Application of Box–Behnken Design in the Optimization of In Situ Surfactant-Based Solid Phase Extraction Method for Spectrophotometric Determination of Quinoline Yellow in Food and Water Samples

In this work, a simple, rapid and sensitive method using in situ surfactant-based solid phase extraction (ISS-SPE) combined with UV–vis spectrophotometry has been developed for the preconcentration and determination of trace amounts of quinoline yellow in food and water samples. The Box–Behnken design was employed to optimize the extraction efficiency. The variables of interest were pH, surfactant volume, extraction time and NaI volume. In the optimal conditions, the calibration graph was linear in the range of 10.0–750 μg L^?1 with a correlation coefficient of 0.9982. The limit of detection (LOD) was 2.1 μg L^?1, and the preconcentration factor was calculated to be 51.8.     

Ultrasound-Assisted Extraction Followed by Solid-Phase Extraction Followed by Dispersive Liquid–Liquid Microextraction for the Sensitive Determination of Diazinon and Chlorpyrifos in Rice

Selectivity of solid-phase extraction (SPE) was combined with the concentration power of dispersive liquid–liquid microextraction (DLLME) to obtain a sensitive, low solvent consumption method for high-performance liquid chromatography determination of diazinon and chlorpyrifos in rice. In this method, rice samples were extracted by ultrasound-assisted extraction followed by SPE. Then, the SPE eluent was used as a disperser solvent in the next dispersive liquid-liquid microextraction step for further purification and enrichment of diazinon and chlorpyrifos. Under the optimal conditions, the linear range was from 5.0 to 250 μg kg^?1 for diazinon and from 2.5 to 250 μg kg^?1 for chlorpyrifos. Limits of detection of diazinon and chlorpyrifos were 1.5 and 0.7 μg kg^?1, respectively. Limits of quantitation of diazinon and chlorpyrifos were 5.5 and 3.0 μg kg^?1, respectively. The precisions and recoveries also were investigated by spiking 10 μg kg^?1 concentration in rice. The recoveries obtained were over 90 % with relative standard deviation (RSD%) below 9.0 %. The new approach was utilized to successfully detect trace amounts of diazinon and chlorpyrifos in different Iranian rice samples.     

EU legislation for Food Safety of Cereals and Cereal Products

Since the discovery of aflatoxins in the early 1960s, regulations have been established in many countries to protect the consumer from the harmful effects of these mycotoxins. The recognition that aflatoxins and other mycotoxins can cause major illness in humans and animals has led to limits being set for aflatoxins and some other mycotoxins in different countries around the world, often however on an ad hoc basis. Currently maximum levels of aflatoxins B1(2ug/kg) and B1 B2 G1 G2 combined (4ug/kg) and och-ratoxin A (3～5ug/kg) exist for cereals (including buckwheat     

Optimization of Ultrasound-Assisted Extraction Procedure to Determine Total Isoflavones in Chinese Soybean Cheese by Box–Behnken Design

Isoflavones from Chinese soybean cheese were extracted with aqueous ethanol. Single-factor experiment design was employed to optimize the solid-to-liquid ratio (in grams per milliliter), ethanol concentration (in percent), extraction time (in hours), and extraction temperature (in degrees Celsius). The solid-to-liquid ratio was 1.5:10 (g/mL), and ethanol concentration (50 %–90 %), extraction time (2–3 h), extraction temperature (50–70 °C) were used for further optimization of extraction conditions. The optimal conditions for the ultrasound-assisted extraction of total isoflavones from Chinese soybean cheese were determined using response surface methodology (RSM) by Box–Behnken design. Three variables “ethanol concentration, extraction time and extraction temperature” were regarded as factors in the optimization study. The optimal conditions for total isoflavone extraction in Chinese soybean cheese were: ethanol concentration of 65.43 %, extraction temperature of 65.38 °C, and extraction time of 2.51 h. The verification experimental OD value was 0.534, which agreed with the predicted value, thus indicating suitability of the model employed and the suitability of RSM in optimizing the extraction conditions.     

Ultrasound-Assisted Chitosan–Surfactant Nanostructure Assemblies: Towards Maintaining Postharvest Quality of Tomatoes

A novel ultrasound-assisted chitosan–surfactant nanostructure assembly was developed to allow better delivery of chitosan particles into intact fruit tissues for extension of postharvest life. Three solutions of 1 % chitosan–surfactant nanostructure assembly with micelle sizes of 400, 600 and 800 nm were prepared and applied as an edible coating on tomatoes. The fruits were stored at 15?±?2 °C and 70–80 % relative humidity for 20 days. The indicators of tomato ripening, which included loss of firmness, decline of titratable acidity, decline of chlorophyll content and increase in soluble solid content, were delayed in the treated fruits in comparison to the control (p?<?0.05). A delay of approximately 5 days in ripening was observed by evaluating the colour evolution from green to red. The treatment significantly (p?<?0.05) enhanced the phenolic content while maintaining a lower level of respiration in comparison to the control, throughout most of the storage duration. However, weight loss was higher in the treated fruits in comparison to the control. No significant difference in the resultant effects was observed by using chitosan–surfactant nanostructure assemblies of different micelle sizes (p?>?0.05).     

Process–Structure–Function Relations of Pectin in Food

Pectin, a complex polysaccharide rich in galacturonic acid, has been identified as a critical structural component of plant cell walls. The functionality of this intricate macromolecule in fruit- and vegetable-based–derived products and ingredients is strongly determined by the nanostructure of its most abundant polymer, homogalacturonan. During food processing, pectic homogalacturonan is susceptible to various enzymatic as well as nonenzymatic conversion reactions modifying its structural and, hence, its functional properties. Consequently, a profound understanding of the various process–structure–function relations of pectin aids food scientists to tailor the functional properties of plant-based derived products and ingredients. This review describes the current knowledge on process–structure–function relations of pectin in foods with special focus on pectin's functionality with regard to textural attributes of solid plant-based foods and rheological properties of particulated fruit- and vegetable-derived products. In this context, both pectin research performed via traditional, ex situ physicochemical analyses of fractionated walls and isolated polymers and pectin investigation through in situ pectin localization are considered.     

Functionalized β-Cyclodextrin Polymer Solid Phase Extraction Coupled with UV–Visible Spectrophotometry for Analysis of Kaempferol in Food Samples

Functionalized β-cyclodextrin polymer, mono-6-deoxy-6-imidazole-β-cyclodextrin polymer (β-CDIMCP), was synthesized as a new solid phase adsorbent coupled with UV–visible spectroscopy to separate/analyze trace kaempferol. The results showed that kaempferol was adsorbed rapidly by β-CDIMCP (adsorption efficiency, 94.7 %) and then eluted by methanol (elution efficiency, 93.4 %). Under the optimum conditions, the calibration curve was linear in the concentration range from 0.10 to 14.0 μg/mL, with a correlation coefficient (R) of 0.9965. And the limit of detection was 0.028 μg/mL for kaempferol. The preconcentration factor of the method was tenfold. The molecular interaction between β-CDIMCP and kaempferol was studied through inclusion constant and FTIR analysis. The present method had been successfully applied to determine kaempferol in red wine samples.     

Comparison of Methodologies for the Extraction of Bacterial DNA from Mussels—Relevance for Food Safety

The control of the microbiological quality of bivalve molluscs assumes particular importance because they are among the most produced seafood products and mostly consumed as a whole, raw, or lightly cooked. The composition of the bacterial community associated with bivalves depends mostly on the microbiology of the surrounding environment at growing sites. Once the relationship between microbiology of bivalves and environment is established, a better classification and monitoring of the shellfish beds and evaluation of depuration strategies can be achieved. In this work, we tested if the methods of DNA extraction commonly used for the culture-independent microbiological analysis of sediment and water could be used directly, or with modifications, for the analysis of bacteria in mussels. The commercial kits Genomic DNA Purification Kit (MBI Fermentas, Vilnius, Lithuania), UltraClean^TM Soil DNA Isolation Kit (MOBIO Laboratories, Inc., Carlsbad, CA) and the method described by Griffiths and collaborators for DNA/RNA co-extraction were compared. The efficiency of extraction was assessed by DNA fluorescence and the denaturing gradient gel electrophoresis gel patterns of 16S ribosomal RNA gene fragments were used to compare the reproducibility and representativeness of the extraction methods. Results showed that the DNA/RNA co-extraction method with modifications was the most suitable. However, the results must be interpreted in the light of the purpose of the study and the relevance of maximizing extraction yield or diversity estimate, without compromising reproducibility. To our knowledge, this was the first attempt to transpose the procedure currently used for DNA extraction from sediments or waters, to the analysis of whole mussels.     

Shelf-life Assessment of Food Undergoing Oxidation–A Review

Oxidation is the most common event leading to the end of shelf life of microbiologically stable foods. Thus, a reliable shelf-life assessment is crucial to verify how long the product will last before it becomes oxidized to an unacceptable level to the consumers.

Shelf-life assessment strategies of foods and beverages suffering oxidation are critically discussed focusing on definition of the acceptability limit, as well as the choice of the proper oxidative indicators, and methodologies for shelf-life testing. Testing methodologies for shelf-life determination under actual and accelerated storage conditions are considered, highlighting possible uncertainties, pitfalls, and future research needs.     

Solid Phase Extraction Combined Direct Spectrophotometric Determination of Brilliant Blue in Food Using β-Cyclodextrin Polymer

A new and sensitive solid phase extraction (SPE) combined direct spectrophotometry for determination of brilliant blue (BB) in food has been developed, in which β-cyclodextrin polymer (β-CDP) is used as a SPE adsorbent to extract BB from aqueous solutions to form a solid supramolecular complex with a 1:3 molar ratio of BB to β-CDP, and BB in β-CDP was directly determined by a solid phase spectrophotometry. SPE conditions were pH 7.0, temperature 20 °C, ionic strength 0.1 mol/l, and shaking time 40 min. The calibration curve is linearity in the concentration range of 0.05–12.0 μg/ml. The proposed method was applied to the determination of BB in food samples at 627 nm maximum absorption wavelength with satisfactory results.     

Development of Multiresidue Analysis for 21 Synthetic Colorants in Meat by Microwave-Assisted Extraction–Solid-Phase Extraction–Reversed-Phase Ultrahigh Performance Liquid Chromatography

A novel ultrahigh performance liquid chromatographic method is developed for analysis of 21 synthetic colorants with different acid–base property, solubility, and polarity. The meat samples were extracted by microwave-assisted extraction followed by cleanup with solid-phase extraction. The effective separation of the colorants in meat matrixes was achieved, and no interfering peaks could be detected at the retention time of the analytes. The calibration curves showed good linearity with correlation coefficients of 0.9940–0.9999. The limits of quantification were 0.48–7.19 μg/kg. The average recovery of the 21 analytes from meat samples spiked with 25 and 75 μg?kg^?1 was 61.29–116.1 % with relative standard deviation (RSD) of <11 %. For blank beef sausage spiked with 50 μg?kg^?1 for each analyte, the intraday precision (as RSD) for 21 analytes was 1.45–9.21 % for six determinations within a day. This method has the advantages of being rapid, sensitive, accurate, and with high-throughput and can be applied for multiresidue analysis of meat samples, including six allowable azo food colorants, ten banned azo food colorants, four banned triphenylmethanes, and rhodamin B food colorant.     

Determination of <Emphasis Type="Italic">Bacillus cereus</Emphasis> Emetic Toxin in Food Products by Means of LC–MS²

Cereulide is the heat-stable toxin produced by certain strains of Bacillus cereus. It is the main virulence factor of emetic B. cereus strains, which causes the emetic food poisoning syndrome, including rare fatal cases of food intoxications. Due to presumably low intoxication doses, a sensitive, specific, and robust technique is needed for its detection. In 2002, a LC–MS method was developed which allowed absolute quantification of cereulide using valinomycin as standard. This study describes the validation, according to the Commission Decision 2002/657/EC, of the LC–MS2 method, a tandem mass spectrometry technique, which guarantees lower detection limit and higher specificity. The LC–MS2 method, calibrated with valinomycin, was validated in rice and tested on various matrices (i.e., red beans, spices, and chili con carne) containing cereulide. The process combines a simple extraction step from the food matrix followed by LC–MS2 analysis and detection by ion trap mass spectrometer. The detection limit for cereulide in rice was 0.5 ng eq/g, which is 20 to 2,500 times lower than currently understood intoxicative doses between 10 and 1.280 ng/g previously reported for cereulide. The validated method was specific, sensitive, repeatable, and reproducible with recoveries ranging from 77% to 101%.     

Determination of Free Amino Acids in Coated Foods by GC–MS: Optimization of the Extraction Procedure by Using Statistical Design

The development and validation of an extraction procedure for quantification of free amino acids in coated products by MTBSTFA derivatization and GC–MS detection is described. The extraction method entailed the sample homogenization with hydrochloric acid (HCl) by stirring at 40 °C followed by two centrifugation steps. The optimum combination of the extraction variables was achieved by response surface methodology. HCl concentration and volume and stirring time influenced free amino acid extraction yield. The selected optimal extraction conditions were 5 g of sample mixed to 7.5 ml of 0.1 N HCl and stirred during 90 min. Consistency between predicted and experimental values as well as in the quality parameters was observed. The calibration curves were linear within the range 5–100 μg ml^?1 with correlation coefficient values (R ² ) higher than 0.99. Detection and quantification limits of the analytical procedure ranged from 2.10^?5 to 18.10^?2 μg μl^?1 and from 8.10^?5 to 60.10^?2 μg μl^?1, respectively. Precision was 0.20–12.59 % for run-to-run and 3.38–17.60 % for day-to-day. The accuracy is between 82.99 and 115.77 %. Nineteen amino acids were analyzed in frozen-thawed and deep-fried coated products from different origin, with cysteine being the most relevant.     

Determination of Polycyclic Aromatic Hydrocarbons (PAHs) in Olive and Refined Pomace Olive Oils with Modified Low Temperature and Ultrasound-Assisted Liquid–Liquid Extraction Method Followed by the HPLC/FLD

The cleanup method of modified low temperature was compared with the standardized method of modified ultrasound-assisted liquid–liquid (UALL) extraction for the analysis of 15 polycyclic aromatic hydrocarbons (PAHs) in olive oil and refined pomace olive oil. The modified UALL extraction consisted in purification on C₁₈ reversed-phase, Florisil-bonded-phase and NH₂ cartridges, and modified low-temperature extraction was followed by alumina-N and NH₂ solid-phase extraction (SPE) cartridges. Both methods are followed by reversed-phase high-performance liquid chromatography with fluorescence detection. The chromatograms of the final extracts showed lower interferences in both of the methods. The solvent consumption and cost for the modified UALL method were higher than those of the modified low temperature, and also, it needed more equipment, but its analysis time was less. The limit of detection and limit of quantitation of the modified UALL method were 0.16–0.97 and 0.57–2.93 μg kg^?1, respectively, and for the modified low temperature, they were 0.09–1.97 and 0.29–5.99 μg kg^?1, respectively. The PAH recoveries for the modified UALL extraction method ranged from 75.0 to 111.0 % (RSD?=?3–8 %), and for the modified low temperature, they ranged from 81.5 to 113.8 % (RSD?=?3–10 %).     

Techniques for Extraction of Brewer’s Spent Grain Polyphenols: a Review

Million tons of brewer’s spent grain (BSG) are annually produced worldwide as brewing industry by-products. BSG represents a valuable source of phenolic compounds, which have attracted much attention due to their diverse health benefits. Relevant strategies have been developed for their efficient extraction, in order to commercially exploit these resources. This review focuses on the current extraction methods used to obtain phenolic compounds from BSG, ranging from more traditional to advanced techniques. The commonly used methods are the conventional solid–liquid extractions, employing organic solvents, alkaline, and enzymatic reactions. However, the inherent difficulties in screening and obtaining these compounds have led to the development of advanced extraction techniques. Pressurized fluid extraction, supercritical extractions, and microwave-assisted and ultrasound-assisted extractions are some of the novel extraction techniques that have been recently explored. These techniques have been mostly applied for phenolic recovery from barley and malt, as well as other types of cereals. In this review, it is shown that these novel techniques may provide an innovative approach to extract phenolics from BSG or related products, following an in-depth discussion on the major strengths and weaknesses identified in each technique.     

Optimization of Microwave-Assisted Extraction Procedure to Determine Metal in Fish Muscles Using Box–Behnken Design

This study describes the application of response surface methodology (RSM) to develop a method for zinc, lead, manganese, nickel, iron, and copper determination by flame atomic absorption spectrometry in Snow trout (Schizothorax zarudnyi) samples after extraction by a microwave system. The effects of various parameters such as irradiation power, temperature, extraction time, and concentration of nitric acid were investigated by a fractional factorial design (2⁴⁻¹) to determine the significant parameters and their interactions. The results showed that all of the parameters were significant (p < 0.05). The RSM, based on Box–Behnken design, was employed to obtain the optimum conditions of the significant parameters. The optimal conditions could be obtained at a power of 685.0 W, temperature of 116 °C, extraction time of 38.0 min, and 2.5 (mol L⁻¹) for nitric acid concentration. The method was applied for determination of zinc, lead, manganese, nickel, iron, and copper in Snow trout (Schizothorax zarudnyi) samples.     

Migration Phenomenon in Food Packaging. Food–Package Interactions, Mechanisms, Types of Migrants, Testing and Relative Legislation—A Review

The development of convenient and low-cost packages, together with the increased consumer demands for safer products, have resulted in the conduction of extensive research and the publication of numerous studies related to the phenomenon of migration. The large number of synthetic materials used for the manufacture of packages makes the evaluation of the food–package interactions quite complicated. Different parameters such as the nature of the food of interest, the type of food–package contact, the time and temperature of contact, the packaging materials used, the properties of the migrating substances, as well as the amount of potential migrants contained in the packaging materials, can drastically affect the migration rate and extent. Due to the extreme variety of foods used, several food simulants have been suggested and applied for testing the migration phenomenon under various laboratory conditions. The use of many of those simulants is defined by national and international legislation. This review article covers the main migration phenomena, which are related to the most commonly used packaging materials. It is clearly demonstrated that the complexity of the migration phenomena requires more research to establish internationally accepted risk management procedures and standardised testing methods.     

Chemical Composition and Potential Health Effects of Prunes: A Functional Food?

Prunes are dried plums, fruits of Prunus domestica L., cultivated and propagated since ancient times. Most dried prunes are produced from cultivar d'Agen, especially in California and France, where the cultivar originated. After harvest, prune-making plums are dehydrated in hot air at 85 to 90 degrees C for 18 h, then further processed into prune juice, puree, or other prune products. This extensive literature review summarizes the current knowledge of chemical composition of prunes and their biological effects on human health. Because of their sweet flavor and well-known mild laxative effect, prunes are considered to be an epitome of functional foods, but the understanding of their mode of action is still unclear. Dried prunes contain approximately 6.1 g of dietary fiber per 100 g, while prune juice is devoid of fiber due to filtration before bottling. The laxative action of both prune and prune juice could be explained by their high sorbitol content (14.7 and 6.1 g/100 g, respectively). Prunes are good source of energy in the form of simple sugars, but do not mediate a rapid rise in blood sugar concentration, possibly because of high fiber, fructose, and sorbitol content. Prunes contain large amounts of phenolic compounds (184 mg/100 g), mainly as neochlorogenic and chlorogenic acids, which may aid in the laxative action and delay glucose absorption. Phenolic compounds in prunes had been found to inhibit human LDL oxidation in vitro, and thus might serve as preventive agents against chronic diseases, such as heart disease and cancer. Additionally, high potassium content of prunes (745 mg/100 g) might be beneficial for cardiovascular health. Dried prunes are an important source of boron, which is postulated to play a role in prevention of osteoporosis. A serving of prunes (100 g) fulfills the daily requirement for boron (2 to 3 mg). More research is needed to assess the levels of carotenoids and other phytochemicals present in prunes to ensure correct labeling and accuracy of food composition tables in order to support dietary recommendations or health claims.     

Food proteins: A review on their emulsifying properties using a structure–function approach

Proteins are of great interest due to their amphiphilic nature, which allows them to reduce the interfacial tension at the oil–water interface. The incorporation of proteins at the oil–water interface has allowed scientists to utilise them to form emulsions (O/W or W/O), which may be used in food formulations, drug and nutrient delivery. The systematic study of the proteins at the interface and the factors that affect their stability (i.e., conformation, pH, solvent conditions, and thermal treatment) has allowed for a broader use of these emulsions tailored for various applications. In this review, the factors affecting the stability of emulsions using food proteins will be discussed. The use of polysaccharides to complex with proteins will also be explored in relation to enhancing emulsion stability.     

Quantitation of Selected Polyphenols in Plant-Based Food Supplements by Liquid Chromatography–Ion Trap Mass Spectrometry

A high-performance liquid chromatography method with electrospray ionization mass spectrometric detection (HPLC-ESI-MS/MS) for the determination of some of the most important polyphenols present in botanical supplements has been developed. The target analytes were five flavonoids (diosmin, hesperidin, quercetin, rutin and troxerutin) and the flavolignan silybin. The extraction of the analytes from the supplements was carried out by ultrasound-assisted extraction using 100 % dimethyl sulfoxide (or methanol) for 15 min. After centrifugation, 1 μL of the diluted supernatant was injected in the HPLC system and the quantitation was performed by ESI-MS using the negative ionization mode, with methylparaben as internal standard. The validation of the method was performed with recovery experiments, observing recoveries in the range of 85–112 %, and relative standard deviations lower than 10 % for the complete analytical procedure, including the extraction. The limits of detection were in the 2.5–120 μg L^?1 range.