vegetables directly. Results showed that A ₂ and M ₁ of different fresh vegetables had no single empirical mathematical model to fit. However, for each kind of these vegetables, the A ₂ and corresponding M ₁ in different MVD stages showed a significant linear relationship. The predicted moisture content (M ₂) of mushroom: M ₂ = 5.25351 × 10^?4 A ₂ ? 0.34042, R = 0.996; carrot: M ₂ = 5.78756 × 10^?4 A ₂ ? 0.14108, R = 0.998; potato: M ₂ = 3.10019 × 10^?4 A ₂ ? 0.10612, R = 0.991; lotus: M ₂ = 2.32415 × 10^?4 A ₂ ? 0.01573, R = 0.998; edamame: M ₂ = 3.13310 × 10^?4 A ₂ ? 0.4198, R = 0.996; vegetable corn: M ₂ = 1.69461 × 10^?4 A ₂ ? 0.09063, R = 0.995. The linear models between M ₂ and A ₂ were able to estimate the end point (M ₁ < 8%) of MVD with a high accuracy (P > 0.950).     

Steady- and Unsteady-State Determination of the Water Vapor Permeance (<Emphasis Type="Italic">WVP</Emphasis>) of Polyethylene Film to Estimate the Moisture Gain of Packed Dry Mango

The water vapor permeance (WVP; g m^?2 d^?1 Pa^?1) of packaging films quantifying the water vapor transfer rate between foods and its surroundings is usually determined in units operating under steady-state conditions that do not necessarily reflect food handling scenarios. This study evaluated the determination of the WVP of a polyethylene (PE) film by steady-state method ASTM F1249-06 using a permeability cell and unsteady-state method ASTM E96/E96M in which 102 vacuum-sealed PE bags containing silica gel were stored (37.8 °C, 75% relative humidity) and weighed over 25 days. Average steady-state WVP (2.935 ± 0.365 × 10^?3, n = 4) fell within the 95% quantiles of unsteady-state WVP values (1.818–3.183 × 10^?3, n = 2142). Moisture uptake of dehydrated mango stored at 37.8 °C and 75% relative humidity was predicted with WVP values obtained by both methods. Predictions were validated by monitoring over 25 days the weight gain of 100 PE bags with dry mango. Experimental moisture averages during storage fell within one standard deviation of predictions using the unsteady-state WVP (R ² = 0.974). The same was observed only until day 15 for predictions obtained with the steady-state WVP. Calculations for days 20–25 overestimated the moisture uptake by 6.0–7.2%, resulting in registered R ² = 0.924. The unsteady-state WVP determination is low-cost, uses large numbers of film samples, and allowed more accurate predictions of dry mango moisture uptake. Knowledge of the moisture uptake controlled by the film WVP is essential when predicting the safety and quality changes limiting the shelf-life of foods.     

A TLC-HPLC Method for Determination of Thiamphenicol in Pig,Chicken, and Fish Feedstuffs

An effective thin-layer chromatography (TLC) purification procedure coupled to high-performance liquid chromatography (HPLC) method was developed for the determination of thiamphenicol (TAP) in pig, chicken, and fish feedstuffs. The feedstuff samples were extracted with ethyl acetate, defatted with n-hexane saturated with acetonitrile, and further purified by TLC. The chromatographic separation was performed on a Waters Symmetry C₁₈ column using an isocratic procedure with acetonitrile-water (21.7:78.3, v/v) at 0.6 mL/min. The ultraviolet (UV) detector was set at a wavelength of 225 nm. The TAP concentrations in feedstuff samples were quantified using a standard curve. Good linear correlations (y?=?162,630x???2381.7, r?>?0.9998) were achieved within the concentration range of 0.05–10.00 μg/mL. The recoveries of TAP spiked at levels of 1, 10, and 100 μg/g ranged from 82.0 to 114.9% with the intra-day and inter-day relative standard deviation (RSD) less than 9.0%. The limit of detection (LOD) and limit of quantitation (LOQ) were 0.02 and 0.03 mg/kg for pig feedstuffs, 0.02 and 0.04 mg/kg for chicken feedstuffs, and 0.02 and 0.03 mg/kg for fish feedstuffs, respectively. This reliable, simple, and cost-effective method could be applied to the routine monitoring of TAP in animal feedstuffs.     

Validated RP-HPLC Method for Simultaneous Determination of Tocopherols and Tocotrienols in Whole Grain Barley Using Matrix Solid-Phase Dispersion

The vitamers of vitamin E such as α-, β-, γ-, and δ-tocotrienol and α-, β-, γ-, and δ- tocopherol are important phytochemical compounds with antioxidant activity and with potential benefits for human health. A high-performance liquid chromatography with fluorescence detection (HPLC-FLD) method was validated for their determination in whole grain barley samples. Tocol extraction was performed by an optimized matrix solid-phase dispersion (MSPD) protocol with neutral alumina (0.5 g) as the dispersion agent and methanol (5 mL) as the elution solvent. The analytical column was an Eclipse XDB C18 column (150?×?4.6 mm, 5 μm) and it was operated at room temperature. Mobile phase was consisted of methanol/acetonitrile/i-propanol (55:40:5?v/v?%) and the elution was isocratic at a flow rate of 0.8 mL/min. Total analysis time was 12 min, and the detection of the tocols was performed with a fluorimetric detector where the excitation and emission wavelengths were set at 295 and 335 nm, respectively. Method validation was performed by means of intra-day (n?=?5) and inter-day accuracy and precision (n?=?8), sensitivity, and linearity. The linear regression coefficient (R ²) was higher than 0.99. The recoveries of the tocols from barley samples with the proposed extraction method were in an acceptable level (74–91 %) where the relative standard deviation ranged from 4.2 to 15.0 %. Limits of detection (LODs) and limits of quantification (LOQs) varied from 0.03 to 0.11 mg kg^?1 and 0.11 to 0.34 mg kg^?1, respectively.     

Dehydrofreezing of Apple Fruits: Freezing Profiles,Freezing Characteristics,and Texture Variation

The present study deals with the dehydrofreezing of apples. Fresh samples (700 % db) and samples dehydrated up to different water contents (200, 100, and 30 % db) were frozen at high practical freezing rate (PFR⁺) and low practical freezing rate (PFR^?). The effects of water content (W) and practical freezing rate (PFR) were investigated in terms of freezing characteristics: initial freezing temperature (IFT), practical freezing time (PFT), specific freezing time (SFT), thaw exudate water (TEW), and texture (maximum puncture force as index of firmness). Only high W samples (700 and 200 % db) had a significant impact of PFR in terms of PFT, SFT, and TEW. IFT decreased sharply with the decrease in the sample W. PFT greatly depended on PFR for fresh apples. PFT varied from 86 to 329 min for fresh apples at PFR⁺ and PFR^?, respectively, whereas it was lower than 32 min for samples with W?=?30 % db. SFT decreased, equally, with sample W decrease. The TEW of fresh frozen samples, during thawing, was approximately 12 g/100 g water for low PFR (PFR^?), whereas it was lower than 3 g/100 g water for samples with W?=?200 % db at the same PFR. Moreover, the impact of PFR on TEW was significant and very important for high W samples. Finally, the firmness increased when W decreased for both PFR⁺ and PFR^?. Nevertheless, an insignificant impact of PFR on apple firmness was found. Thus, partial removal of water constitutes a promising solution to prevent the negative impacts of freezing on apple fruit firmness.     

Combined Application of Fluorescence Spectroscopy and Chemometrics Analysis in Oxidative Deterioration of Edible Oils

Combined methods of fluorescence spectrometry with chemometrics were used to monitor oxidation deterioration of edible oil. Synchronous and three dimensional fluorescence spectroscopy techniques were proposed for monitoring palm oil, camellia oil, sunflower oil and perilla oil during oven accelerated oxidation. Principal component analysis plot of fluorescence intensity (λex = 320–700 nm) clearly showed oxidative evolution of oils over heating time. High saturated or monounsaturated oils exhibited high regression coefficients between peroxide values and fluorescence intensity (R ²  = 0.973 for 400 nm in palm oil; R ²  = 0.956 for 370 nm in camellia oil). High diunsaturated oil exhibited high regression coefficient between nonpolar carbonyl compounds and fluorescence intensity (R ²  = 0.970 for 370 nm in sunflower oil). High triunsaturated oil exhibited high regression coefficient between p-anisidine value and fluorescence intensity (R ²  = 0.938 for 665 nm in perilla oil). In conclusion, Fluorescence spectroscopy is a rapid and green nondestructive method for oxidation monitoring. Differences of fatty acid compositions played key rules in formation of oxidation products and evolution of fluorescence spectra.     

In situ density estimation of timber pieces by drilling residue analysis

Density values are essential for the characterization of wood elements in existing structures. A new method for the in-situ density estimation of timber pieces is proposed based on weighting the residue generated by conventional drilling. This research includes the design and development of a residue collector device coupled to a conventional drill and testing on four Spanish coniferous species: Laricio pine, Scots pine, Radiata pine and Maritime pine (Pinus nigra Arn., Pinus sylvestris L., Pinus radiata D. Don. and Pinus pinaster Ait., respectively). For each species, 44 specimens (except Scots pine, with 42) 60?×?90 mm cross-section and 150 mm length (half radial and half tangential orientation) were tested. Specimen density was obtained by mass/volume ratio. Three 8 mm diameter 46.5 mm deep holes were drilled in each specimen using a brad point bit. The drilling residue was weighed and density was calculated as a ratio to bore volume. Although only slightly smaller, residue density statistically differs from average specimen density. But the specimen density can be inferred by the correlation, statistically significant, with residuals drilling density (R²?=?80.7%) and even better with residual drilling mass (R²?=?84.4%).     

Glucose Biosensor Based on a Glassy Carbon Electrode Modified with Multi-Walled Carbon Nanotubes-Chitosan for the Determination of Beef Freshness

In this study, the glucose biosensor was developed for the determination of the beef meat freshness based on a glassy carbon electrode (GCE) modified with multi-walled carbon nanotubes (MWCNTs) and chitosan (Chi). Glucose oxidase (GOx) was immobilized onto the MWCNTs-Chi/GCE surface by cross-linking the enzyme through glutaraldehyde with bovine serum albumin (BSA). Glutaraldehyde solution (0.25%, w/w) was also added to prevent enzyme release. The properties of the developed biosensor were characterized with cyclic voltammetry (CV), differential pulse voltammetry (DPV), and electrochemical impedance spectroscopy (EIS) using [Fe (CN)₆]^3?/4?as the supporting electrolyte. The influence of various parameters was investigated, and 0.1 mol L^?1 PBS with pH = 6.4 was chosen as the optimal supporting electrolyte for this experiment. The linear relationship between the current and the concentration of glucose was obtained from 0.2 to 1.2 mmol L^?1, with a detection limit of 0.05 mM at a signal-to-noise ratio of 3 and displayed good linearity (R ² = 0.9902), while the biosensor showed a rapid response to glucose. In addition, the developed glucose biosensor was applied in the determination of glucose in beef as an indicator of beef freshness compared to the total volatile basic nitrogen (TVB-N) method. The glucose level was decreased with increasing beef storage time.     

Non-destructive Assessment of Guava (<Emphasis Type="Italic">Psidium guajava</Emphasis> L.) Maturity and Firmness Based on Mechanical Vibration Response

Storage potential and eating quality of guava (Psidium guajava L.) fruit depend on its maturity. Segregation of guava according to maturity and firmness measured using non-destructive technologies would help the industry to designate ripe fruit to immediate market and less ripe fruit for distant market (e.g., exportation). This research was conducted to evaluate the potential of experimental resonant frequency (f _e) and elasticity index (EI) to estimate fruit firmness, which has been reported to be inversely correlated to its maturity. A maturity index (I _m) was calculated as the ratio of total soluble solids/titratable acidity (TSS/TA). It was proved that TSS, TA, and I _m were significantly correlated (P?<?0.05) to skin firmness (F _s), flesh firmness (F _f), stiffness (S), and analytical resonant frequency (ω _n ), being S the attribute best fitted to I _m (R ²?=?0.77). Since it was observed that f _e and EI were sensitive to changes in fruit firmness, both of them were explored as alternatives to predict F _s, F _f, S, and ω _n of guava fruit. In some cases, EI improved the models to predict guava firmness traits (e.g., F _s vs f _e had a coefficient of determination of R ²?=?0.58, whereas for F _s vs EI, it was R ²?=?0.62). The best model occurred when plotting ω _n vs f _e (R ²?=?0.86), followed by S vs EI (R ²?=?0.84), making these promising features for the development of a new practical application using frequency response measurement as a non-destructive method to assess guava maturity.     

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.     

A Rapid and Specific Biosensor for <Emphasis Type="Italic">Salmonella</Emphasis> Typhimurium Detection in Milk

This paper reports the application of an amperometric biosensor for rapid and specific Salmonella Typhimurium detection in milk. This device was developed from self-assembled monolayer technique on a gold screen-printed electrode, using cysteamine thiol. Polyclonal antibodies were oriented by protein A immobilization. The biosensor structure was characterized by cyclic voltammetry, Fourier transform infrared spectroscopy, and scanning electron microscopy. The analytical response was obtained by a chronoamperometry technique, using a direct-sandwich peroxidase-labeled system. The biosensor device showed a qualitative behavior with a very low limit of detection of 10 CFU mL^?1 and a detection time of 125 min. The biosensor specificity was demonstrated in pure and mixed samples with strains of Escherichia coli and Citrobacter freundii. The performance of the biosensor was found satisfactory, and the device was tested in skimmed and whole milk samples, being able to detect S. Typhimurium quickly, without an enrichment step. This structure of immunosensor assembly can be expended in future studies for other food matrices and bacterial species, making it a useful tool to ensure food safety.     

Modeling the Inactivation of <Emphasis Type="Italic">Listeria innocua</Emphasis> and <Emphasis Type="Italic">Escherichia coli</Emphasis> in Fresh-Cut Tomato Treated with Pulsed Light

The effectiveness of pulsed light (PL) treatments to inhibit microorganisms on fresh-cut tomatoes (Lycopersicon esculentum Mill., cv. Daniela) was investigated. Tomato slices inoculated with Escherichia coli or Listeria innocua were exposed to PL treatments (4, 6, or 8 J cm^?2 fluence) and kept cold at 4 °C for 20 days. L. innocua and E. coli counts, gases in the headspace of the containers (O₂ and CO₂), pH, titratable acidity, and soluble solid content were monitored throughout the cold storage. The PL treatments reduced significantly (p < 0.05) initial loads of both microbes. The effect of the PL fluence on the survival number of microoganisms was described by a log-linear model (R ² = 0.849–0.999). At any fixed time within the cold storing, the microbial counts for untreated samples were always higher than those cut tomatoes that had been previously PL-treated. The behavior of L. innocua and E. coli during the storage were well adjusted (R ² > 0.930) by Gompertzian models; the studied microorganisms exhibited different patterns during the storage period. On the other hand, O₂ and CO₂ partial pressures in containers with fresh-cut tomatoes were also significantly affected by PL treatments (p < 0.05). The highest PL fluence caused the greatest changes of O₂ and CO₂ contents. In addition, the application of PL triggered an acceleration of the O₂ consumption during the cold stage. PL treatments might be used to effectively extend the safety of fresh-cut tomatoes over 12 days of storage against E. coli and L. innocua growth.     

Optimization of Ultrasound-Assisted Extraction of Lycopene from Papaya Processing Waste by Response Surface Methodology

Lycopene possesses strong antioxidant ability, which may provide protection against cancer and other degenerative diseases. An ultrasound-assisted extraction method has been developed for the extraction of lycopene from papaya (Carica papaya L.) processing waste. Optimization conditions were firstly determined using single factor experiment, and then response surface methodology was used. Analysis showed that second-order polynomial models produced a satisfactory fitting of the experimental data with regard to lycopene (R ²?=?0.9147, P?<?0.001). The optimal conditions were 42.28 % ethanol in ethyl acetate as a solvent and extraction for 26.09 min at 50.12 °C. Under these conditions, the maximum yield of lycopene was 189.8?±?4.5 μg/g fresh weight (FW), which was higher than that obtained using the traditional extracting method (153.9?±?7.8 μg/g FW) and the Soxhlet extraction method (68.3?±?4.1 μg/g FW). The crude extract obtained could be used as either food additive or for further isolation and purification of lycopene. The results obtained are helpful for full utilization of papaya.     

Improved Detection of Ascorbic Acid with a Bismuth-Silver Nanosensor

Bismuth-silver bimetallic nanoparticles glassy carbon electrode (Bi-AgNPs/GCE) was employed for the determination of ascorbic acid (AA) in fruit and pharmaceutical samples. In this study, the Bi-AgNPs/GCE showed excellent electrochemical catalytic activities toward AA oxidation compared with bare GCE. Ascorbic acid gave a sensitive oxidation peak at 0.23 V using differential pulse voltammetry. Under optimized experimental conditions, the limit of detection for AA was 0.16 μM (for S/N?=?3), the analytical range for AA was between 0.4 and 1.2 μM (R ²?=?0.994) and the RSD was 5.84 % (n?=?10). The proposed method showed good stability, reproducibility, and repeatability as well as good recovery in fruit and pharmaceutical samples.     

Validation of HPLC-UV Methods for the Quantification of Betaine in Foods by Comparison with LC-MS

The importance of dietary betaine is increasingly recognized. The aim of this study was to develop a simple high-performance liquid chromatography with standard ultraviolet spectrometric detection (HPLC-UV) method for betaine (N,N,N-trimethylglycine) determination in foods after derivatization. Two methods were used for betaine derivatization. Thereafter, derivatized betaine was quantified using HPLC-UV, and the results were compared with liquid chromatography mass spectrometry (LC-MS). The established derivatizing agent 2′-naphthacyl triflate and a novel derivatizing agent 2-bromo-2′-acetonaphthone produced the same cationic derivative when they react with betaine. The calibration curves were linear up to 1000 μmol/L (R ²?=?0.9974 for 2′-naphthacyl triflate and 0.9995 for 2-bromo-2′-acetonaphthone). The limit of detection was 1 μmol/L for both methods (2′-naphthacyl triflate and 2-bromo-2′-acetonaphthone), confirming sufficient sensitivity for betaine quantification in foods. The average recovery from different food matrices (wheat flour and spinach) (n?=?12) was 99?±?9 %, 95?±?10 %, and 101?±?8 % for LC-MS, 2′-naphthacyl triflate, and 2-bromo-2′-acetonaphthone, respectively. Inter- and intra-assay coefficients of variation (CVs) in the control samples (whole wheat flour) were below 10 %. Quantitative results for foods analyzed using 2′-naphthacyl triflate and 2-bromo-2′-acetonaphthone were comparable to LC-MS (R ²?=?0.992 and 0.990), respectively. The highest betaine content (~160 mg/100 g) was found in spinach followed by faba bean, wheat flour, and beetroot. These methods can be widely used for betaine quantification because of the simplicity of the derivatization procedures, and the commercial availability of the derivatizing reagent (2-bromo-2′-acetonaphthone) or through the relatively easy synthesis of 2-naphthacyl triflate.     

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.     

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.