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Starches-rich and protein-rich cereal samples commonly need tedious sample preparation steps before instrumental analysis. This study developed a miniaturized centrifugal integrated cold-induced phase separation (CIPS) method for convenient sample preparation. A small-sized centrifuge tube (2 mL) and a low-temperature centrifuge, both of which are easily accessible, make up the basic components of the system. Unlike conventional sample preparation methods that need a step-by-step extraction, enrichment, purification, and centrifugation, this centrifugal integrated CIPS method can be performed by a one-step combination protocol under a low-temperature centrifuge. As a proof-of-concept study, satisfactory recoveries and enrichment factors were demonstrated for the extraction of fumonisins and ochratoxins from cereals. A sensitive and selective quantification method was yielded by combining LC-HRMS using tSIM acquisition mode, with good linearity (R2 > 0.998), accuracy (82.9–106.5%), and precision (<13.4%). This strategy is convenient, low-cost, repeatable, and easy to semi-automate, further expanding the extraction potential for other acidic mycotoxins. [Display omitted] • A centrifugal integrated cold-induced phase separation method (CIPS) was proposed. • A CIPS was successfully applied for extraction of acidic mycotoxins in cereals. • The studied method demonstrates a convenience with a one-step combination protocol. • The greenness profile and practicality of the developed method was evaluated. [ABSTRACT FROM AUTHOR]

Waste rubber bark abundant in phenolics can be used to produce an adsorbent for the enrichment and determination of tetracycline. Fe 3 O 4 magnetic nanoparticles (Fe 3 O 4 MNPs) coated with naturally extracted phenolics from waste rubber bark were synthesized for the first time by ultrasound combined with a continuous flow approach. The production of Fe 3 O 4 MNPs with effective contact surface areas (45.3 m 2  g -1 ) was employed as a novel attractive sorbent in magnetic solid phase extraction (MSPE) to selectively preconcentrate oxytetracycline, tetracycline, chlortetracycline, and doxycycline before HPLC-UV analysis. This MSPE-HPLC exhibited wide linear ranges (14.0-260.0 μg kg -1 ), with low limits of detection (10.0 μg kg -1 ) and quantitation (14.0-20.0 μg kg -1 ), and was successfully applied to quantify tetracycline residues in honey samples, with recoveries ranging from 81.3 % to 117.9 %. This method offers a potential alternative for determining tetracycline in food with a high enrichment factor, high precision, and more effective accuracy, selectivity, and sensitivity., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

This study presents the development of ion chromatography coupled with inductively coupled plasma optical emission spectrometry (IC-ICP-OES) for the simultaneous determination and quantification of inositol phosphates (InsP x ). Using a CarboPac PA100 column with a nitric acid-water gradient, 28 InsP x isomers (InsP 6 to InsP 2 ) were separated within 33 min. The method eliminates baseline drift and post-column derivatization thereby simplifying detection and quantification. It achieves low detection limits of 63 μg/L P across a range of 63-3200 μg/L P. Various extraction and sample preparation methods for food and feed matrices were tested, including acidic and alkaline agents, C 18 SPE and spin concentrators. The analysis shows intra-day and intra-laboratory reproducibility with deviations smaller than 1 % for standard solutions and under 4 % for feed samples (80 % recovery rate of phytate). This methodology is applicable to explore enzymatic degradation pathways and the analysis of InsP x in complex food and animal feed matrices., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 The Authors. Published by Elsevier Ltd.. All rights reserved.)

The use of pesticides has led to environmental pollution and posed a global health risk, since they remain as residues on foods. Beans one of the most widely cultivated crop in Africa, and susceptible to attack by insects both on field and during storage, leading to the application of pesticides to control pests' infestation. However, misuse of these chemicals by farmers on beans has resulted in the rejection of beans exported to European countries, due to the presence of pesticide residues at concentrations higher than the maximum residues levels (MRLs). In this study, the effectiveness of the Association Official Analytical Chemists (AOAC) Official Method and the European Committee of Standardization (CEN) Standard Method, were determined using multivariate approach for the analysis of organochlorine pesticide residues in 6 varieties of beans samples. The significance of factors (mass of sample, volume of acetonitrile, mass of magnesium sulphate, sample pH, centrifugation time and speed) affecting the efficiency of extraction was estimated using Plackett-Burman design, while central composite design was used to optimize the significant factors. The following optimum factors were subsequently used for method validation, recovery tests, and real sample analysis: 4 g of sample sludge (1:1 v/v), 10 mL of acetonitrile, 4.45 g of MgSO 4 , and 5 min of centrifugation at 5000 rpm. The figure of merit of analytical methodology estimated using matrix-matched internal standard calibration method gave linearity ranging from 0.25 to 500 μg/kg, with correlation coefficient (R 2 ) greater than 0.99, the recovery ranged from 75.55 to 110.41 (RSD = 0.70-16.65), with LOD and LOQ of 0.23-1.77 μg/kg and 0.76-5.88 μg/kg, respectively., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

A simple and effective ultrasound-assisted dispersive micro solid-phase extraction (UA-dμSPE) method was developed for the spectrophotometric determination of traces maneb in food and water. In this study, a new hybrid block copolymer poly (vinyl benzyl chloride-b-dimethyl aminoethyl methacrylate) (Pvb-DMA) was synthesized and characterized using techniques such as FTIR, SEM-EDX. The synthesized Pvb-DMA was used as an adsorbent for the extraction of maneb for first time in this study. The effects of different experimental variables such as pH, adsorbent amount, sample volume, eluent type were optimized. The statistical toll factorial design was applied to estimate the individual and combined impact of parameters on the extraction of maneb. The applicability of different solvents such as acetone, methanol, ethanol, tetrahydrofuran, acetonitrile for maneb recovery from adsorbent was tested. The detection and quantification limits were found to be 3.3 ng mL−1 and 10.0 ng mL−1, respectively. In addition, the preconcentration factor and linear range was obtained 300 and 10–500 ng mL−1. The extraction recovery and relative standard deviation were found to be 95 % and 2.8 %, respectively. [Display omitted] • A low-cost, simple, green and selective ultrasound-assisted dispersive micro solid phase extraction (dμSPE) was developed. • A block copolymer (Pvb-DMA) was synthesized and used as adsorbent for the first time. • Extraction factors were optimized using central composite design, saving time and chemical consumption. • The developed dμSPE technique provided low LOD, LOQ, RSD and high PF. • Present method was applied to maneb determination in water and food samples. [ABSTRACT FROM AUTHOR]

Per- and polyfluoroalkyl substances (PFASs) are extensively found in foods, posing potential toxicity to humans. Therefore, rapid analysis and monitoring of PFASs in foods are crucial for public health and also a challenge. To detect trace PFASs in foods, construction of sorbents with multiple interactions could be an effective approach. Herein, a cationic-fluorinated covalent organic framework (CF-COF) was prepared by post-modification and used as a magnetic solid-phase extraction adsorbent for adsorption of PFASs. By combining magnetic solid-phase extraction based on CF-COF with liquid chromatography−tandem mass spectrometry (LC − MS/MS), a novel method was developed for determination of eight long-chain PFASs in foods. Under optimized conditions, the method exhibited low detection limits (0.003–0.019 ng/g) and satisfactory recovery rates (73.5–118%) for PFASs. This study introduces a novel idea for the development of adsorbents targeting PFASs, along with a new analytical method for monitoring of PFASs in foods. • CF-COF was synthesized for extracting per- and polyfluoroalkyl substances (PFASs). • There are electrostatic interactions and fluorous affinity between CF-COF and PFASs. • The MSPE−HPLC−MS/MS method was applied for determination of 8 PFASs in food. [ABSTRACT FROM AUTHOR]

[Display omitted] • Sample preparation strategies were compared according to 6 categories of plant-derived foodstuffs. • Detection methods based on liquid chromatography were summarized and discussed. • Limitations were summarized and new directions were proposed for future advancement. Neonicotinoids (NEOs) are the most widely used insecticides globally. They can contaminate or migrate into foodstuffs and exert severe neonic toxicity on humans. Therefore, lots of feasible analytical methods were developed to assure food safety. Nevertheless, there is a lack of evaluation that the impacts of food attributes on the accurate determination of NEOs. This review aims to provide a comprehensive overview of sample preparation methods regarding 6 categories of plant-derived foodstuffs. Currently, QuEChERS as the common strategy can effectively extract NEOs from plant-derived foodstuffs. Various enrichment technologies were developed for trace levels of NEOs in processed foodstuffs, and multifarious novel sorbents provided more possibility for removing complex matrices to lower matrix effects. Additionally, detection methods based on liquid chromatography were summarized and discussed in this review. Finally, some limitations were summarized and new directions were proposed for better advancement. [ABSTRACT FROM AUTHOR]

[Display omitted] • MIC-DV was proposed for food digestion and fluorine determination by ISE. • LOQ values for F after MIC-DV were lower than the AOAC method. • F-ISE determination was carried out directly in the absorbing solution without dilution. • MIC-DV was whiter than MIC and AOAC methods according to WAC principles. This work presents the first report of the application of microwave-induced combustion in disposable vessels (MIC-DV) as a simple and fast sample preparation step for fluoride determination by ion-selective electrode (ISE) in leguminous seeds and oilseeds samples. Several experimental conditions of MIC-DV were evaluated, such as sample mass, absorbing solution, volume of combustion igniter, purging time with oxygen, and the use of successive combustion cycles. The accuracy of MIC-DV/ISE method was evaluated by comparing the results obtained by microwave-induced combustion and determination by ion chromatography, with agreements ranged from 94 to 106%. The method allowed to achieve relatively low limits of quantification (8.3 to 16 µg g−1) comparing to AOAC method (40 µg g−1), besides the use of small amounts of reagents, less handling of digests, making the method greener and with portable features comparing to other methods. [ABSTRACT FROM AUTHOR]

Highlights • Functionalization of amino-terminated carbon nanotubes with isocyanates. • Application of functionalized magnetic carbon nanotubes in MSPE. • Development of MSPE-LC-HRMS method for sulfonamides analysis. Abstract A simple modification method was developed for the functionalization of amino terminated carbon nanotubes (CNT-NH 2) by using isocyanates as modifiers via the nucleophilic addition reaction. Two types of functionalized magnetic carbon nanotubes (MCNT) were prepared through deposition of magnetic nanoparticles on CNT-NH 2 and modification with different isocyanates. p-Tolyl-functionalized MCNT (Tol-MCNT) with better adsorption performance were selected as adsorbent for magnetic solid phase extraction (MSPE), which could extract sulfonamides (SAs) from various milk samples with a enrichment factor of about 30 after optimization. By combining the MSPE with liquid chromatography–high resolution mass spectrometry (LC–HRMS), a new method was developed. Both skimmed and whole milk samples of three brands were analyzed with this method, and 4 SAs including sulfadiazine, sulfisomidine, sulfamethazine and sulfameter were detected with the concentration from unquantifiable to 72 ng/L, which were all well below the maximum residue limits in milk according to the regulations of China and EU. [ABSTRACT FROM AUTHOR]

Highlights • Potential of fast solubilization of 2 g of sample using only HNO 3. • Simple and low cost system with a halogen lamp was used as IR source. • Samples with different fat/protein ratios were used to study the system. • Factorial design and chemometric tools provide fast optimization of the system. Abstract A fast sample preparation procedure based on use of infrared (IR) assisted heating for mineralization of soybean derived samples has been developed for their subsequent multielement analysis by inductively coupled plasma optical emission spectrometry (ICP-OES) and flame atomic absorption spectrometry (FAAS). A cold finger was examined for refluxing of acid vapors to determine its impact on efficiency and economy of digestion. The optimized procedure, based on 1 g subsamples, 8 mL of HNO 3 (65% w/w) and exposure of the mixture to a 500 W IR source for 5 min without refluxing, permitted accurate determination of all analytes in NIST SRM 1568b (rice flour). Detection limits using ICP-OES were (µg/kg) 97, 1.0, 39, 185, 0.47 and 1200 for Ca, Cu, Fe, K, Mn and P, respectively, and 18 for Zn by FAAS. The IR-assisted digestion approach provided a low cost, easy to use system having great potential for implementation in routine analysis of trace elements in soybean and similar matrices. [ABSTRACT FROM AUTHOR]

Highlights • QuEChERS-GC–MS/MS was applied for the extraction of 35 multiclass pesticides. • Four tropical fruits cultivated and exported in Colombia were selected. • The use of analyte protectants and matrix effects were evaluated. • Acceptable recovery values were obtained being the LCL 5 µg/kg. • Samples of each type of tropical fruit were analysed. Abstract In this work, a method has been applied and validated for the determination of a group of 35 multiclass pesticides in the minor tropical fruits rose apple/pomarrosa (Syzygium malaccense), starfruit/carambola (Averrhoa carambola), yoyomo (Spondias purpurea) and papayuela (Vasconcellea pubescens) cultivated and exported in Colombia. The AOAC 2007.1 QuEChERS method, that uses an acetic acid/acetate buffer, was applied together with gas chromatography coupled to a triple quadrupole mass spectrometer. The method was validated in terms of calibration, recovery at three levels of concentration and matrix effects (MEs). A mixture of analyte protectants was also used. A good linearity was obtained in all cases, while the study of the ME revealed the need of developing matrix-matched calibration for many pesticides. Recovery values were in the range 70–120% with relative standard deviation values less than 20% for most of the pesticides studied. The lowest calibration level was 5 µg/kg. Several samples of each type were analysed. [ABSTRACT FROM AUTHOR]

Highlights • A method for the analysis of typical HMOs was validated. • Neutral and acidic HMOs are concomitantly quantified in the same analysis. • The method was applied to analyze HMOs in real human milk samples. • Accurate and reliable quantification of HMOs was achieved. • The method allows the Lewis and Secretor phenotype of the mother to be determined. Abstract Human milk oligosaccharides (HMOs) are free glycans naturally present in human milk that act as prebiotics, prevent pathogen binding, modulate the immune system and support brain development in infants. The HMOs composition and concentrations vary significantly among different women mainly because of the direct influence of the Secretor and Lewis phenotypes on HMOs biosynthesis. Analytical methods that can identify the differences in the HMOs composition and concentrations are a fundamental tool in HMOs research. This paper describes a simple HMOs extraction and analysis for the simultaneous and absolute quantification of neutral and acidic HMOs by graphitized carbon liquid chromatography–electrospray ionization–mass spectrometry. This method was validated and applied to analyze HMOs in the human milk obtained from 10 women. This method allows accurate and reliable quantification of HMOs and can be used to determine differences in HMOs concentrations throughout lactation and among women with different Secretor and Lewis phenotypes. [ABSTRACT FROM AUTHOR]

Highlights • A unified residue analysis method for regulatory testing of veterinary drugs & pesticides in milk was developed. • Sample preparation involved a single sub-sample followed by analysis using UFLC-MS/MS and GC–MS/MS. • The method was validated for 238 pesticides and 78 veterinary drugs. • The method provides precise and accurate analysis with significant savings in time & cost of analysis. Abstract This paper reports a unified sample preparation approach for high-throughput multi-residue analysis of veterinary drugs and pesticides in a single sub-sample of bovine milk. The sample (5 g) was deproteinized with acetonitrile before an aliquot (I) was withdrawn, and the remainder was phase-separated using MgSO 4 and NaCl. The acetonitrile layer (II) was recovered and the extracts combined, cleaned, and solvent-exchanged before the concentrations of veterinary drugs and pesticides were measured by ultra-fast liquid chromatography tandem mass spectrometry (UFLC-MS/MS). As a unique approach, extract II was analyzed simultaneously using gas chromatography tandem mass spectrometry (GC–MS/MS). Method performance for 78 drugs and 238 pesticides complied with CD 2002/657/EC and SANTE/11813/2017 guidelines, respectively, with significant savings in time and cost. Thus, it would be ideal for regulatory analysis of analytes ranging from non-polar organochlorine pesticides to polar drugs, including penicillins, quinolones, and tetracyclines. [ABSTRACT FROM AUTHOR]

Highlights • Rapid extraction of 3 biologically active chemical families from citrus juices. • 16 Major citrus methoxyflavones, coumarins and psoralens separated in 30 min. • UV/fluorescence peak ratios provided unique information for identifications. • Some juices hydrolyze epoxides, form dihydroxides of different biological activity. • Two coumarins identified in orange juice for the first time, confirmed by LC-MS-MS. Abstract A synergistic combination of analytical techniques was developed for the simultaneous determination of the three most biologically active chemical families in citrus juices: methoxylated flavones, coumarins, and furanocoumarins. No rapid methodology has been available to determine them together. A solid phase extraction concentrated these groups and a ternary reverse phase HPLC gradient completely resolved them from other juice components. Two coumarins, isomeranzin and osthole, were identified in a sweet orange (C. sinensis) cultivar, Changyecheng, for the first time. Pummelo juice was characterized by coumarin and furanocoumarin epoxides such as meranzin and epoxybergamottin. No epoxides were observed in the more acidic juices. Added furanocoumarin epoxides hydrolyzed rapidly in the most acidic juices. The ratios of the UV peak areas at 320 nm to the fluorescence emission peaks as well as the ratio of fluorescence emission peaks at 450–400 nm could be used to identify chromatographic peaks. [ABSTRACT FROM AUTHOR]

Highlights • The CCD planning was used to optimize the SPME and SDME techniques. • SDME and SPME showed efficiency in the extraction of 2-phenoxyethanol in fish. • The time determined in this study for total elimination of anesthetic was 24 h. Abstract Solid-phase microextraction (SPME) and single-drop microextraction (SDME) in headspace mode, were used in the residual determination of the anesthetic 2-phenoxyethanol in fish fillets, to ensure food safety. For the optimization of the methodologies the experimental central composite design (CCD) was used, resulting in accurate evaluations with less amount of analysis. The developed methodologies presented good precision in the evaluated range, o limits of detection (LD) and quantification (LQ) for SDME were 0.2 and 0.62 μg mL−1 and for SPME were 0.18 and 0.56 μg mL−1, respectively. In the analyzed samples the determined elimination time of post-anesthesia 2-phenoxyethanol was 12 h for the SDME and 24 h for the SPME, at the anesthesia concentrations evaluated (450–1050 μg mL−1). The two techniques presented viability of application for the residual determination of 2-phenoxyethanol in fish, SPME being more sensitive and automated and SDME with lower operation cost. [ABSTRACT FROM AUTHOR]

[Display omitted] • Optimized, validated and green procedure to quantify xanthophylls in corn grains. • It is efficient, simple, and employs only water and ethanol in the whole process. • It was applied to a variety of samples, evidencing some to be high in zeaxanthin. • Extraction could be scaled up to produce bioactive, food-compatible extracts. Corn grains are a major source of both the bioactive carotenoids zeaxanthin and lutein. Current methods to quantify these substances have some disadvantages related to sustainability and sample throughput. This work aimed to develop a green, efficient, rapid, and reproducible analytical method to quantify these xanthophylls in corn grains. Solvents recommended by the CHEM21 solvent selection guide were screened. The extraction by dynamic maceration and separation by ultra-high-performance liquid chromatography were optimized by design of experiments. Then, the entire analytical procedure was validated and compared with procedures used for the same purpose, including an official one, and applied to different corn samples. The proposed method was demonstrated to be greener, equal to or more efficient, faster, and more reproducible than the comparative methods. The extraction step could be scaled up for industrial production of zeaxanthin- and lutein-enriched extracts, as it uses only compatible food grade ethanol and water. [ABSTRACT FROM AUTHOR]

[Display omitted] • A sorbent composite was one-step electrodeposited on a modified plaswood substate. • The sorbent composite had a large surface area and was highly porous. • The design of the substrate improved the extraction of PAHs in coffee drinks. • The device highly efficiently extracted PAHs in coffee drinks. • The developed device could be reused up to 18 times. Coffee beans can be contaminated during roasting by polycyclic aromatic hydrocarbons (PAHs), some of which have been classified as carcinogens. An extraction device for PAHs in coffee drinks was designed with six compact DC motors rotating six sorbents. The sorbents were plaswood propellers modified by one-step electrodeposition of a poly(ortho -phenylenediamine) and Zn composite (P o PD-Zn). Benzo(a)anthracene (BaA), chrysene (Chry), benzo(b)fluoranthene (BbF), and benzo(a)pyrene (BaP) were chosen as representative PAHs. Scanning electron micrographs of the P o PD-Zn showed a porous structure. The extracted PAHs were quantified by gas chromatography coupled with a flame ionization detector. Detected concentrations of PAHs in coffee drink samples were as follows: BaA 1.4 ± 0.4 to 16.5 ± 0.8 µg L−1; Chry 0.5 ± 0.2 to 2.1 ± 0.5 µg L−1; BbF 2.2 ± 0.6 µg L−1; and BaP 6.2 ± 1.0 µg L−1. Good recoveries ranging from 82.7 ± 1.9% to 99.0 ± 0.5% were obtained. [ABSTRACT FROM AUTHOR]

A fully automated focused infrared lightwave ashing sample preparation system was proposed and applied to the pretreatment of volatile arsenic, cadmium and lead in plant foods prior to inductively coupled plasma mass spectrometry (ICP-MS) determination. All the steps of ashing pretreatment were automatically accomplished within forty minutes. Gold-plated infrared quartz tubes produced focused infrared to supply a rapid heating. Ozone was used to accelerate sample carbonization. A cool trap was used to capture volatile arsenic, cadmium and lead. Three certified plant food reference materials were determined. The recoveries of the three elements were between 90% and 107%. Five real plant foods were analyzed by the proposed method and microwave digestion. The results showed no significant difference. [ABSTRACT FROM AUTHOR]

A sensitive GC–MS method is reported for the determination of twelve polycyclic aromatic hydrocarbons (PAHs) in baby food. The sample preparation involves QuEChERS extraction combined with low-density solvent dispersive liquid–liquid microextraction (LDS-DLLME) and ultra-low temperature (−80 °C). Plackett–Burman screening design was employed to identify the main sample preparation variables that affect the extraction efficiency, such as the volume of toluene used in LDS-DLLME. The suitability of proposed method was verified by analytical selectivity, linearity in solvent and matrix-matched calibration curves and adequate recoveries (72–112%) and precision (RSD values ≤11%), under repeatability and within-laboratory reproducibility conditions. High analytical sensitivity was achieved for the monitoring of PAHs at the strict limit of 1 µg kg −1 fixed by the European Commission for baby foods. The validated method was applied to thirty-two commercial baby food samples, and the investigated PAHs were not detected in any sample. [ABSTRACT FROM AUTHOR]

A method for arsenic speciation in shark, shrimp, squid, oyster and scallop using liquid chromatography coupled to inductively coupled plasma triple quadrupole mass spectrometry (LC-ICP-MS/MS) was proposed. Suitable sensitivity and selectivity by LC-ICP-MS/MS were obtained using 10 mmol L −1 (NH 4 ) 2 HPO 4 diluted in 1% methanol (pH 8.65) as mobile phase. Recoveries from 90 to 104% for arsenobetaine (AsB), arsenite [As(III)], dimethylarsinic acid (DMA), monomethylarsonic acid (MMA) and arsenate [As(V)] were obtained for all samples. A certificated reference material was also analyzed and the sum of As species was in agreement with the total As concentration. Limits of quantification (LOQ) for AsB, As(III), DMA, MMA, and As(V) were 6, 30, 6, 12 and 26 ng g −1 , respectively. Higher concentration of AsB was found in all seafood, while As(III) and DMA were found only in oyster. Arsenate was found in squid and scallops, and MMA was below the LOQ in all samples. [ABSTRACT FROM AUTHOR]

Aiming to develop a straightforward magnetic-based sample preparation methodology for the selective extraction of dimethoate from olive oil, the synthesis of dimethoate-imprinted polymer on the surface of modified magnetic nanoparticles has been attempted. Molecular recognition assays have proven their suitability for the selective pre-concentration of dimethoate. Mechanistic basis for template selective recognition has been explored using a quantum chemical approach, providing new insights about the mechanisms underlying template recognition. Thus, a magnetic molecularly imprinted solid-phase extraction method was developed allowing the extraction of dimethoate from spiked olive oil samples, at levels similar to the maximum residue limits imposed by legislation, followed by the quantification of their levels by high-performance liquid chromatography with diode-array detection. Recoveries of 94.55% were obtained, with relative standard deviations lower than 0.53% (n = 3). The developed sample preparation technique enables a selective pre-concentration/enrichment of dimethoate from olive oil matrix with minimum handling and less solvent consumption. [ABSTRACT FROM AUTHOR]

In this study a simple and fast multi-class method for the determination of veterinary drugs in bovine liver, kidney and muscle was developed. The method employed acetonitrile for extraction followed by clean-up with EMR-Lipid® sorbent and trichloracetic acid. Tests indicated that the use of TCA was most effective when added in the final step of the clean-up procedure instead of during extraction. Different sorbents were tested and optimized using central composite design and the analytes determined by ultra-high-performance liquid chromatographic-tandem mass spectrometry (UHPLC-MS/MS). The method was validated according the European Commission Decision 2002/657 presenting satisfactory results for 69 veterinary drugs in bovine liver and 68 compounds in bovine muscle and kidney. The method was applied in real samples and in proficiency tests and proved to be adequate for routine analysis. Residues of abamectin, doramectin, eprinomectin and ivermectin were found in samples of bovine muscle and only ivermectin in bovine liver. [ABSTRACT FROM AUTHOR]

An eco-friendly method for indirect determining phosphorus and sulfur in animal feed by ion chromatography was proposed. Using this method, it was possible to digest 500 mg of animal feed in a microwave system under oxygen pressure (20 bar) using only a diluted acid solution (2 mol L −1 HNO 3 ). The accuracy of the proposed method was evaluated by recovery tests, by analysis of reference material (RM) and by comparison of the results with those obtained using conventional microwave-assisted digestion. Moreover, P results were compared with those obtained from the method recommended by AOAC International for animal feed (Method nr. 965.17) and no significant differences were found between the results. Recoveries for P and S were between 94 and 97%, and agreements with the reference values of RM were better than 94%. Phosphorus and S concentrations in animal feeds ranged from 10,026 to 28,357 mg kg −1 and 2259 to 4601 mg kg −1 , respectively. [ABSTRACT FROM AUTHOR]

Booster biocides have been widely applied to ships and other submerged structures. These compounds can be released into the marine environment as the result of vessel hull leaching and may remain in different environmental compartments. This study aimed at introducing an environmentally friendly procedure for the extraction of irgarol and diuron from fish samples by vortex-assisted matrix solid phase dispersion (VA-MSPD) with detection by liquid chromatography tandem mass spectrometry. Different types of solid supports and solvents were evaluated. The best results were found when 0.5 g mussel shell, 0.5 g sodium sulfate and 5 mL ethanol were used. Analytical recoveries ranged from 81 to 110%, with RSD below 10%, whereas the matrix effect was between −17 and 1% (for all samples under study). LOQ values of irgarol and diuron were 5 and 50 ng g −1 , respectively. The method under investigation proved to be a promising alternative to controlling contamination of fish by booster biocides, with low consumption of biodegradable reagents. [ABSTRACT FROM AUTHOR]

The bioaccessibility of Ca, Cu, Fe, Mg, Zn, and crude protein was evaluated after submitting beef, pork, and chicken to five different thermal treatments. The bioaccessibility of crude protein and metals were simulated by using in vitro enzymatic digestion with a gastric fluid solution and dialysability approach. Inductively coupled plasma optical spectrometry was used to quantify the dialyzable fraction and the total mineral content after microwave-assisted digestion. Graphite furnace atomic absorption spectrometry quantified Cu in chicken dialyzable fraction. The increase of temperature and heat exposure period decreased the protein bioaccessibility. Considering the total and dialyzable fraction, beef is an important source of Cu, Fe, Mg, and Zn to the human diet. The results of Fourier-transform infrared spectroscopy indicated physical changes in the treated samples related to protein denaturation, which was probably responsible for the decreased bioaccessibility of minerals and protein, mainly at higher temperatures. [ABSTRACT FROM AUTHOR]

[Display omitted] • Imazalil used in postharvest for disease and pest control in papaya. • Monitoring the dissipation/migration of imazalil in papaya skin, pulp, and seeds. • Extraction and chromatographic methods for determination of pesticide residues. • Evaluation of papaya physicochemical parameters during refrigerated storage. Methods involving solid-liquid extraction with low-temperature partition and analysis by gas chromatography coupled to mass spectrometry (GC–MS) were validated to investigate the dissipation/migration of residues of the postharvest fungicide imazalil in papaya skin, pulp, and seeds. The fruits were stored for 23 days (14 °C). Every two days, fruits from the control group and those treated with imazalil had their skin, outer pulp, inner pulp, and seeds separated and then analyzed by GC–MS. After the 23rd day, about 70% of the imazalil had dissipated. Most of the remaining residue was found in the skin; however, the small amount migrating into the pulp was above the maximum residue levels allowed by the regulatory agencies. Imazalil residue was also detected in seeds at concentrations lower than the LOQ (0.025 mg kg−1). Mass loss was the only quality parameter that showed a significant difference between the fruits of the control and study groups. [ABSTRACT FROM AUTHOR]

Fabric phase sorptive extraction (FPSE), a novel sorbent-based microextraction method, was evaluated as a simple and rapid strategy for the extraction of four penicillin antibiotic residues (benzylpenicillin, cloxacillin, dicloxacillin and oxacillin) from cows’ milk, without prior protein precipitation. Time-consuming solvent evaporation and reconstitution steps were eliminated successfully from the sample preparation workflow. FPSE utilizes a flexible fabric substrate, chemically coated with sol-gel derived, highly efficient, organic-inorganic hybrid sorbent as the extraction medium. Herein short-chain poly(ethylene glycol) provided optimum extraction sensitivity for the selected penicillins, which were analysed using an RP-HPLC method, validated according to the European Decision 657/2002/EC. The limit of quantitation was 10 μg/kg for benzylpenicillin, 20 μg/kg for cloxacillin, 25 μg/kg dicloxacillin and 30 μg/kg oxacillin. These are a similar order of magnitude with those reported in the literature and (with the exception of benzylpenicillin) are less than the maximum residue limits (MRL) set by European legislation. [ABSTRACT FROM AUTHOR]

A new approach to the analysis of Cu, Fe, Mn and Zn in flaxseed was developed based on infrared-assisted acid digestion. Quantitation by flame atomic absorption spectrometry yields results in agreement with those arising from aggressive total decomposition using conventional microwave-assisted (MW) digestions. A full factorial design in two levels was applied to evaluate the impact of significant variables for all elements to determine optimal experimental conditions. A desirability function revealed these to be: 2.0 g sample mass, 8 mL of HNO 3 and 8 min of heating time in the IR system. Precision better than 10% (RSD) was obtained, superior to that of a combined IR-MW approach. Sample preparation based on IR-assisted digestion provides a rapid and inexpensive alternative to other conventional techniques for the analysis of complex samples and is able to accommodate relatively large masses of sample, alleviating potential homogeneity issues as well as enhancing detection power. [ABSTRACT FROM AUTHOR]

A method for Br and I determination in whole egg powder and its fractions (egg white and yolk) was developed by combining microwave-induced combustion (MIC) and inductively coupled plasma mass spectrometry (ICP-MS). Using the MIC method, 350 mg of whole egg powder and its fractions were efficiently digested using 50 mmol L −1 NH 4 OH as an absorbing solution. The limits of detection for Br and I using the MIC method followed by ICP-MS determination were 0.039 and 0.015 μg g −1 , respectively. Using the proposed method, agreements with the reference values between 97 and 104% for Br and I were obtained by analysis of reference material NIST 8435. Finally, it was possible to observe that Br concentration (4.59–5.29 μg g −1 ) was higher than I (0.150–2.28 μg g −1 ) for all the evaluated samples. [ABSTRACT FROM AUTHOR]

[Display omitted] • Progress of microextraction techniques and the trends in automation are summarized. • Evolution and break though of HRMS in determination of sweeteners are discussed. • Pros and cons of extraction and determination methods are comprehensively compared. • Applications and perspective of purification and quantification ways are presented. Sweeteners play an irreplaceable role in daily life and have been found in multitudinous food products. However, excessive or unreasonable intake of sweeteners as food additives brings about untoward problems due to the accumulation in the human body. Therefore, a comprehensive review of different sweeteners' pretreatment and determination methods is urgently needed. In this review, we comprehensively reviewed the progress of different pretreatment and detection methods for sweeteners in various food, focusing on the latest development since 2015. Current state-of-the-art technologies, such as headspace single-drop microextraction, ultrasound-assisted emulsification microextraction, solid-phase microextraction, two-dimensional liquid chromatography, and high-resolution mass spectrometry, are thoroughly discussed. The advantages, disadvantages, critical comments, and future perspectives are also proposed. This review is expected to provide rewarding insights into the future development and broad application of pretreatment and detection methods for sweeteners in different food samples. [ABSTRACT FROM AUTHOR]

• Bidimensional analysis composed of PLE-SPE and HPLC-PDA is proposed. • New PLE mode with solvent gradient is efficiently applied to industrial apple pomace. • Gradient extraction method, temperature, and static time play important roles in PLE. • PLE-SPE-HPLC-PDA process shows feasible to analyze industrial apple pomace comprehensively. • PLE-SPE-HPLC-PDA achieves quantitative extraction while real-time process monitoring. Due to the complex characteristics and variable composition of apple pomace, sample preparation for chromatographic analysis is a great challenge. To solve this problem, we proposed using a solvent gradient using Pressurized Liquid Extraction (PLE), where the solvent gradually changes from water to ethanol during the extraction. Different dynamic gradients, static time, and temperatures were evaluated and showed relevant effects on the yields of target analytes. It was possible to improve extraction yields of compounds with different characteristics using the extraction solvent gradient. By coupling solid-phase extraction in-line, it was possible to separate compounds into fractions, where furfural, HMF, and chlorogenic acid gradually eluted from the adsorbent. At the same time, flavonoids were retained and eluted in the later fractions. On-line analysis by HPLC provided real-time information about the process and permitted the creation of a 3D chromatogram of the sample. [ABSTRACT FROM AUTHOR]

• A simplified d-SPE method was designed and developed by using shaped MOF sorbent. • The method avoids the centrifugation or filtration that is needed in normal d-SPE. • The sorbent can directly extract the targets from homogenized samples. • The matrix interferences were efficiently removed. • The adsorption interactions between the shaped sorbent and targets were studied. A facile, efficient and reliable method was designed and established to analyze the plant growth regulators (PGRs) in citrus fruit, based on a simplified dispersive solid-phase extraction (d-SPE) using a shaped zirconium-based metal–organic framework (UiO-66-PDMS bead) as the sorbent. In this method, UiO-66-PDMS beads directly extracted the targets from the homogenized and could be easily separated with a tweezer. It avoided the centrifugation or filtration operation required in normal d-SPE, greatly simplifying the d-SPE process. Moreover, the matrix substances were efficiently removed by this d-SPE process. The method showed good linearities (R2 ≥ 0.9995) and limits of detection (0.09–0.17 ng/g). The recoveries were in the range of 80.7–97.5 %. The intra-day and inter-day precisions were 1.5–6.3 % and 4.6–11.7 %, respectively. Additionally, the adsorption interactions between UiO-66-PDMS bead and PGRs were studied by ATR-FTIR and UV–vis DRS. Furthermore, the method was employed to screen the PGRs in ten different citrus fruits. [ABSTRACT FROM AUTHOR]

[Display omitted] • The types of functionalized COFs were presented. • The recent applications of functionalized COFs in food sample preparation were reviewed. • Functionalization overcame the flaws and enhanced the advantages of COFs. • Functionalization of COFs improved extraction efficiency and selectivity of targets. • The challenges and opportunities in the field were described. Because food contaminants harm human body in varied degrees, accurate detection of them has drawn great interest. Due to the complex matrix effect and the trace level of contaminants, efficient and reliable sample preparation is required before detection. Covalent organic frameworks (COFs) used as extraction materials for sample preparation, displayed great prospect in the food field. However, extraction selectivity and enrichment effect were limited by available COFs. To solve the issues, some COFs were functionalized for specific functions and applications. This paper overviews the main functionalized strategy for COFs, and the applications of functionalized COFs in food field from 2018 to 2022. Different types of species, such as organic group-modified COFs, Fe 3 O 4 @COFs, COFs@metal organic frameworks, molecularly imprinted polymer-functionalized COFs, etc., have been introduced in solid-phase extraction and microextraction. These adsorbents effectively captured various analytes from foods. Moreover, challenges and prospects of the functionalized COFs in food sample preparation are presented. [ABSTRACT FROM AUTHOR]

• MIP-PR prepared at room temperature recognised PFOA and PFOS. • MIP-PR had the advantages of large surface area, easy synthesis, and low cost. • MIP-PR had large adsorption capacity, strong selectivity, and rapid mass transfer. • MIP-PR-DFE allowed extraction of PFOA and PFOS from milk in 5 min. • MIP-PR-DFE-LC-MS/MS provided a new idea for the analysis of PFOA and PFOS. Perfluorooctanoic acid (PFOA) and perfluorooctane sulfonate (PFOS) are emerging pollutants that threaten food safety. Herein, a rapid, accurate, and selective method for determination of PFOA and PFOS in milk was established by using new molecularly imprinted phenolic resin (MIP-PR) as the adsorbent of dispersive filter extraction (DFE) combined with liquid chromatography-tandem mass spectrometry (LC-MS/MS). MIP-PR was synthesized at room-temperature using m-aminophenol, glutaraldehyde, and perfluorononanoic acid as the monomers, cross-linkers, and virtual templates, respectively, and exhibited rapid mass transfer (30 s), high selectivity (imprinted factors > 3.7), and large adsorption capacity (>54.6 mg/g). Compared with reported methods, the developed MIP-PR–DFE method is fast, selective, inexpensive, and shows good purification and enrichment efficiency. The proposed MIP-PR–DFE–LC-MS/MS exhibited low limits of detection (0.006–0.022 ng/mL), high recoveries (94.7–109 %), and good precision (RSDs ≤ 9.5 %). This study provides a new idea for the development of imprinted resin adsorbents for perfluorinated compound, and a new method for sample pretreatment for monitoring of PFOA and PFOS in food. [ABSTRACT FROM AUTHOR]

• Quantitative validation study for mycotoxins in food by LC-MS/MS. • Estimation of uncertainty by bottom-up method. • Co-occurrence of multi-mycotoxins in cocoa beans. The aim of this manuscript was to validate and apply an analytical methodology for the simultaneous determination of 34 mycotoxins in cocoa. The extraction method used in the tests was a liquid–liquid partition by NaCl addition with a freezing step followed by quantification using LC-MS/MS. The results were discussed based on national and international directives for food contaminants. The recoveries and precision were adequate, except for the mycotoxins ionized with the ammonium adduct (NH 4 +), E-cristinine and β-ZOL. This result directly influenced the measurement uncertainty of these mycotoxins, because the precision and the correction factor of the recovery were the factors with the greatest impact on the uncertainty of the method. The evaluation of the matrix effect showed considerable signal suppression for 53 % of the evaluated mycotoxins. Nevertheless, the mycotoxins exhibited relatively low quantification limits, with values between 1 and 75 μg kg−1. The validated methodology was applied to 15 cocoa samples collected in warehouses in Brazil. Positive results were found for all the evaluated samples, in which nine toxins were detected out of the 34 investigated. [ABSTRACT FROM AUTHOR]

A new high-performance liquid chromatography with ​fluorescence detection (HPLC-FLD) method was developed for determination of piperazine residues in food animal products. Samples were extracted with formic acid in water and purified using the PCX cartridge. Following purification, the samples were derivatized using dansyl chloride, and the analyte was separated using water/acetonitrile as a mobile phase. The calibration curves showed good linearity over a concentration range of 20–120 ng/g with coefficient of determination ( R 2 ) ⩾ 0.996. The intra-day accuracy (presented as recovery %) and precision (presented as relative standard deviation, RSD %) were 81–97.3% and 0.83–6.87%, whereas, the inter-day values were 80.5–96.8% and 1.7–6.8%, respectively. The limit of quantification (LOQ) was 20 ng/g, which was considerably lower than the maximum residue limit (MRL). The developed method was used to monitor market samples, and piperazine was not detected in any of the samples. To our knowledge, this is the first study in which the detection of piperazine in various food and animal products by using a sensitive and reliable analytical method has been described. [ABSTRACT FROM AUTHOR]

An ultrasound-assisted extraction procedure was evaluated for the multi-element determination of Cu, Mn, Ca, and Mg in alternative oilseed crops using flame atomic absorption spectrometry. The best results were obtained when 0.3 g of samples were used to extract the mineral content using 10 mL of a 1.40 mol L −1 HNO 3 solution for 10 min at 25 °C. The accuracy and precision of the analysis were evaluated using two oilseed reference materials, and the results were in agreement with reference values at 95% confidence level (paired t- test). The method was used to analyze five oilseed samples and the results were in agreement with those obtained using a closed-vessel microwave-assisted acid digestion system for sample preparation. The relative standard deviations were 0.52–6.13% for all of the standard and sample measurements, and the limits of detection were 666.7, 416.7, 333.4 μg g −1 , and 3.5 mg g −1 for Cu, Mn, Ca, and Mg, respectively. [ABSTRACT FROM AUTHOR]

Fabric phase sorptive extraction (FPSE) is a novel sample preparation technique which utilizes advanced material properties of sol–gel derived microextraction sorbents and the hydrophilic property of the cellulose fabric substrate, resulting in a highly sensitive and fast microextraction device, capable of extracting target analyte(s) from any complex aqueous sample matrices. Due to the low organic solvent consumption, FPSE meets all green analytical chemistry (GAC) criteria. This technique was applied, for the first time, for the determination of sulfonamides residues in milk using a highly polar sol–gel poly(ethylene glycol) (sol–gel PEG) coated FPSE media. The developed HPLC method was validated according to the European Union Decision 2002/657/EC. Decision limit (CC α ) values were 116.5 μg kg −1 for sulfamethazine, 114.4 μg kg −1 for sulfisoxazole and 94.7 μg kg −1 for sulfadimethoxine, whereas the corresponding results for detection capability (CC β ) were 120.4 μg kg −1 for sulfamethazine, 118.5 μg kg −1 for sulfisoxazole and 104.1 μg kg −1 for sulfadimethoxine. [ABSTRACT FROM AUTHOR]

This study describes a combination between hollow fiber membrane and dispersive liquid–liquid microextraction for determination of aflatoxins in soybean juice by HPLC. The main advantage of this approach is the use of non-chlorinated solvent and small amounts of organic solvents. The optimum extraction conditions were 1-octanol as immobilized solvent; toluene and acetone at 1:5 ratio as extraction and disperser solvents (100 μL), NaCl at 2% of the sample volume and extraction time of 60 min. The optimal condition for the liquid desorption was 150 μL acetonitrile:water (50:50 v/v) and desorption time of 20 min. The linear range varied from 0.03 to 21 μg L −1 , with R 2 coefficients ranging from 0.9940 to 0.9995. The limits of detection and quantification ranged from 0.01 μg L −1 to 0.03 μg L −1 and from 0.03 μg L −1 to 0.1 μg L −1 , respectively. Recovery tests ranged from 72% to 117% and accuracy between 12% and 18%. [ABSTRACT FROM AUTHOR]

This paper reports a selective and sensitive method for multiresidue determination of 119 chemical residues including pesticides and polyaromatic hydrocarbons (PAH) in high fatty fish matrix. The novel sample preparation method involved extraction of the target analytes from homogenized fish meat (5 g) in acetonitrile (15 mL, 1% acetic acid) after three-phase partitioning with hexane (2 mL) and the remaining aqueous layer. An aliquot (1.5 mL) of the acetonitrile layer was aspirated and subjected to two-stage dispersive solid phase extraction (dSPE) cleanup and the residues were finally estimated by gas chromatography mass spectrometry with selected reaction monitoring (GC–MS/MS). The co-eluted matrix components were identified on the basis of their accurate mass by GC with quadrupole time of flight MS. Addition of hexane during extraction and optimized dSPE cleanup significantly minimized the matrix effects. Recoveries at 10, 25 and 50 μg/kg were within 60–120% with associated precision, RSD < 11%. [ABSTRACT FROM AUTHOR]