Preparation of a barley bran protein–gelatin composite film containing grapefruit seed extract and its application in salmon packaging

The physical properties of a composite film prepared from barley bran protein and gelatin (BBG) were investigated. Tensile strength (TS) and elongation at break (E) values of the BBG film decreased as barley bran protein content increased. TS increased with increasing gelatin content, but E values decreased. The optimal conditions for the preparation of the BBG film were 3 g barley bran protein, 3 g gelatin, and 1 g sorbitol in 100 mL film-forming solution. In order to inhibit the growth of pathogenic bacteria, a BBG film containing grapefruit seed extract (GSE) was prepared. After 15 days of storage, populations of Escherichia coli O157:H7 and Listeria monocytogenes inoculated on salmon packaged with the BBG film containing GSE decreased by 0.53 and 0.50 log CFU/g, respectively, compared to the control. Also, packing salmon with the BBG film containing GSE decreased the peroxide value and thiobarbituric acid value by 23.0% and 23.4%, respectively.     

Biodegradable gelatin–chitosan films incorporated with essential oils as antimicrobial agents for fish preservation

Essential oils of clove (Syzygium aromaticum L.), fennel (Foeniculum vulgare Miller), cypress (Cupressus sempervirens L.), lavender (Lavandula angustifolia), thyme (Thymus vulgaris L.), herb-of-the-cross (Verbena officinalis L.), pine (Pinus sylvestris) and rosemary (Rosmarinus officinalis) were tested for their antimicrobial activity on 18 genera of bacteria, which included some important food pathogen and spoilage bacteria. Clove essential oil showed the highest inhibitory effect, followed by rosemary and lavender. In an attempt to evaluate the usefulness of these essential oils as food preservatives, they were also tested on an extract made of fish, where clove and thyme essential oils were the most effective. Then, gelatin–chitosan-based edible films incorporated with clove essential oil were elaborated and their antimicrobial activity tested against six selected microorganisms: Pseudomonas fluorescens, Shewanella putrefaciens, Photobacterium phosphoreum, Listeria innocua, Escherichia coli and Lactobacillus acidophilus. The clove-containing films inhibited all these microorganisms irrespectively of the film matrix or type of microorganism. In a further experiment, when the complex gelatin–chitosan film incorporating clove essential oil was applied to fish during chilled storage, the growth of microorganisms was drastically reduced in gram-negative bacteria, especially enterobacteria, while lactic acid bacteria remained practically constant for much of the storage period. The effect on the microorganisms during this period was in accordance with biochemical indexes of quality, indicating the viability of these films for fish preservation.     

Active chitosan–chestnut extract films used for packaging and storage of fresh pasta

A tannins-rich chestnut extract was used to enhance the antioxidant and antibacterial properties of chitosan-based film materials. The favourable mechanical properties of the novel material enabled its application in the preparation of the sachets that were used for packing and storage of filled fresh pasta. The fresh pasta ageing progressed in conventional refrigerated storage conditions of 8 °C with 60 ± 2% relative humidity in the absence of light for 60 days. The rapid moisture mobility between a starchy food and sachets during the first 9 days of storage induced retrogradation of the fresh pasta, whereby total phenolic content show dependency on moisture throughout the shelf life. Active components within the sachet prevented microbial growth on the food surface during the entire 60 days.     

β-Galactosidase-immobilised microreactor fabricated using a novel technique for enzyme immobilisation and its application for continuous synthesis of lactulose

In this study, several surface functionalisation techniques were used to immobilise β-galactosidase in a microreactor. β-Galactosidase was pretreated with lactose before immobilisation, and functionalised multi-walled carbon nanotubes (MWNTs), DNA-wrapped single-walled carbon nanotubes and glutaraldehyde as a linker were used to immobilise β-galactosidase on a microchannel surface. When functionalised MWNTs were used as a linker for immobilisation of pretreated β-galactosidase, the enzyme microreactor showed the highest performance. The K_m(app) and V_max were 2.84 mM and 0.52 mM/min, respectively, and the conversion of o-nitrophenyl-β-d-galactopyranoside (ONPG) reached 78.3% during the continuous flow reaction at a flow rate of 2.5 μL/min. In an enzyme microreactor, continuous synthesis of lactulose was performed, and the lactulose concentration was maintained at about 1.29 g/L for 48 h.     

Soluble starch–based biodegradable and microporous microspheres as potential adsorbent for stabilization and controlled release of coix seed oil

Soluble starch–based biodegradable and microporous microspheres (SDM-Ms) were prepared by emulsion chemical cross-linking technique using trisodium trimetaphosphate (TSTP) as the cross-linker. The resultant amorphous SDM-Ms were excellently identified by scanning electron microscopy (SEM), X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FT-IR). The internal rupture and surface-controlled erosion were the predominant degradation mechanisms for SDM-Ms. The obtained SDM-Ms were applied to adsorb coix seed oil (CSO) by immersing method. The adsorption capacity of CSO within SDM-Ms was determined, namely 0.5238 g/g, and the thermal stability was shown higher than that of the free CSO. A burst release appeared in the second hour, followed by controlled release. Diffusion, degradation, and erosion mechanisms might coexist for the full release processes. The soluble starch (Ss) was demonstrated a promising biodegradable polymer for preparing the porous microspheres. Meanwhile, after being adsorbed into the SDM-Ms, the CSO can be powerfully applied in food and pharmaceutical industries.     

Development and characterization of an edible chitosan–whey protein nano composite film for chestnut (Castanea mollissima Bl.) preservation

Chitosan (CHI) and whey protein are usually used to prepare edible films for food preservation. However, the composite film composed of the two components does not yield satisfactory properties for chestnut preservation. In this study, nano-cellulose and cinnamaldehyde (CMA) were added to CHI and whey protein, creating a new composite film with strong water retention, bacteriostatic, and mechanical properties. The water vapor permeability (WVP) of the film decreased by 21.61% with the addition of 0.5% (w/v) nano-cellulose, and 23.02% with the addition of 0.3% (w/v) CMA. Furthermore, water solubility (WS) decreased 22.05%, and the density of the film was significantly improved with the addition of 0.3% (w/v) CMA. The optimized formula of the film was CHI 2.5% (w/v), whey protein 3.0% (w/v), nano-cellulose 0.5% (w/v), CMA 0.3% (w/v), and pH 3.8, as determined by orthogonal testing L9(3⁴), with fuzzy comprehensive assessment, of WVP, WS, tensile strength, and elongation at break. The film clearly inhibited the growth of E. coli, S. aureus, and Chinese chestnut fungus, destroying the mycelial structure of the fungus. In addition, coating effectively reduced the weight loss, mildew rate, and calcification index during 16 days of storage of chestnuts at 25 °C.     

Comparison of headspace-SPME-GC–MS and LC–MS for the detection and quantification of coumarin,vanillin, and ethyl vanillin in vanilla extract products

A headspace-solid phase micro-extraction (HS-SPME) GC–MS method has been developed for the determination of coumarin, vanillin and ethyl vanillin in vanilla products. Limits of detection ranged from 1.33 to 13.2 ng mL⁻¹. Accuracy and precision data for the method were measured and compared to those obtained using LC-ESI-MS. A survey of 24 commercially available vanilla products was completed using both techniques. No coumarin was detected in any of the samples. Examination of the GC–MS chromatograms revealed the presence of 18 other flavor related compounds in the samples. The method validation and sample analysis data using HS-SPME-GC–MS were comparable to those obtained using the LC–MS method. Because the two methods are conceptually different from one another, both methods would not be subject to the same interferences. This would allow them to be used as confirmatory methods for each other.     

Prediction equations for Warner–Bratzler shear force using principal component regression analysis in Brahman-influenced Venezuelan cattle

A database consisting of 331 beef animals (Brahman-crossbred) was used to determine the multivariate relationships between carcass and beef palatability traits of Venezuelan cattle and to develop prediction equations for Warner–Bratzler shear force (WBSF). The first three principal components (PC) explained 77.53% of the standardized variance. Equations were obtained for each sex class and the total variability observed in WBSF could be explained by its orthogonal regression with carcass weight (CW), fat cover (FC), fat thickness (FT), and skeletal maturity (SM). Prediction equations were: WBSF_steers = 3.566 + 0.003(CW) − 0.033(FC) − 0.015(FT) + 0.0004(SM); WBSF_heifers = 4.824 + 0.002(CW) − 0.229(FC) + 0.096(FT) − 0.064(SM); WBSF_bulls = 3.516 + 0.009(CW) + 0.154(FC) − 0.129(FT) − 0.006(SM). A higher proportion of the variation was explained by the PC when variables of greater weight were selected to define each PC. The equation set presented herein could become an important tool to improve the Venezuelan carcass grading system.     

Coating of Sol–Gel Film on Silver Nanodendrite as a Novel Solid-Phase Microextraction Fiber for Determination of Volatile Aldehydes in Edible Oils

In this work, a novel solid-phase microextraction fiber was fabricated by a new substrate applied for quantitative analysis of trace volatile aldehydes emitted during thermal oxidation of edible oils, analyzed by GC–MS. Ag nanodendrites as a porous substrate, spontaneously coated on a Cu wire, and polydimethylsiloxane/polyethylene glycol (PDMS/PEG) were deposited onto the substrate by sol–gel dip-coating. Parameters affecting the extraction efficiency, such as the substrate porosity, extraction time and temperature, and desorption time and temperature were investigated and optimized. The desorption temperature was chosen as 260 °C, and desorption time was set at 3 min. Results shows that extraction efficiency of sol–gel coating deposited on Ag nanodendrite substrate is meaningfully higher than that of deposited on bare Cu wire. Under the optimum conditions, the limits of detection (LODs) ranged between 0.5 to 0.2 μg/L. The relative standard deviations including repeatability (within fibers) and reproducibility (between fibers) varied between 7.5–11.2 and 9.3–16.2%, respectively.     

Multiresidue method for determination of 88 pesticides in berry fruits using solid-phase extraction and gas chromatography–mass spectrometry: Determination of 88 pesticides in berries using SPE and GC–MS

A method using solid phase extraction (SPE) cleanup followed by gas chromatography–mass spectrometry (GC–MS) has been established for quantitative determination of 88 pesticide residues in berry fruits including raspberry, strawberry, blueberry and grape. Based on an appraisal of the characteristics of GC–MS, validation experiments were conducted for 88 pesticides. In the method, solid-phase extraction was carried out using Envi-Carb cartridge coupled with NH₂-LC cartridge with acetonitrile–toluene (3:1, v/v) as the eluted solvent. In the linear range of each pesticide, the correlation coefficient was R² ? 0.99. At the low, medium and high three fortification levels of 0.05–0.5 mg kg⁻¹, recoveries fell within 63–137%. The relative standard deviation was between 1% and 19% for all 88 pesticides. Low limits of detection (0.006–0.05 mg kg⁻¹) and quantification (0.02–0.15 mg kg⁻¹) were readily achieved with this method for all tested pesticides.     

Confirmatory method for the determination of various acetylgestagens in animal kidney fat using liquid chromatography–tandem mass spectrometry

A confirmatory method has been developed and validated that allows for the simultaneous detection of medroxyprogesterone acetate (MPA), megestrol acetate (MGA), melengestrol acetate (MLA), chlormadinone acetate (CMA) and delmadinone acetate (DMA) in animal kidney fat using liquid chromatography–tandem mass spectrometry (LC–MS/MS). The compounds were extracted from kidney fat using acetonitrile, defatted using a hexane wash and subsequent saponification. Extracts were then purified on Isolute? CN solid-phase extraction cartridges and analysed by LC–MS/MS. The method was validated in animal kidney fat in accordance with the criteria defined in Commission Decision 2002/657/EC. The decision limit (CCα) was calculated to be 0.12, 0.48, 0.40, 0.63 and 0.54 µg kg^–1, respectively, for MPA, MGA, MLA, DMA and CMA, with respective detection capability (CCβ) values of 0.20, 0.81, 0.68, 1.07 and 0.92 µg kg^–1. The measurement uncertainty of the method was estimated at 16, 16, 19, 27 and 26% for MPA, MGA, MLA, DMA and CMA, respectively. Fortifying kidney fat samples (n = 18) in three separate assays showed the accuracy of the method to be between 98 and 100%. The precision of the method, expressed as % RSD, for within-laboratory reproducibility at three levels of fortification (1, 1.5 and 2 µg kg^–1 for MPA, 5, 7.5 and 10 µg kg^–1 for MGA, MLA, DMA and CMA) was less than 5% for all analytes.     

A sensitive immunochromatographic assay using colloidal gold–antibody probe for rapid detection of fumonisin B1 in corn

A sensitive immunochromatographic assay (ICA) using a colloidal gold–antibody probe for the rapid detection of fumonisin B₁ (FB₁) in corn samples was developed. The colour density of the test line correlated with the concentration of FB₁ in the range 2–40 ng ml^–1 by the assay, and the detection limit for FB₁ was 2 ng ml^–1. The linear range for FB₁ was 50–1000 µg kg^–1, and the visual limit detection of the test was 1000 µg kg^–1 in corn samples. The ICA to detect FB₁ is sensitive, specific and rapid. Specific anti-FB₁ monoclonal antibody (mAb) and FB₁-ovalbumin (FB₁-OVA) conjugate antigen were prepared. FB₁ mAb, labelled with colloidal gold, was used as the probe on the immunochromatographic strip. FB₁-OVA and goat-anti-mouse IgG were coated onto a nitrocellulose (NC) membrane as test lines and control lines, respectively. FB₁ in samples will competitively combines the FB₁ mAb with the FB₁-OVA in an NC membrane and the results are directly observed by the colour of the detection and quality control lines. The concentrations of FB₁ mAb labelled with colloidal gold, detecting antigen and goat anti-mouse IgG, were optimised. The results indicate that the test strip is specific for FB₁, with no cross-reactivity to other toxins. The strip assay for FB₁ was simple, only needing one step without complicated assay performance and expensive equipment, and the total time for visual evaluation was less than 10 min. A survey of 24 corn samples from Hefei, China, was performed with the test strip and HPLC, and the detection results showed that the developed ICA and the HPLC were in excellent agreement. Hence, the developed ICA can be used as a method for rapid detection of FB₁ in corn samples.     

A sensitive immunochromatographic assay using colloidal gold–antibody probe for the rapid detection of semicarbazide in meat specimens

A rapid immunochromatographic assay (ICA) was developed for the detection of semicarbazide (SEM), a nitrofurazone metabolite in meat specimens. Colloidal gold–labeled monoclonal antibody specific to a SEM derivative, 4[(4-carboxyphenyl)methylene]-hydrazinecarboxamide (CPSEM), was used as a probe for the presence of SEM. The assay is based upon the competitive reactivity theory that SEM derivatized with 4-carboxybenzaldehyde (4-CBA) competes with CPSEM-conjugated bovine serum albumin for binding the colloidal gold–labeled monoclonal antibody, the result of which could be read directly by naked eyes. Under optimal conditions, the visual detection limit is 0.72 ng mL⁻¹, which demonstrated the high sensitivity of this assay. The stability test indicated that the immunochromatographic strips could be used within 7 weeks at room temperature without significant loss of activity. Spiked pork samples were detected by ICA and confirmed by enzyme-linked immunosorbent assay (ELISA). The assay time for SEM detection was within 5 min, suitable for a rapid on-site testing for meat samples.     

Pepper leaf matrix as a promising analyte protectant prior to the analysis of thermolabile terbufos and its metabolites in pepper using GC–FPD

During gas chromatography (GC), the matrix can deactivate the active site during the transport of the compound from the injector to the detector. This deactivation capacity varies among matrices, as it is dependant on the concentrations of the different constituent compounds of each matrix. During the analysis of terbufos and its metabolites, two of its metabolites were highly thermolabile, and were readily decomposed inside the GC system. As the matrix can mask the active site, we carried out a matrix-matched calibration in an effort to protect the analyte against decomposition. As a component of our analysis, the pepper matrix was the first to be matched; however, it failed to completely protect the metabolites. Subsequently, a variety of different compounds, including 3-ethoxy-1,2-propanediol, gulonolactone, and sorbitol at 10, 1, and 1 mg/mL were tested; however, none of these generated the desired effect. We surmised that some of the compounds may have decomposed inside the injection port, so we introduced a carbofrit inlet liner, which is highly inert. But, this step did not improve the protective qualities of the matrices. Finally, pepper leaf matrix was added to the pepper matrix, and we observed a profound protective effect for almost all of the analytes tested. A selective detector (flame photometric detector with phosphorus filter) was used to facilitate a high matrix concentration without interaction with the analyte. After resolving the problem of these two metabolites, terbufos and its five toxic metabolites were analyzed in pepper and pepper leaf samples. The recovery rates for terbufos and its metabolites were 73–114.5% with a relative standard deviation of <12%. This method was successfully applied to field samples, and terbufos sulfone, terbufos sulfoxide, and terbufoxon sulfoxide were found as residues in the suspected pepper and pepper leaf samples.     

A method for the determination of acrylamide in a broad variety of processed foods by GC–MS using xanthydrol derivatization

A novel GC–MS method was developed for the determination of acrylamide, which is applicable to a variety of processed foods, including potato snacks, corn snacks, biscuits, instant noodles, coffee, soy sauces and miso (fermented soy bean paste). The method involves the derivatization of acrylamide with xanthydrol instead of a bromine compound. Isotopically labelled acrylamide (d ₃-acrylamide) was used as the internal standard. The aqueous extract from samples was purified using Sep-Pak? C₁₈ and Sep-Pak? AC-2 columns. For amino acid-rich samples, such as miso or soy sauce, an Extrelut? column was used for purification or extraction. After reaction with xanthydrol, the resultant N-xanthyl acrylamide was determined by GC–MS. The method was validated for various food matrices and showed good linearity, precision and trueness. The limit of detection and limit of quantification ranged 0.5–5 and 5–20?µg?kg^?1, respectively. The developed method was applied as an exploratory survey of acrylamide in Japanese foods and the method was shown to be applicable for all samples tested.     

Improved method for the determination of 12 non-nutritive sweeteners and monitoring in various foods using liquid chromatography–tandem mass spectrometry

An improved and highly sensitive method was developed and validated for the determination of 12 (7 permitted and 5 non-permitted in Korea) non-nutritive sweeteners in various foods using liquid chromatography-electrospray ionisation-tandem mass spectrometry. The chromatographic separation was performed on an Xbridge BEH C18 column (3 mm × 100 mm, 2.5 μm) with gradient elution using 10 mM ammonium acetate in water and 10 mM ammonium acetate in methanol. Sample preparation consisted of simple dilution, homogenisation, centrifugation and purification with a C18 cartridge prior to analysis. The relative matrix effect (%ME) was within ±20% for all sweeteners. The method also showed good linearity (R² > 0.99). The limit of detection and limit of quantification values in sample were in the range of 0.02–2.66 and 0.06–8.05 mg kg^?1, respectively. The recoveries at three concentration levels ranged between 80% and 119%, with relative standard deviation values below 10%. In addition, the expanded uncertainties determined for 12 sweeteners in 5 different food matrices were confirmed to be <14%. Finally, the method was successfully applied to the analysis of sweeteners in 681 food samples purchased in Korea, Australia and Turkey. These results demonstrate that the method is suitable for the simultaneous determination of multiple-sweeteners in a variety of foods.