Food Analytical Methods最新文献

Fish is a food with high nutritional value, but its quickly perishable nature requires a hygiene process to maintain product quality and increase shelf life. The aim of this study was to evaluate different concentrations of chlorine in the water used to sanitize Nile tilapia fillets on the formation of trihalomethanes (THM) in fresh and frozen products at different storage times. A completely randomized experimental design was used, in a 2 × 3 split-plot arrangement, with 15 replications; the plots consisted of fresh and frozen fish fillets, and the subplots consisted of the three chlorine concentrations in the water for sanitizing the fillets (100, 175, and 250 mg L⁻¹). Fresh fish analysis showed the following variations in THM levels: 1.4 to 6.8 μg kg⁻¹ (chloroform), 0.5 to 3.2 μg kg⁻¹ (bromodichloromethane), and 0.4 to 1.2 μg kg⁻¹ (dibromochloromethane). Bromoform ranged from 3.7 μg kg⁻¹ to undetected levels in the different tested storage times. Frozen fish analyses showed concentrations ranging from 2.1 to 5.2 μg kg⁻¹ (chloroform) and 0.6 to 2.0 μg kg⁻¹ (bromodichloromethane), while dibromochloromethane and bromoform levels were below the technique’s quantification limits in all storage times. THM formation depends on the binomial chlorine concentration in the washing water and time storage; fresh fish presented higher THM levels than frozen fish.

Selenium is an essential element and the main source of it is food. The ingestion of food rich in this element as nuts (Brazil nuts) is important to keep the body healthy. In this work, the development of a green and low-cost methodology for selenium analysis in beans was carried out using the photochemical vapor generation method coupled to atomic absorption spectrometry. The efficiency of the photochemical vapor generation (PVG) was optimized by evaluating the experimental conditions, such as type and concentration of the organic acid, flow rate of the carrier gas, and sample UV irradiation time. The formation of volatile species was more efficient using 6% v v⁻¹ acetic acid, carrier gas flow rate of 10 mL min⁻¹, and 20-s UV irradiation time. The method of standard addition calibration curves was performed to analyze total Se in green bean samples acquired in the market of different cities of northeast and north regions of Brazil. The accuracy of the proposed method was tested comparing results for Se content with hydride generation (HG) in a sample of Ceara state. The analyzed samples showed total Se content varying from 0.9 to 2.2 mg kg⁻¹ in dry matter of green beans. The amount of Se found in green beans is within the expected range when compared to other types of beans reported in the literature.

To protect consumers from non-halal and shubha-halal foods, it is essential to authenticate chicken meat based on its slaughtering process. The objective of the present study is to authenticate the halalness of chicken meat based on the slaughter process. Untargeted metabolomics, utilizing UHPLC-HRMS combined with chemometrics, offers a selective and accurate method for verifying the halal status of chicken meat based on the slaughter process. The results of this research identified 28 metabolite profiles, with creatine, carnosine, and 3-methylhistidine being the most prominent metabolites. Principal component analysis (PCA) clearly distinguished the metabolite profiles of chicken meat slaughtered using different methods. Additionally, cluster analysis effectively grouped chicken meat based on similarities in metabolite profiles. The correlation network revealed that 21 types of metabolites are interrelated in the halal authentication process. Partial least squares discriminant analysis (PLS-DA) accurately identified 13 potential biomarkers for halal authentication, including creatine, betaine, 2-amino-1,3,4-octadecanetriol, L-isoleucine, L-phenylalanine, L-histidine, L-glutamic acid, L-glutathione, DL-glutamine, taurine, carnosine, and acetyl-L-carnitine. Overall, untargeted metabolomics combined with UHPLC-HRMS and chemometrics represents a promising method for authenticating the halal status of chicken meat, distinguishing between halal, non-halal, shubha-halal, and mixtures of halal with non-halal or shubha-halal meat.

Atrazine (ATZ) and simazine (SMZ) are major herbicides in Brazilian cultivation areas, and through environmental persistence and bioaccumulation, these compounds can contaminate bovine milk and other products for human consumption. Thus, the present study aimed to develop an analytical method for the determination of ATZ and SMZ in bovine milk using ultrasound-assisted solvent-terminated dispersive liquid‒liquid microextraction (UA-ST-DLLME) and gas chromatography coupled with mass spectrometry (GC–MS). Protein precipitation was carried out by the addition of 0.8 g of NaCl and 5.0 mL of acetonitrile to 8.0-mL samples. The optimized UA-ST-DLLME method consisted of the addition of 1.8 mL of precipitation supernatant to 8.0 mL of 10.0% (m/V) NaCl solution, followed by sonication for 5 min, after which 1.75 mL of acetonitrile was added for the demulsifying step, which was completed after 5 min. Adequate linearity was observed for SMZ (5–350 µg/L) and ATZ (10–350 µg/L). Interday precision and accuracy (n = 3) were ascertained for the lower concentration levels, 100 and 350 µg/L. The relative standard deviation (RSD) values were less than 20% for the lowest concentration levels and less than 15% for the remaining concentrations; however, for all the concentration levels evaluated in these assays, the accuracy values ranged from 95.2 to 109.9% for SMZ and from 100.8 to 113.2% for ATZ.

Graphical Abstract

A single particle inductively coupled plasma mass spectrometry (SP-ICP-MS) method was developed for the determination and characterization of selenium nanoparticles (SeNPs) in dietary supplements in syrup formulations containing selenium dioxide and ascorbic acid. Experimental parameters affecting the signal intensities of the SeNPs, such as torch distance, sample flow rate, and addition of organic solvent, were optimized. It was observed that adding 3.0% (v/v) of propan-2-ol to the solutions increased the selenium nanoparticle signal by 3.4 times. SeNPs were detected in all of the five dietary supplements studied, and it was found that 19.3–60.4% of the total selenium was in the form of nanoparticles and that their mean diameters were in the range of 50–130 nm. Under the optimized conditions, the limit of detection for nanoparticle number concentration (LOD_conc) and the limit of detection for nanoparticle size (LOD_size) of the proposed SP-ICP-MS method were 770 particle mL⁻¹ and 36 nm, respectively. The recovery of total selenium determination was in the range of 102.1–106.4%. The recovery in terms of the particle number concentration in samples spiked with 140 nm and 50 nm SeNPs was between 88.8 and 114.0%. The developed SP-ICP-MS method is sensitive, rapid, and suitable for routine applications with minimum sample preparation for the characterization and determination of SeNPs in dietary supplements.

Two coupling methods, dicyclohexylcarbodiimide (DCC) and carbonyldiimidazole (CDI), are designed to prepare the complete antigen of deoxynivalenol (DON). The synthesized complete antigen is identified using high-performance liquid chromatography (HPLC), ultraviolet spectrophotometry (UV), and sodium dodecyl sulfate–polyacrylamide gel electrophoresis (SDS-PAGE). The complete antigen (DON-BSA) and antibody (DON-Ab) are then covalently coupled to carboxylated polystyrene (PS) microspheres to prepare PS-DON-BSA and PS-Ab. A new method for detecting DON is developed by constructing a microchannel resistance immunosensor (MCRS) based on the competitive bio-recognition reaction between these components and DON. The change of current value caused by the change of resistance in the detection platform can realize DON concentration. The results showed that the UV spectra of the complete antigens prepared by the two methods are significantly different from those of the hapten and carrier protein, with measured coupling ratios of approximately 9.8:1 and 7.8:1, respectively. SDS-PAGE also indicates good coupling effects. When the complete antigen is applied to the self-developed DON detection platform, this method shows a good linear relationship in the range of 100 pg/mL to 1000 ng/mL, with a correlation coefficient of 0.991, a detection limit of 499 pg/mL, a recovery rate of 89.26 to 108.50%, and a relative standard deviation of 4.15 to 6.57%, which meets the requirements for DON analysis and samples detection.

A new solid-phase microextraction (SPME) Arrow device was fabricated using mesoporous silica (MCM-41) as the coating material and integrated with a portable mass spectrometer (PMS) to develop a sensitive and selective method for the detection of amantadine, thiabendazole, sulfadimethoxine, clenbuterol, and ractopamine in milk and chicken samples. The influence of different functional groups on the extraction performance of MCM-41 was investigated by synthesizing amine-, vinyl-, and carboxyl-modified MCM-41, representing basic, neutral, and acidic surface properties. Among these, the carboxyl-modified MCM-41 (MCM-41-C) exhibited the highest selectivity and adsorption capacity, attributed to its strong electrostatic interactions and hydrogen bonding with the analytes. The MCM-41-C-SPME Arrow was fabricated using electrospinning to produce a uniform, stable coating, which was then systematically optimized for key extraction and desorption parameters. This novel SPME Arrow-PMS platform enables rapid detection of five analytes within 30 s, with a broad linear range (5–1000 μg kg^–1) and low limits of detection (1.6–30.6 μg kg^–1). The developed method demonstrated excellent intra-day and inter-day reproducibility (RSD < 12%) and high recovery (82–117%). This method offers rapid, sensitive detection of multiple veterinary drugs in complex food matrices, providing a practical solution for on-site food safety monitoring.

Carica papaya (Family Caricaceae) is endowed with a myriad of biological activities as gastroprotective, antidiabetic, antimalarial, antiviral, and anti-inflammatory agent. We performed for the first time an extensive comparative metabolite profiling of different plant organs considering both male and female leaves, seeds, and fruits of different maturity stages. The phytochemical fingerprinting-via UPLC/MS/MS- of C. papaya led to tentative identification of 84 metabolites belonging to different primary and secondary phytoconstituents to include alkaloids (carpaine derivatives), flavonoids, glucosinolates, organic and phenolic acids, amino acids, and carbohydrates. The seeds’ profile was enriched with hydroxybenzoic acids and their derivatives, while leaves were characterized by the prevalence of carpaine alkaloids, flavonoids, lipids, and alkylated sugars. Correlation analysis revealed a significant positive correlation between total phenolic content and the antioxidant assays (ferric reducing antioxidant property (FRAP), 2, 2-diphenyl-1- picrylhydrazyl (DPPH), 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid (ABTS), cupric-reducing antioxidant capacity (CUPRAC), and total antioxidant capacity (TAC)). Principal component analysis was applied to find out possible phytochemical trends across C. papaya matrices, where PC1 and PC2 accounted for 46.57 and 19.93% of the variability in the data set with well-separated extracts into groups mostly on the basis of plant organ. The PCA model showed that immature seeds had the highest antioxidant properties, while leaves separated from fruit and mature seeds due to higher butyrylcholinesterase and α-amylase inhibition, but lower acetylcholinesterase and α-glucosidase inhibition activity. We corroborate the better exploitation of both edible and inedible parts of C. Papaya in nutraceutical supplements after sufficient in vivo and toxicity studies.

To establish a highly sensitive chemiluminescent enzyme-linked immunosorbent assay (ci-ELISA) method for the determination of florfenicol (FF) in egg and chicken meat. Based on the obtained monoclonal antibodies against florfenicol, a chessboard test was employed to determine the optimal working concentration of artificial antigen and antibody, and then established a ci-ELISA method, and characterized its performance. The results showed that the ci-ELISA method had a detection limit of 5.433 pg/mL, an IC₅₀ of 30.893 pg/mL, and a detection range between 5.433 and 193.577 pg/mL. The coefficient of variation was below 10%, indicating satisfactory precision. The spiked recoveries in egg samples were between 90.03% and 95.24%, and the spiked recoveries in chicken meat samples were between 90.56% and 93.04%. In conclusion, the developed ci-ELISA method is highly sensitive and suitable for monitoring and detection of trace amounts of FF residues in eggs and chicken meat.

A novel, eco-friendly, and efficient dispersive liquid–liquid microextraction method was developed, utilizing pH-switchable hydrophobic deep eutectic solvents. This method, which combines with liquid chromatography and fluorescence detection, allows for the extraction and analysis of aflatoxin M1 in milk-based sports supplements. At first, twelve deep eutectic solvents were prepared and their pH switchability was investigated. pH-Switchable solvents were used for extraction and preconcentration of aflatoxin M1. The strength of the proposed method is that the dispersion of extraction solvent in the aqueous phase and the separation of phases occurred only by pH change and do not require the addition of dispersing solvent, ultrasonic, vortex, and centrifugation. In this study, the key factors that affect the extraction process, including the type and volume of DES (deep eutectic solvent), KOH concentration, volume of hydrochloric acid, the effect of adding salt, and the duration of extraction, were investigated, and the optimal conditions for each of these parameters were determined to maximize the extraction efficiency. Under optimum conditions, the relative standard deviations (RSDs) including intra- and inter-day precision of the method were determined by analyzing 5 μg kg⁻¹ of aflatoxin M1 in target samples seven times. The RSDs were 2.6% for intra-day and 4.5% for inter-day precision. The calibration curves showed linearity in the range of 0.015 to 50 μg kg⁻¹. The limit of detection (LOD) for this method was 0.005 μg kg⁻¹. When real milk-based sports supplements were spiked with varying concentrations of aflatoxin M1, the relative recoveries ranged from 92.0 to 105.0%.