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.     

Design of Sonotrode Ultrasound-Assisted Extraction of Phenolic Compounds from <Emphasis Type="Italic">Psidium guajava</Emphasis> L. Leaves

Psidium guajava L. has gained a special attention as health plant due to the presence of phenolic compounds. Box-Behnken design (BBD) has been applied for the extraction of target compounds from guava leaves via sonotrode ultrasound-assisted extraction (UAE). Different extraction times (5, 30, and 55 min), ratios of ethanol/water (50, 75, and 100% (v/v)), and ultrasound (US) power (80, 240, and 400 W) were tested to find their effect on the sum of phenolic compound (SPC), flavonols and flavan-3-ols via HPLC-ESI-QqQ-MS, and antioxidant activity (DPPH and TEAC assays). The best process conditions were as follows: 40 min, 60% ethanol/water (v/v), and 200 W. Established method has been used to extract phenolic compounds in two guava leaves varieties (pyrifera and pomifera). Pyrifera var. showed greater values of the SPC via HPLC-ESI-QqQ-MS (49.7 mg/g leaf dry weight (d.w.)), flavonols (12.51 mg/g d.w.), flavan-3-ols (7.20 mg/g d.w.), individual phenolic compounds, and antioxidant activity (8970 ± 5 and 465 ± 6 μmol Trolox/g leaf d.w, respectively) than pomifera var. Conventional extraction showed lower amounts of phenolic compounds (7.81 ± 0.03 and 4.64 ± 0.01 mg/g leaf d.w. for flavonols and flavan-3ols, respectively) in comparison to the ultrasound-assisted ones.     

Preparation and Release Behavior of Gelatin-Based Capsules of Antioxidants from Ethanolic Extracts of Thai Riceberry Bran

This study aimed to devise an environment-friendly and effective, yet simple and practicable, antioxidant extraction and encapsulation method from Riceberry bran, whose extract was used thereafter for developing highly efficient antioxidant capsules. Ethanolic Riceberry bran extracts with high total phenolic content, total flavonoid content, total anthocyanin content, and antioxidant activity (using DPPH radical scavenging activity and ferric reducing antioxidant power assay) were obtained using ultrasonic-assisted extraction. The optimum conditions for producing the capsules, such as types of gelatin, concentrations of gelatin, and the Riceberry bran extract concentrations, were studied. Capsules produced by incorporating 1% (w/v) of acid-treated gelatin (type A) and 1% (w/v) of Riceberry bran extract yielded higher chemical properties. When dispersed in water at 37 °C, the capsules exhibited a high release of antioxidants. Moreover, the capsule showed a lower degradation rate of antioxidants under simulated gastrointestinal conditions compared to the crude extract.     

Dispersive Liquid–Liquid Microextraction Combined With Micellar Electrokinetic Chromatography for the Determination of Some Photoinitiators in Fruit Juice

A fast and simple technique composed of dispersive liquid–liquid microextraction (DLLME) and micellar electrokinetic chromatography (MEKC) with diode array detector (DAD) was developed for the determination of multi-photoinitiators in fruit juice. Seven photoinitiators were separated in MEKC using a 25 mM borate buffer of pH 8.0, containing 24 mM sodium dodecyl sulfate (SDS), 10 mM β-cyclodextrin (β-CD), and 12.5 % acetonitrile (v/v). A CD-modified MEKC made this method more suitable for the determination of isopropylthioxanthone (ITX) isomers including 2-IXT and 4-ITX than the recently prescribed methods. A DLLME procedure was used as an offline preconcentration strategy. The satisfactory recoveries obtained by DLLME spiked at two spiked levels ranged from 85.6 to 124.7 % with relative standard deviations (RSDs) below 14 %. The limits of quantification (LOQs) ranged from 2.1 to 6.0 μg kg^?1.     

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.     

Characterization of Biodegradable Films Based on <Emphasis Type="Italic">Salvia hispanica</Emphasis> L. Protein and Mucilage

Biodegradable films of chia by-products (mucilage and protein-rich fraction (PF)) incorporated with clove essential oil (CEO) were obtained and characterized. The effects of polymer concentration (PC; 1.0–3.0 %, w/v) and CEO concentration (0.1–1.0 %, v/v) were evaluated as well as the pH (7–10), using a 2³ factorial design with four central points. The films exhibited moisture values between 11.6 and 52.1 % (d.b.), which decreased (p?<?0.05) with increasing PC and CEO. The thickness of the films increased (p?<?0.05) with increasing PC. PC and pH influenced (p?<?0.05) the lightness (L) and variation in color between red and green (a). The orientation of the color to yellow-blue hues (b) decreased significantly (p?<?0.05) with increasing PC. Transparency was significantly lower and higher (p?<?0.05) than PC and CEO, respectively. The film surface morphology was evaluated using atomic force miscrocope images, and thermogravimetric analysis (TGA) was performed to study the thermal stability of the films. The displacement and tensile strength were significantly lower (p?<?0.05) at higher concentrations of CEO, this variable being the only one with a significant effect. The chemical composition of the films was confirmed utilizing Fourier transform infrared (FTIR) spectroscopy. The proportion of CEO added to the films had a significant influence on antimicrobial activity, inhibiting the growth of both Escherichia coli and Staphylococcus aureus.     

Automated Sequential Injection Method for Determination of Caffeine in Coffee Drinks

An automated sequential injection analysis spectrophotometric assay for the determination of purine alkaloids in coffee drinks was developed. The sample was treated with a carrez reagent for matrix suppression followed by filtration; subsequently, alkaloids were separated from organic acids using a short C18 monolithic column (10 × 4.6 mm). The flow rate of the separation step was 10 μL s^?1 with 10% v/v of methanol as the mobile phase. The sum of alkaloids evaluated as caffeine was detected at 274 nm. The influence of the main parameters affecting the quantification of purine alkaloids was optimized. One sample analysis lasted 15 min when aspirated in triplicate. The linear range was 1–15 mg L^?1, and the determination coefficient (r ²) was 0.9969. The limit of detection and limit of quantitation were 0.128 and 0.425 mg L^?1, respectively. The repeatability evaluated as the relative standard deviation (RSD) was 3.58% (n = 12, 10 mg L^?1). Under optimal conditions, the method was successfully applied to determine purine alkaloids in different real samples including soluble coffee, coffee from an espresso machine, and brewed coffee drinks.     

Optimization of Extraction Parameters of Total Phenolics from <Emphasis Type="Italic">Annona crassiflora</Emphasis> Mart. (Araticum) Fruits Using Response Surface Methodology

In this study, response surface methodology was used to optimize the extraction temperature (25–75 °C) and ethanol concentration (0–70 %, ethanol/water, v/v) to maximize the extraction of total phenolic compounds (TPC) from araticum pulp. The efficiency of the extraction process was monitored over time, and equilibrium conditions were reached between 60–90 min. A second-order polynomial model was adequately fit to the experimental data with an adjusted R ² of 0.9793 (p < 0.0001) showing that the model could efficiently predict the TPC content. Optimum extraction conditions were ethanol concentration of 46 % (v/v), extraction temperature of 75 °C and extraction time of 90 min. Under the optimum conditions, the araticum pulp showed high TPC content (4.67 g GAE/100 g dw) and also high antioxidant activity in the different assays used (46.56 μg/mL, 683.65 μmol TE/g and 1593.72 μmol TE/g for DPPH IC₅₀, TEAC and T-ORAC_FL, respectively). From our extraction procedure, we successfully recovered a significantly higher amount of TPC compared to other studies in the literature to date (1.5–22-fold higher). Furthermore, TPC and antioxidant activity were present in the fruit in levels that are difficult to find in other common fruits. These results expose a potential approach for improving human health through consumption of araticum fruit.     

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.     

Tocopherols and Tocotrienols: an Adapted Methodology by UHPLC/MS Without Sample Pretreatment Steps

Ultra high-performance liquid chromatography-electrospray ionization-mass spectrometry (UHPLC/ESI/MS) methodology was adapted for identification and quantification of tocopherols and tocotrienols in vegetable oils with no derivatization or sample preparation steps. The UHPLC analysis was performed using a C18 column and mobile phase composed of methanol: water: ammonium hydroxide (99:1:0.1 v/v/v) and isopropanol. A single mass spectrometer with electrospray on negative mode was used as a detector for tocopherols and tocotrienols. The samples were diluted in isopropanol. The limit of quantification for tocopherols was 0.006 μg mL^?1, and the linear range was 0.006 to 0.01 μg mL^?1; for tocotrienols, the limit of quantification was 0.002 μg mL^?1, and the linear range of analysis was 0.002 to 0.003 μg mL^?1. The correlation coefficients were higher than 0.99, indicating that the method has suitable linearity. The methodology has proven to be precise, reproducible, and robust for the parameters studied.     

Optimization of Matrix Solid-Phase Dispersion Method for Extraction of Aflatoxins from Cornmeal

An extraction method for simultaneous determination of aflatoxins (AFLAs) G2, G1, B2, and B1 in cornmeal, based on vortex-assisted matrix solid-phase dispersion (MSPD) and high-performance liquid chromatography (HPLC) with fluorescence detection was optimized by a central composite design, validated and applied. Multivariate analysis was performed to evaluate the effect of cornmeal composition on AFLA extraction. The amount and proportion of solid support (celite and C18) and volume of elution solvent (methanol and acetonitrile) were the variables tested. The mobile phase of methanol/acetonitrile/water (24:14:62, v/v/v) in isocratic elution mode provided satisfactory AFLA separation. The best recoveries (85.7 to 114.8%) were obtained when the sample preparation contained 25 mg C18 as solid support and 10 mL of elution solvent. The limits of detection ranged from 0.01 to 0.04 ng g^?1, and the limits of quantification varied from 0.02 to 0.1 ng g^?1. The optimized method was suitable for coarse and medium grind cornmeal. Multivariate correlation analysis showed that the main interferers for AFLA recovery were proteins and sugars.     

LC-ESI-MS/MS Analysis and Extraction Method of Phenolic Acids from Gluten-Free Precooked Buckwheat Pasta

In many countries, common buckwheat (Fagopyrum esculentum Möench) has been cultivated for its nutritive value as food ingredient. This plant is a rich source of vitamins and exogenic amino acids. Many of the health-promoting effects of F. esculentum have been attributed to a large amount of phenolic compounds. Presented in this paper, precooked buckwheat pasta, produced by extrusion cooking, is a gluten-free product without any technological additives. Moreover, it contains natural polyphenolic antioxidants and therefore could be classified as convenience food. The phenolic acid compositions of precooked buckwheat pasta were as follows: gallic, protocatechuic, gentisic, 4-OH-benzoic, vanillic, trans-caffeic, cis-caffeic, trans-p-coumaric, cis-p-coumaric, trans-ferulic, cis-ferulic, and salicylic. A very important step of sample pretreatment before quantitative analysis is the choice of extraction conditions. Therefore, in this study, before quantitative analysis (liquid chromatography-mass spectrometry, LC-ESI-MS/MS), optimization of ultrasound-assisted extraction (UAE) of phenolic acids from precooked buckwheat pasta was performed. The most effective conditions for the isolation of phenolic acids from precooked buckwheat pasta with the use of UAE were as follows: 80 % aqueous ethanol, 60 °C, ultrasound frequency 20 kHz, power 100 W, and time 40 min.     

Effect of Tannin Extracts on Biofilms and Attachment of <Emphasis Type="Italic">Escherichia coli</Emphasis> on Lettuce Leaves

Lettuce is often involved in foodborne outbreaks caused by pathogenic Escherichia coli. Current control strategies have often proved ineffective to ensure safe food production. For that reason, the present study compared the efficacy of tannin extracts and chlorine treatments on the reduction of E. coli ATCC 25922 adhered to lettuce leaves. E. coli was inoculated artificially on leaf surfaces of fresh crisp lettuce. Effectiveness of water, chlorine (200 mg/L), and three commercial available tannin extracts from Acacia mearnsii De Wild. (tannin AQ (2 %, w/v), tannin SG (1 %, v/v) and tannin SM (1 %, v/v)) treatments was evaluated using the viable plate count method and scanning electron microscopy (SEM). SEM results revealed that bacterial cells are attached as individual cells and in clusters to the leaf surface after 2 h of incubation. Biofilm formation was observed after 24 h of incubation. The tannin SM treatment was able to reduce counts in approximately 2 log CFU/cm² on leaf segments. However, treatment was less effective in the reduction of E. coli counts after 24 h of incubation when compared to 2 h incubation of the same extract. The results suggest that the tannin SM extract diminishes E. coli counts adhered to and under biofilm formation on lettuce leaves and its effect is similar to the use of chlorine solutions.     

Novel Intact Bitter Cassava: Sustainable Development and Desirability Optimisation of Packaging Films

Novel biomaterials and optimal processing conditions are fundamental in low-cost packaging material production. Recently, a novel biobased intact bitter cassava derivative was developed using an intrinsic, high-throughput downstream processing methodology (simultaneous release recovery cyanogenesis). Processing of intact bitter cassava can minimise waste and produce low-cost added value biopolymer packaging films. The objective of this study was to (i) develop and characterise intact bitter cassava biobased films and (ii) determine the optimal processing conditions, which define the most desirable film properties. Films were developed following a Box-Behnken design considering cassava (2, 3, 4 % w/v), glycerol (20, 30, 40 % w/w) and drying temperature (30, 40, 50 °C) and optimised using multi-response desirability. Processing conditions produced films with highly significant (p?<?0.05) differences. Developed models predicted impact of processing conditions on film properties. Desirable film properties for food packaging were produced using the optimised processing conditions, 2 % w/v cassava, 40.0 % w/w glycerol and 50 °C drying temperature. These processing conditions produced films with 0.3 %; transparency, 3.4 %; solubility, 21.8 %; water-vapour-permeability, 4.2 gmm/m²/day/kPa; glass transition, 56 °C; melting temperature, 212.6 °C; tensile strength, 16.3 MPa; elongation, 133.3 %; elastic modulus, 5.1 MPa and puncture resistance, 57.9 J, which are adequate for packaging applications. Therefore, intact bitter cassava is a viable material to produce packaging films that can be tailored for specific sustainable, low-cost applications.     

Chlorophyll Fluorescence Imaging for Monitoring the Effects of Minimal Processing and Warm Water Treatments on Physiological Properties and Quality Attributes of Fresh-Cut Salads

In this study, chlorophyll fluorescence imaging (CFI) was used to monitor plant stress induced by cutting of mini romaine lettuce (Lactuca sativa L. var. longifolia) and by cutting and washing of endive (Cichorium endivia L.) during storage. Regarding the more detailed study of endive fresh-cut salads, we additionally monitored respiratory activity, phenylalanine ammonia lyase (PAL) activity, contents of plant pigments, and cut edge browning. Determination of maximum quantum efficiency F _v/F _m was feasible through sealed consumer-sized film bags, thus, enabling the non-invasive monitoring of both fresh-cut salad types in the corresponding modified atmosphere during storage. Cutting of romaine lettuce provoked a partially reversible drop of F _v/F _m during the first 24 h. Subsequently, F _v/F _m of cut romaine strongly decreased with elapsing shelf life, whereas intact leaves exhibited only a slight decline. Regarding minimally processed endive, warm water washing progressively reduced F _v/F _m with increasing heat exposure, while respiratory activities and the content of accessory pigments remained unaffected. The heat-dependent decrease of F _v/F _m was correlated to the inhibition of the PAL activity. Mildly warm washing (40 °C, 120 s; 45 °C, 60 s) reduced PAL activities, while F_v/F_m remained widely unaffected and visual quality was only partially improved. However, warm water washing at elevated temperatures (45 °C, 120 s; 50 °C, 30–60 s) enabled maximum visual quality retention, accompanied by a significant decrease of F _v/F _m. CFI may represent a useful tool to monitor the stress conditions due to cutting and warm water treatments, hence, allowing the systematic improvement of fresh-cut produce.     

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.     

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).     

Simultaneous Determination of Five Neonicotinoid Insecticides in Edible Fungi Using Ultrahigh-Performance Liquid Chromatography-Tandem Mass Spectrometry (UHPLC-MS/MS)

A robust analytical method for simultaneously determining five neonicotinoid insecticides (clothianidin, dinotefuran, imidacloprid, thiacloprid, and thiamethoxam) in commonly consumed edible fungi (Agaricus bisporus, Flammulina velutipes, Hypsizygus marmoreus, Lentinus edodes, and Pleurotus eryngii) was provided in the present study. Samples were pretreated using a modified QuEChERS (quick, easy, cheap, efficient, rugged, and safe) method with the detection of neonicotinoids by ultrahigh-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). A number of optimizations performed to sample pretreatment and detection conditions were discussed. Limits of detection (LODs) for all analytes in edible fungi were between 0.03 and 0.7 μg kg^?1, while limits of quantitation (LOQs) ranged from 0.1 to 2 μg kg^?1. Mean recoveries for clothianidin, dinotefuran, imidacloprid, thiacloprid, and thiamethoxam were in the range of 100.5–118.0, 73.9–89.5, 88.6–117.8, 72.9–121.8, and 98.9–117.2%, respectively, with RSDs less than 8.1%. This method could be used for fast screen of the five neonicotinoid insecticides in edible fungi for risk assessing aims.     

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.     

Determination of Baclofen Residue in Muscle,Liver, Kidney and Fat of Swine by Liquid Chromatography-Tandem Mass Spectrometry

Baclofen was illegally used in veterinary clinical medicine as a growth-promoting agent. To date, few methods have been developed for the monitoring of baclofen in animal tissues. In this study, a sensitive and efficient liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to identify and quantify baclofen in the muscle, liver, kidney, and fat of swine was developed and validated. Baclofen was extracted from tissues with ammonium acetate buffer (pH 5.2) and isolated with isopropyl-ethyl acetate (4:6, v/v). Then, a solid phase extraction using MCX cartridge was used to clean up the extracts. The elution was evaporated to dryness and reconstituted with water/methanol (90:10 v/v). All samples were determined by LC-MS/MS system through positive ionization in a multiple reaction monitoring (MRM) mode. The proposed method was validated by evaluation of specificity, linearity, recovery, accuracy, precision, LOD, and LOQ values according to Commission Decision 2002/657/EC. Estimated limit of quantification for baclofen in the muscle, liver, kidney, and fat of this method was 1.00 μg/kg, respectively. The mean intra- and inter-day assay accuracies fell within a range 88.5–93.9% and 86.2–93.2%, respectively. The mean intra- and inter-day precisions were 1.78 and 4.95% (RSD < 15%), respectively. The proposed method has proved to be suitable for accurate quantitative determination of baclofen for residue analysis.