Rice sample preparation method for ICP-MS and CV-AFS analysis: Elemental levels and estimated intakes.

Eight sample digestion procedures were compared to determine 41 elements in rice samples by ICP-MS and CV-AFS. Analytical methods were evaluated using certified rice flour reference material (NIST 1568b) and recovery experiments. The microwave-assisted digestion of 0.5 g rice sample and reagent mixture of 2 mL HNO3, 0.5 mL H2O2, and 0.5 mL deionized water yielded the best recovery for all elements ranging from 90 to 120% at three different levels, bias% within 10%, and precision (coefficient of variation percent, CV% intra- and inter-day) below 15%. The best analytical method was applied to the elemental determination in nine types of rice available on the Italian market. Daily or weekly rice consumption meets the nutritional and safety requirements of EFSA and WHO. The present study allows extensive and detailed knowledge of the content of essential and non-essential/toxic elements in different types of rice produced or packaged in Italy.

Colorimetric and fluorescent probes for cysteine detection: Applications in food safety and cellular imaging.

In this study, three BODIPY-based fluorescent probes were designed and synthesized. The ultraviolet-visible spectra, fluorescence spectra, smartphone color recognition application and bioimaging were utilized to evaluate the capacity of the probes. By comparing key parameters, BDP-SIN had optimal performances including fastest response (10 min), highest signal-to-noise ratio (815 times) and lowest limit of detection (LOD = 49 nM). The recovery rate ranged from 92.04 % to 103.25 %. Meanwhile, BDP-SIN was triumphantly employed for determination of Cys in different daily food samples. Moreover, the test strips and microporous filter membrane loaded with BDP-SIN were developed for the portable real-time visualization and quantitative detection of Cys in food samples, which the contents ranged from 0.27 µM to 0.49 µM. Besides, BDP-SIN could image Cys in the living cells and mice. The novelty of this work was that developed an effective tool for researching the roles of Cys in food industry and living organisms.

One-pot derivatization spectrofluorimetric method for detection of aspartame in sweetener commercial tablets and soft drinks: Greenness assessments of the methodology.

Aspartame is an artificial sweetener used in drinks and many foods. International Agency for Research on Cancer classified aspartame as possibly carcinogenic to humans (IARC Group 2B). In this study, a sensitive and selective spectrofluorimetric method was developed to detect aspartame. The method is based on switching on the fluorescence activity of aspartame upon its condensation with O-phthalaldehyde (Roth's reaction) in the presence of 2-mercaptoethanol. The reaction product was detected fluorometrically at λem of 438 nm after λex of 340 nm. All reaction conditions required to yield the optimal fluorescence intensity were observed and investigated. Furthermore, the approach was validated according to ICH guidelines. Upon plotting the concentrations of aspartame against their associated fluorescence intensity values, the relationship between the two variables was linear within the range of 0.5-3.0 µg/mL. Furthermore, the method was employed to analyze the quantity of aspartame in commercial packages and soft drinks with an acceptable level of recovery. In addition, the Green Solvents Selecting Tool, Complementary Green Analytical Procedure Index, and the Analytical Greenness Metric tool were used to evaluate the sustainability and the greenness of the developed methodology.

Cost-effective fully 3D-printed on-drop electrochemical sensor based on carbon black/polylactic acid: a comparative study with screen-printed sensors in food analysis.

3D-printing technology allows scientist to fabricate easily electrochemical sensors. Until now, these sensors were designed employing a large amount of material, which increases the cost and decreases manufacturing throughput. In this work, a low-cost 3D-printed on-drop electrochemical sensor (3D-PES) was fully manufactured by fused filament fabrication, minimizing the number of printing layers. Carbon black/polylactic acid filament was employed, and the design and several printing parameters were optimized to yield the maximum electroanalytical performance using the minimal amount of material. Print speed and extrusion width showed a critical influence on the electroanalytical performance of 3D-PES. Under optimized conditions, the fabrication procedure offered excellent reproducibility (RSD 1.3% in working electrode diameter), speed (< 3 min/unit), and costs (< 0.01 $ in material cost). The 3D-PES was successfully applied to the determination of phloridzin in apple juice. The analytical performance of 3D-PES was compared with an equivalent commercial on-drop screen-printed electrode, yielding similar precision and accuracy but lower sensitivity. However, 3D-PES provides interesting features such as recyclability, biodegradability, low-cost, and the possibility of being manufactured near the point of need, some of which meets several demands of Green Chemistry. This cost-effective printing approach is a green and promising alternative for manufacturing disposable and portable electroanalytical devices, opening new possibilities not only in on-site food analysis but also in point-of-care testing.

Oven-Roasting Effects the Fatty Acid Composition, Antioxidant Properties, and Oxidative Stability of Pomegranate (Punica granatum L.) Seed Oil.

In this study, we investigated the effect of roasting conditions and time on the physicochemical properties of pomegranate seed oil. We analyzed the fatty acid, total phenolic, flavonoid, tocopherol, and phytosterol contents of pomegranate seed oil extracted under four conditions: raw, heated at 160°C for 15 min, heated at 160°C for 20 min, and heated at 180°C for 10 min, which included three that were well-established to enhance nutritional and flavor properties. Furthermore, the oxidative stability was evaluated based on the acid value, peroxide value, and induction period. Roasting significantly decreased the contents of punicic acid, polyunsaturated fatty acids, tocopherol, and phytosterol and the 2,2-diphenyl-1-picrylhydrazyl radical scavenging capacity (P<0.05) of the oil. Conversely, saturated fatty acids, monounsaturated fatty acids, acid value, peroxide value, total phenolic and flavonoid contents, and induction period were significantly increased (P<0.05). Our results suggest that the roasting conditions were nutritionally and oxidatively stable, thereby enhancing the roasting process and providing a database for essential roasting treatments for pomegranate seed oil.

Semi-quantitative analysis of formaldehyde in food using calibration chart based on number of colored wells of microwell plate titration.

Microplate titration quantifies sodium hydroxide generated from formaldehyde reacting with excess sulfite in a 96-microwell plate. Phenolphthalein indicators change from red to colorless when all hydroxide ions react. Methodology optimized reagent concentrations, and reaction time and created a Calibration Chart for semi-quantitative determination. The chart shows formaldehyde concentration ranges corresponding to red well counts from 0 to 200 mM in 20 mM increments. Inter-operator repeatability demonstrates precision (3 replicates), correlating red wells with standard formaldehyde concentrations. This instrument-free technique uses readily available commercial plates, eliminating the need for specialized equipment and calibration. The methodology offers simplicity with its reliance on readily available commercial plates and minimal specialized equipment, hence it is cost-effective and easily transportable 96-microwell plates enhancing the methodology's portability, and efficient semi-quantitative analysis of formaldehyde. The analysis of twelve solutions from food samples agrees with the quantitative values using titration.

Dietary Intake of Minerals and Potential Human Exposure to Toxic Elements via Coffee Consumption.

In this study, we investigated the levels of macro, minor, and trace elements in roasted ground and instant coffees (n = 56). We assessed dietary mineral intake and health risks associated with potentially toxic elements (PTEs) using deterministic and probabilistic approaches. The limits of detection (LOD) ranged from 0.13 µg/kg for Be to 3.7 mg/kg for K, with corresponding limits of quantification (LOQ) at 0.43 µg/kg and 12.2 mg/kg. The recovery values (R%) ranged from 89 to 107%. The most abundant element was K, followed by Mg, Ca, and Na. Other elements followed this order: Fe > Mn > B > Cu > Sr > Zn > Al > Ba > Ni > Cr > Co > Se > Sn > Pb > Li > Ag > V > As > Cd > Hg > Be. Instant coffees generally exhibited higher K, Mg, and Na levels than ground-roasted coffees. Notably, Hg, Li, and Se were not detected in 34, 2, and 1 samples, respectively. Coffee samples were generally a good source of dietary elements such as Cu, Mn, Cr, and Se. The PTEs found in coffee products posed negligible risks to human health. The total target hazard quotient (TTHQ) remained below 1, and the incremental lifetime cancer risk (ILCR) did not exceed the threshold of 1 × 10-6. Nevertheless, coffee consumption contributed to Pb and As levels below 15% of the benchmark dose lower confidence limit (BMDL) values, and Sn, Hg, and Cd levels below 0.90% of the provisional tolerable weekly intake (PTWI).

Detection of cadmium heavy metal ions using a nanostructured green sensor in food, biological and environmental samples.

Heavy metals are one of the most important pollutants in the environment due to their toxic properties, accumulation, and indestructibility. So that when the metals enter the body of plants from natural and artificial sources, they accumulate in the organs and tissues. Therefore, in the present study, a sensitive and selective strategy is reported for the detection of cadmium(II) ions. To achieve this purpose, first sodium aluminate nanostructures were synthesized using a sol-gel method and green route. Then, using the nanostructures, a modified nanostructured sensor was designed. The characterization of the nanostructures was performed using various techniques. Next, the electrochemical behavior of the modified nanostructured electrode was investigated. The studies show the environment-friendly sensor has an enhanced voltammetric response than the unmodified sensor for cadmium(II) ions. After confirming the performance of the modified sensor, the analysis of cadmium(II) ions at the surface of the nanostructured modified electrode was investigated. Then, by differential pulse voltammetry (DPV) technique, the detection limit of cadmium(II) ions in optimal conditions was obtained at 1.10 nM with a broad dynamic linear range of 0.02-20.00 µM and 20.00-900.00 µM. Finally, the performance of the modified nanostructure sensor was investigated in food, biological and environmental samples, and acceptable results were obtained using the proposed method.

A practical and eco-friendly method for the determination of polycyclic aromatic hydrocarbons in açaí-based food products by vacuum-assisted sorbent extraction coupled to gas chromatography-mass spectrometry.

For the first time, a method for the simultaneous analysis of fifteen polycyclic aromatic hydrocarbons (PAHs), including light and heavy PAHs, in açaí-based food products (AFPs) was developed using vacuum-assisted sorbent extraction (VASE) combined with gas chromatography-mass spectrometry (GC-MS). The method requires no organic solvents and is amenable to full automation. To achieve optimal analytical extraction conditions, VASE parameters including stirring rate, extraction time, desorption temperature, desorption time, preheat time, and preheat temperature were optimized using sequential multivariate optimization. The method was validated and yielded limits of quantification below 1 µg kg-1 for all analytes, with recoveries ranging from 65 % to 112 % and good precision (≤11 % relative standard deviation). Additionally, the greenness and practical aspects of the method were investigated using the Green Analytical Procedure Index (GAPI), eco-scale, and the Blue Applicability Grade Index (BAGI), respectively. The VASE-GC-MS approach is suitable for routine analysis and exhibits characteristics of a green analytical method. No PAHs were detected above the limits of detection in thirty samples of AFPs.

A novel LD-targeting cysteine-activated fluorescent probe for diagnosis of APAP-induced liver injury and its application in food analysis.

Cysteine (Cys) not only plays an indispensable role in maintaining the redox balance in organisms, but is also an important nutrient in the food industry. Fluorescence-based detection systems have emerged as an effective method to track the locations and concentrations of different species. To achieve efficient monitoring of Cys in both food samples and biological systems, a novel lipid droplet (LD) targeted fluorescent probe (namely NIT-Cys) was constructed for the turn-on detection of Cys, characterized by a large Stokes shift (142 nm), a short response time (<8 min), and a low Cys detection limit (39 nM). Furthermore, the NIT-Cys probe has been successfully used not only to quantify the amounts of Cys in selected food samples, but also to enable the visualization of endogenous Cys in acetaminophen (APAP)-induced drug-induced liver injury cells, zebrafish larvae and mice models. Consequently, the work presented here provides an efficient tool for monitoring Cys.

Invasive Round Goby (Neogobius melanostomus) Fish from the Southern Baltic as a Source of Arsenic and Selenium-Food Safety Aspects.

Minimizing human exposure to arsenic (As) and ensuring an adequate dietary intake of selenium (Se) are significant issues in research on food sources. This study measured the content of As and Se in the muscles, gills, liver, and gonads of the fish round goby (Neogobius melanostomus) to assess the benefits and risks associated with their consumption. This was achieved by using dietary reference intake (DRI), estimated daily intake (EDI), target hazard quotient (THQ), and carcinogenic risk (CR). The elements were analyzed by atomic absorption spectrometry. The mean concentrations of As and Se (in µg kg-1 wet weight) were 25.1 and 161.4 in muscle, 58.8 and 367.4 in liver, 47.4 and 635.3 in gonads, and 16.4 and 228.5 in gills, respectively. Arsenic in the muscle portion of fish accounted for up to 0.5% of the DRI, while Se constituted approximately 30% of the DRI. The EDI values were below the reference oral dose (RfD). The THQ were much below the permissible levels (THQ < 1), and the CR were at least within the permissible limit (CR < 10-4). With regard to the As content, round goby muscles can be deemed safe for consumers. They may also be a valuable source of Se in the human diet. However, round goby consumption should be monitored for the proper and safe intake of these elements.

Nickel-manganese-cobalt tetragonal spinel ternary oxide nanocomposite as an effective adsorbent for dispersive solid phase micro-extraction of cadmium in food and water samples.

Nickel-manganese-cobalt tetragonal spinel ternary oxide nanocomposite (NMC-TSO) was synthesized. It was utilized as an efficient sorbent for the dispersive solid phase microextraction (D-SPµE) without vortexing of cadmium. The analysis of the cadmium was carried out by FAAS. The effective analytical parameters including pH (6) contact times (no vortexing), sample volume (70 mL), eluent volume (3 mL of 2 mol L-1 HCl), linear dynamic ranges (1.07-85.7 µg L-1), and re-useability (33) on the D-SPµE efficiency were investigated. The PF, RSD% and LOD of the D-SPµE for cadmium were 23.3, ≤ 2.8% and 0.49 µg L-1, respectively. The tolerable concentrations of Ca2+, Mg2+, K+ and Na+ on Cd(II) were 50,000 mg L-1, 50,000 mg L-1, 25,000 mg L-1 and 7500 mg L-1, respectively. The method was accurated by analysis of food and water certificate reference materials (NW-TMDA-54.6 Lake water, SPS-WW1 121 Batch wastewater, 1573a Tomato Leaves and TORT-3 Lobster Hepatopancreas) and - recovery experiments. The D-SPµE-FAAS method was applied for the cadmium determination in dam water, wastewater, river water, well water, sea water, tea, cacao, nut, bitter chocolate, rice, leek, cinnamon and parsley.

Screening method for the analysis of Rhodamine B in chili powder.

Rhodamine B is a synthetic dye known to enhance the visual appearance of chili powder. Due to its toxicity and carcinogenicity, chromatographic methods have been developed to monitor its presence in adulterated chili powder, but their assays are laborious, time consuming and expensive for screening purposes. The present studies propose an alternative for screening Rhodamine B in chili powder samples. The method combines thin layer chromatography (TLC) to solid surface room-temperature fluorescence spectroscopy. The scrape-dissolution procedure common to the instrumental analysis of TLC procedures was replaced with a fiber optic probe coupled to a commercial spectrofluorometer. The determination of Rhodamine B on the chromatographic plate is based on its retardation factor and maximum excitation and emission wavelengths. The limit of detection (1.9 ng.mL-1) and the limit of quantitation (5.2 ng.mL-1) are well below the usual contamination of Rhodamine B in adulterated foods.

Development of a vortex-assisted switchable-hydrophilicity solvent-based liquid phase microextraction for fast and reliable extraction of Zn (II), Fe (II), Pb (II), and Cd (II) from various baby food products.

This manuscript describes the development of a novel liquid phase microextraction (LPME) method for the extraction and determination of Zn (II), Fe (II), Pb (II), and Cd (II) in various infant/baby food and supplements products. The method is based on vortex-assisted extraction combined with a switchable-hydrophilicity solvent (SHS) sample preparation. The SHS, which undergoes reversible phase changes triggered by pH change, enables selective extraction and easy phase separation. A flame atomic absorption spectroscopy was used in the final determination step. Optimization studies revealed, that the optimal pH of the sample solution (after digestion) during analytes extraction is 5.5. A l-proline is added to the sample (375 mM) to ensure the complexation of the target metal cations. After the complexation step, 750 µL of SHS - a N, N-Dimethylcyclohexylamine along with 0.9 mL of 2 M of acetic acid solution is added (hydrophilicity switch-on stage) and mixed manually to obtain a homogeneous solution. In the last stage, 0.45 mL of 10 M NaOH solution (hydrophilicity switch-off stage) is added to the sample solution and a vortex for 100 s is applied to ensure the effective extraction and separation of the complex containing the analytes. At this stage, a cloudy solution is immediately obtained. Finally, the effective phase separation is obtained at the centrifugation step (4000 rpm for 2 mins). The method limit of detection was as 0.03, 0.009, 0.6, and 0.2 ng/L for Zn (II), Fe (II), Cd (II), and Pb (II) respectively with RSD% below 2.0 %. The analysis of certified reference materials and real samples proved the full applicability of the method for routine analysis, contributing to the field of heavy metal analysis and ensuring the safety of baby products. According to the AGREE methodology, this method can be named as green analytical chemistry method with a score of 0.77.

Nano-palladium-decorated bismuth sulfide microspheres on a disposable electrode integrated with smartphone-based electrochemical detection of nitrite in food samples.

Nitrite (NO2-) is widely used as an additive to extend the shelf life of food products. Excessive nitrite intake not only causes blood-related diseases but also has the potential risk of causing cancers. A disposable screen-printed electrode was modified with nano­palladium decorated bismuth sulfide microspheres (nanoPd@Bi2S3MS/SPE), and integrated with a smartphone-interfaced potentiostat to develop a portable, electrochemical nitrite sensor. NanoPd@Bi2S3MS was prepared by the hydrothermal reduction of a Bi2S3MS and Pd2+ dispersion and drop cast on the SPE. The nanoPd@Bi2S3MS/SPE was coupled with a smartphone-controlled portable potentiostat and applied to determine nitrite in food samples. The linear range of the sensor was 0.01-500 µM and the limit of detection was 0.0033 µM. The proposed system showed good repeatability, reproducibility, catalytic stability, and immunity to interferences. The proposed electrode material and a smartphone-based small potentiostat created a simple, portable, fast electrochemical sensing system that accurately measured nitrite in food samples.

A new method based on extraction induced by emulsion breaking for determination of Co and Ni in chocolate bars by graphite furnace atomic absorption spectrometry.

This paper describes a new experimental configuration of extraction induced by emulsion breaking method to extract and determine Ni and Co in chocolate bars by graphite furnace atomic absorption spectrometry. At optimized conditions, the sample (0.08 g) was mixed with 4 mL of extractant solution (4% m/v Triton X-100 and 10% v/v HNO3) in a plastic syringe to form a solid-oil-water emulsion. Then, emulsion breaking was assisted by membrane filtration. The total extraction procedure took approximately 1 min, in opposition to 25 (centrifugation) and 50 min (heating). Extraction yields ranged from 94.8 to 114.3% for Co and from 85.9 to 108.4% for Ni. The limits of detection and quantification were, respectively, 24.73 and 82.45 µg Kg-1 for Co and 49.05 and 163.5 µg Kg-1 for Ni. Recoveries ranged from 92.1 (Ni) to 105.4% (Co).

Assessment of Impact of Dietary Patterns on Obstructive Sleep Apnea Patients.

Objective Obstructive sleep apnea syndrome (OSAS) is characterized by episodic cessations of breathing due to upper airway obstruction during sleep, which may cause disturbances in dietary patterns resulting from appetite-related hormonal changes. The aim of the present study was to investigate the relationship between OSAS and nutritional and dietary patterns. Materials and Methods A total of 20 female and 53 male OSAS patients aged > 30 years were enrolled. Demographic data, as well as data on smoking and alcohol habits, were noted, anthropometric measures were made, and a questionnaire regarding chronic diseases including OSAS and four questionnaires on recent food intake frequency and content of nutrition were filled out. The content of nutrition was noted under seven categories: meat, legumes, milk and dairy products, fruits and vegetables, bread and cereals, fat and carbohydrates, and beverages. Results The severity of OSAS (assessed by the apnea-hypopnea index. AHI) was positively correlated with the body mass index (BMI), the circumferences of the waist, chest, and buttocks, and, in males, with the circumference of the neck as well. There was no correlation between the AHI and nutritional habits in terms of the frequency of meals or snacks, the scores on the Snoring, Tiredness, Observed Apnea, and High Blood Pressure-Body Mass Index, Age, Neck Circumference, and Gender (STOP-BANG) Questionnaire and the corresponding macro- and micronutrients. Worsening apnea scores led to increased intake of macronutrients of carbohydrate and protein and micronutrients of niacin and pyridoxine ( p < 0.05), and decreased intake of fat ( p < 0.05). Conclusion The present study demonstrated an association between OSAS severity and recent food intake, manifested in increased intake of carbohydrates, niacin, and pyridoxine, and decreased fat intake.

Multivariate optimization for extraction of 2-methylimidazole and 4-methylimidazole from açaí-based food products using polymeric ionic liquid-based sorbent coatings in solid-phase microextraction coupled to gas chromatography-mass spectrometry.

In this study, polymeric ionic liquids featuring different functional moieties were applied as sorbent coatings in direct-immersion solid-phase microextraction (DI-SPME) for the extraction of 2-methylimidazole (2-MI) and 4-methylimidazole (4-MI) from açaí-based food products followed by gas chromatography-mass spectrometry (GC-MS) analysis. The analytical method was optimized using a sequential experimental design. Variables used in GC-MS such as desorption time, as well as for SPME-DI, including extraction time, extraction temperature, incubation time of extraction, amount of NaCl in the extract, and stirring rate, were optimized. The fitness-for-purpose of the method was verified by the linearity of matrix-matched calibration curves (R2 ≥ 0.9921), adequate recoveries (81.7-89.7 %), and precision (relative standard deviations ≤11.2 %). The method was applied to twenty-five samples of açaí-based food products. 4-MI was found in four samples whereas 2-MI was not detected above the limit of detection. The method was found to be suitable for quality control analysis.

Analysing polypeptide antibiotics residues in animal muscle tissues: The crucial role of HRMS.

A confirmatory method for the determination of polypeptide antibiotics (bacitracin, colistin, and polymyxin B) in muscle samples has been developed. Extraction is performed with acidified methanol, and a clean-up step by solid-phase extraction with polymeric cartridges is applied. Separation by ultra-high performance liquid chromatography (UHPLC) is carried out using a solid core C18 column and gradient elution with water/acetonitrile containing 0.2% formic acid. High-resolution mass spectrometry (HRMS) (Q-Orbitrap) detection using different working modes has proved to be highly advantageous in eliminating interfering signals from endogenous matrix components. The analytical method has been successfully validated according to Commission Regulation 2021/808/EU and is currently used in a public health laboratory involved in veterinary medicines residue surveillance activities.

Capillary electromigration methods for food analysis and Foodomics: Advances and applications in the period March 2021 to March 2023.

This work presents a revision of the main applications of capillary electromigration (CE) methods in food analysis and Foodomics. Papers that were published during the period March 2021 to March 2023 are included. The work shows the multiple CE methods that have been developed and applied to analyze different types of molecules in foods and beverages. Namely, CE methods have been applied to analyze amino acids, biogenic amines, heterocyclic amines, peptides, proteins, phenols, polyphenols, pigments, lipids, carbohydrates, vitamins, DNAs, contaminants, toxins, pesticides, additives, residues, small organic and inorganic compounds, and other minor compounds. In addition, new CE procedures to perform chiral separation and for evaluating the effects of food processing as well as the last developments of microchip CE and new applications in Foodomics will be also discussed. The new procedures of CE to investigate food quality and safety, nutritional value, storage, and bioactivity are also included in the present review work.