An HS-SPME method was developed using multivariate experimental designs, which was conducted in two stages. The significance of each factor was estimated using the Plackett-Burman (P-B) design, for the identification of significant factors, followed by the optimization of the significant factors using central composite design (CCD). The multivariate experiment involved the use of Minitab® statistical software for the generation of a 2(7-4) P-B design and CCD matrices. The method performance evaluated with internal standard calibration method produced good analytical figures of merit with linearity ranging from 1 to 500 μg/kg with correlation coefficient greater than 0.99, LOD and LOQ were found between 0.35 and 8.33 μg/kg and 1.15 and 27.76 μg/kg respectively. The average recovery was between 73% and 118% with relative standard deviation (RSD=1.5-14%) for all the investigated pesticides. The multivariate method helps to reduce optimization time and improve analytical throughput.
Solid-phase microextraction (SPME) is a solvent-less sample preparation method which combines sample preparation, isolation, concentration and enrichment into one step. In this study, multivariate strategy was used to determine the significance of the factors affecting the solid phase microextraction of pesticide residues (fenobucarb, diazinon, chlorothalonil and chlorpyrifos) using a randomised factorial design. The interactions and effects of temperature, time and salt addition on the efficiency of the extraction of the pesticide residues were evaluated using 2(3) factorial designs. The analytes were extracted with 100 μm PDMS fibres according to the factorial design matrix and desorbed into a gas chromatography-mass spectrometry detector. The developed method was applied for the analysis of apple samples and the limits of detection were between 0.01 and 0.2 μg kg(-)(1), which were lower than the MRLs for apples. The relative standard deviations (RSD) were between 0.1% and 13.37% with average recovery of 80-105%. The linearity ranges from 0.5-50 μg kg(-)(1) with correlation coefficient greater than 0.99.
The formation of 3-monochloropropane-1,2-diol (3-MCPD) esters in refined palm oil during deodorisation is attributed to the intrinsic composition of crude palm oil. Utilising D-optimal design, the effects of the degumming and bleaching processes on the reduction in 3-MCPD ester formation in refined palm oil from poor-quality crude palm oil were studied relative to the palm oil minor components that are likely to be their precursors. Water degumming remarkably reduced 3-MCPD ester formation by up to 84%, from 9.79 mg/kg to 1.55 mg/kg. Bleaching with synthetic magnesium silicate caused a further 10% reduction, to 0.487 mg/kg. The reduction in 3-MCPD ester formation could be due to the removal of related precursors prior to the deodorisation step. The phosphorus content of bleached palm oil showed a significant correlation with 3-MCPD ester formation.
The synergistic antioxidant effects of ethanolic extracts of Centella asiatica (CE), and α-tocopherol have been studied. The types of interactions exhibited by CE and α-tocopherol combined at different ratios were measured using three assays: 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid) diammonium salt (ABTS) radical-scavenging capacity, the β-carotene bleaching system and liposome peroxidation assays. Fixed-fraction isobolographic analysis was used to detect any inducement of the antioxidant activity compared with the individual activities of CE and α-tocopherol. Of all synergistic combinations of CE and α-tocopherol, only fraction 2/3 showed the synergistic combination that fits well in three different assays and can be explained by the regeneration of α-tocopherol by CE despite the interaction effect of β-carotene present in the analytical assay. This phenomenon involved complex interactions between CE and α-tocopherol to exhibit different degrees of interactions that eventually increased antioxidant activity.
A solvent displacement method was used to prepare lutein nanodispersions. The effects of processing parameters (addition method, addition rate, stirring time and stirring speed) and emulsifiers with different stabilizing mechanisms (steric, electrostatic, electrosteric and combined electrostatic-steric) on the particle size and particle size distribution (PSD) of the nanodispersions were investigated. Among the processing parameters, only the addition method and stirring time had significant effects (p<0.05) on the particle size and PSD. For steric emulsifiers, Tween 20, 40, 60 and 80 were used to produce nanodispersions successfully with particle sizes below 100nm. Tween 80 (steric) was then chosen for further comparison against sodium dodecyl sulfate (SDS) (electrostatic), sodium caseinate (electrosteric) and SDS-Tween 80 (combined electrostatic-steric) emulsifiers. At the lowest emulsifier concentration of 0.1%, all the emulsifiers invariably produced stable nanodispersions with small particle sizes (72.88-142.85nm) and narrow PSDs (polydispersity index<0.40).
The stability of lutein nanodispersions was evaluated during storage and when exposed to different environmental conditions. Lutein nanodispersions were prepared using Tween 80, sodium dodecyl sulfate (SDS), sodium caseinate (SC) and SDS-Tween 80 as the emulsifiers. During eight weeks of storage, all samples showed remarkable physical stability. However, only the SC-stabilized nanodispersion showed excellent chemical stability. Under different environmental conditions, the nanodispersions exhibited a varied degree of stability. All nanodispersions showed constant particle sizes at temperatures between 30 and 60°C. However, at pH 2-8, only the SC-stabilized nanodispersion was physically unstable. The addition of NaCl (300-400mM) only caused flocculation in nanodispersion stabilized by SDS-Tween 80. All nanodispersions were physically stable when subjected to different centrifugation speeds. Only Tween 80-stabilized nanodispersion was stable against the effect of freeze-thaw cycles (no phase separation observed). In this study, there was no particular emulsifier that was effective against all of the environmental conditions tested.
The method of liquid chromatographic tandem mass spectrometry was utilized and modified to confirm and quantify acrylamide in heating cooking oil and animal fat. Heating asparagine with various cooking oils and animal fat at 180°C produced varying amounts of acrylamide. The acrylamide in the different cooking oils and animal fat using a constant amount of asparagine was measured. Cooking oils were also examined for peroxide, anisidine and iodine values (or oxidation values). A direct correlation was observed between oxidation values and acrylamide formation in different cooking oils. Significantly less acrylamide was produced in saturated animal fat than in unsaturated cooking oil, with 366ng/g in lard and 211ng/g in ghee versus 2447ng/g in soy oil, followed by palm olein with 1442ng/g.
Soy sauce fermentation was simulated in a laboratory and subjected to 10min of sonication. A full factorial design, including different cycles, probe size, and amplitude was used. The composition of 17 free-amino acids (FAAs) was determined by the AccQ-Tag method with fluorescent detection. Main effect plots showed total FAAs extraction was favoured under continuous sonication at 100% amplitude using a 14mm diameter transducer probe, reaching 1214.2±64.3mg/100ml of total FAAs. Moreover, after 7days of fermentation, sonication treatment caused significantly higher levels (p<0.05) of glutamic acids (343.0±22.09mg/100g), total FAAs (1720.0±70.6mg/100g), and essential FAAs (776.3±7.0mg/100g) 3days sooner than the control. Meanwhile, enzymatic and microbial behaviours remained undisturbed. Collectively, the sonication to moromi resulted in maturation 57% faster than the untreated control.
The effects of frying duration, frying temperature and concentration of sodium chloride on the formation of 3-monochloropropane-1,2-diol (3-MCPD) esters and glycidyl esters (GEs) of refined, bleached and deodorized (RBD) palm olein during deep-fat frying (at 160°C and 180°C) of potato chips (0%, 1%, 3% and 5% NaCl) for 100min/d for five consecutive days in eight systems were compared in this study. All oil samples collected after each frying cycle were analyzed for 3-MCPD esters, GEs, free fatty acid (FFA) contents, specific extinction at 232 and 268 nm (K232 and K268), p-anisidine value (pAV), and fatty acid composition. The 3-MCPD ester trend was decreasing when the frying duration increased, whereas the trend was increasing when frying temperature and concentration of NaCl increased. The GEs trend was increasing when the frying temperature, frying duration and concentration of NaCl increased. All of the oil qualities were within the safety limit.
Corresponding the high presence of 3-monochloropropane-1,2-diol esters (3-MCPDE) and glycidyl esters (GE) in refined palm oil, this paper re-evaluated degumming and bleaching processes of physical palm oil refining to reduce the amount of said contaminants. Separation-free water degumming was incorporated into the process, and this significantly (p
The reduction of the 3-monochloropropane-1,2-diol esters (3-MCPDE) and glycidyl esters (GE) was successfully achieved by the optimization of four processing parameters: phosphoric acid dosage, degumming temperature, bleaching earth dosage, and deodorization temperature by response surface methodology without the need for additional processing steps. The optimized processing conditions were 0.31% phosphoric acid dosage, 50 °C degumming temperature, 3% bleaching earth dosage, and 240 °C deodorization temperature. The optimization resulted in more than 80% and 65% reduction of 3-MCPDE and GE levels, respectively with color and FFA contents maintained in the acceptable range specified by Palm Oil Refiners Association of Malaysia. The optimized refining condition was transferred to macro scale refining units of 1 kg and 3 kg capacities to investigate its successful application during scale-up process.
The effect of different types of oils including camellia oil (CLO), sunflower oil (SFO), corn oil (CO) and linseed oil (LO) on the formation, crystal network structure and mechanical properties of 4%wt beeswax (BW) in oleogel was investigated. BW oleogels containing oils with higher contents of polyunsaturated fatty acids gelled first (1%wt), especially LO with higher contents of linolenic acid rather than CLO with higher contents of monounsaturated fatty acids. In comparison, oils with higher polyunsaturated fatty acid contents exhibited higher Db with more extensive microstructure at different cooling rates, which was related to shorter nucleation induction time of crystal and higher crystallinity. Stronger van der Waals forces were observed in oleogels with higher polyunsaturated fatty acid contents especially for LO oleogel. Rheology also showed that LO oleogel with higher content of linolenic acid had higher crystallinity and lower crystal melting interfacial tension, resulting in the formation of a more stable network structure.
Tocotrienol microcapsules (TM) were formed by firstly preparing Pickering emulsion containing tocotrienols, which was then gelled into microcapsules using alginate and chitosan. In this study, we examined the stability of TM during storage and when applied into a model food system, i.e. yogurt. During storage at 40°C, TM displayed remarkably lower tocotrienols loss (50.8%) as compared to non-encapsulated tocotrienols in bulk oil (87.5%). When the tocotrienols were incorporated into yogurt, the TM and bulk oil forms showed a loss of 23.5% and 81.0%, respectively. Generally, the tocotrienols were stable in the TM form and showed highest stability when these TM were added into yogurt. δ-Tocotrienol was the most stable isomer in both forms during storage and when incorporated into yogurt. The addition of TM into yogurt caused minimal changes in the yogurt's color and texture but slightly altered the yogurt's viscosity.
This work investigated the underlying formation of acrylamide from amino acids in frying oils during high temperatures and at different times via modeling systems. Eighteen amino acids were used in order to determine which one was more effective on acrylamide production. Significantly the highest amount of acrylamide was produced from asparagine (5987.5µg/kg) and the lowest from phenylalanine (9.25µg/kg). A constant amount of asparagine and glutamine in palm olein and soy bean oils was heated up in modelling system at different temperatures (160, 180 and 200°C) and times (1.5, 3, 4.5, 6, 7.5min). The highest amount of acrylamide was found at 200°C for 7.5min (9317 and 8511µg/kg) and lowest at 160°C for 1.5min (156 and 254µg/kg) in both frying oils and both amino acids. Direct correlations have been found between time (R2=0.884), temperature (R2=0.951) and amount of acrylamide formation, both at p<0.05.
A new optosensor for visual quantitation of nitrite (NO2(-)) ion has been fabricated by physically immobilizing Safranine O (SO) reagent onto a self-adhesive poly(n-butyl acrylate) [poly(nBA)] microspheres matrix, which was synthesized via facile microemulsion UV lithography technique. Evaluation and optimization of the optical NO2(-) ion sensor was performed with a fiber optic reflectance spectrophotometer. Scanning electron micrograph showed well-shaped and smooth spherical morphology of the poly(nBA) microspheres with a narrow particles size distribution from 0.6μm up to 1.8μm. The uniform size distribution of the acrylic microspheres promoted homogeneity of the immobilized SO reagent molecules on the microspheres' surfaces, thereby enhanced the sensing response reproducibility (<5% RSD) with a linear range obtained from 10 to 100ppm NO2(-) ion. The micro-sized acrylic immobilization matrix demonstrated no significant barrier for diffusion of reactant and product, and served as a good solid state ion transport medium for reflectometric nitrite determination in food samples.
The effects of a novel technology utilizing a simultaneous combination of Ultraviolet-C radiation and ultrasound energy postharvest treatment on tomato bioactive compounds during 28 days' storage period was investigated by varying Ultraviolet-C radiation intensities of 639.37 or 897.16 µW/cm2 at a constant ultrasound intensity of 13.87 W/L from a 40 kHz-1 kW transducer. A minimal treatment time of 240 s at Ultraviolet-C dosage of 2.15 kJ/m2 was observed to provoke a considerable increase in bioactive compounds content, proportionated to treatment time. Although treatment led to temperature increase in the system reaching 39.33 °C due to heat generation by ultrasonic cavitation, the extractability and biosynthesis of phytochemicals were enhanced resulting in 90%, 30%, 60%, 20%, and 36% increases in lycopene, total phenols, vitamin C, hydrophilic and lipophilic antioxidant activities respectively. Results present the potential use of the combined non-thermal technologies as post-harvest treatment to improve bioactive compounds and antioxidant activity during storage.
Bacteriocin is an important peptide which can be used as an anti-microbial agent in food. However, simpler and more cost-effective purification methods need to be developed compared to chromatography to enhance its commercial viability. Surfactant precipitation was employed for the first time to purify bacteriocin-like inhibitory substance (BLIS) from a fermentation broth of Pediococcus acidilactici Kp10, and the amount precipitated was investigated as a function of anionic surfactant (AOT) concentration, and pH. Protein recovery from the precipitate was accomplished using solvent extraction, and solvent type, NaCl concentration, and ionic strength of the final solution were optimised. Optimal conditions were; 1.05mM of AOT at pH 4 for precipitation, and acetone extraction (with 1mM NaCl), which resulted in an 86.3% yield, and 53.8 purification factor. This study highlighted the fact that surfactant precipitation can be used as a primary recovery method for BLIS from a complex fermentation broth.
The main objectives of this study were to (i) isolate newly autochthonous yeast strains from the Tikveš region of Macedonia and (ii) test their impact on the quality of red wines from Vranec and Cabernet Sauvignon grape varieties. The newly isolated yeast strains were obtained by spontaneous fermentation of grape must from Vranec and Cabernet Sauvignon varieties collected from ten different micro-regions in Macedonia. The grapevines from both varieties grown in "Barovo" micro-region were the richest sources of yeast strains. In addition, the molecular identification and typing of strains were also carried out. The monomeric anthocyanins, polyphenolic content and other oenochemical characteristics of the wines were also compared with the wines from commercial yeast strain "SiHa". The Vranec wine from yeast strain F-8 and Cabernet Sauvignon wine from yeast strain F-20 had significantly (p<0.05) higher concentrations of monomeric anthocyanins and total phenolic compounds than other wines.
Resistant starch has potential health benefits but the factors affecting its formation in bread and baked products are not well studied. Here, the formation of resistant starch in wholemeal bread products was evaluated in relation to the processing conditions including fermentation time, temperature and the inclusion of palm oil as a vitamin source. The effects of each the factor were assessed using a full factorial design. The impact on final starch content of traditional sourdough fermentation of wholemeal rye bread, as well as the bulk fermentation process of wheat and wheat/oat blends of wholemeal bread, was also assessed by enzyme assay. Palm oil content was found to have a significant effect on the formation of resistant starch in all of the breads while fermentation time and temperature had no significant impact. Sourdough fermentation of rye bread was found to have a greater impact on resistant starch formation than bulk fermentation of wheat and wheat blend breads, most likely due the increased organic acid content of the sourdough process.
Catechin is astringent in taste, sparingly soluble in water and sensitive to oxygen, light and pH. These properties restrict its application in food products. The present study investigated the stability of inclusion complex (IC) and catechin in various food matrices and investigated in vitro recovery profile of catechin and IC in liquid, semi-solid and solid food matrices. Besides, the sensory profile of IC added yogurt was also determined. Results showed that IC and catechin was more stable in solid matrix compared to semi-solid and liquid matrices. IC added in milk and yogurt show the highest percentage recovery of catechin compared to IC added in cheese and catechin added in all the matrices in in vitro digestive system. Through IC, β-CD masked the bitterness of catechin. These results suggest that protection of antioxidant such as catechin by β-CD inclusion complex may have applications in functional foods and health supplements.