Microplastics and nanoplastics: Exposure and toxicological effects require important analysis considerations.

Microplastics (MPs) and nanoplastics (NPs) pervade both the environment and the food chain, originating from the degradation of plastic materials from various sources. Their ubiquitous presence raises concerns for ecosystem safety, as well as the health of animals and humans. While evidence suggests their infiltration into mammalian and human tissues and their association with several diseases, the precise toxicological effects remain elusive and require further investigation.

Partitioning and in vitro bioaccessibility of apple polyphenols during mechanical and physiological extraction: A hierarchical clustering analysis with LC-ESI-QTOF-MS/MS.

Polyphenol partitioning during mechanical (cold-pressing) and physiological (digestion) extraction at the individual polyphenol and subclass level was investigated. UHPLC-ESI-QTOF-MS/MS analysis yielded a comprehensive identification of 45 polyphenols whose semi-quantification revealed a hierarchical clustering strongly determined by polyphenol structure and their location within the apple tissue. For instance, pomace retained most flavonols and flavanols (degree of polymerization DP 5-7), which were highly hydrophobic, hydroxylated, or large (>434 Da), and more abundant in peel.

Untargeted screening and in silico toxicity assessment of semi- and non-volatile compounds migrating from polysaccharide-based food contact materials.

The chemical safety of representative polysaccharide films made with pea starch, organocatalytic acetylated pea starch and pectin was investigated at different migration conditions (20 °C/10 days, 70 °C/2 h) using two official simulants signifying hydrophilic (simulant A, 10% ethanol) or lipophilic (simulant D1, 50% ethanol) foods. Migrating semi-volatile and non-volatile compounds were identified and semi-quantified by ultra-high performance liquid chromatography-trap ion mobility time-of-flight mass spectrometry (UHPLC-TIMS-TOF-MS/MS), whereas their toxicity was evaluated by in silico models based on qualitative structure activity (QSAR). Physicochemical analysis revealed polymer wash-off into the simulants.

Analysis of oligomers to assess exposure to microplastics from foods. A perspective.

There is an emerging interest in evaluating the presence of microplastic (MP) and nanoplastic (NP) residues in food. Despite their potential threat to human health, there is still a need for harmonized methods to evaluate and quantify their presence. Incomplete polymerization may occur during the production of plastic.

Impact of the Structural Modifications of Potato Protein in the Digestibility Process under Semi-Dynamic Simulated Human Gastrointestinal In Vitro System.

The raising consumer demand for plant-derived proteins has led to an increased production of alternative protein ingredients with varying processing histories. In this study, we used a commercially available potato protein ingredient with a nutritionally valuable amino acid profile and high technological functionality to evaluate if the digestibility of a suspension with the same composition is affected by differences in the structure. Four isocaloric (4% protein, /) matrices (suspension, gel, foam and heat-set foam) were prepared and their gastrointestinal fate was followed utilizing a semi-dynamic in vitro digestion model.

Thermal degradation of metabolites in urine using multiple isotope-labelled internal standards for off-line GC metabolomics - effects of injector and oven temperatures.

Thermal processes are widely used in small molecule chemical analysis and metabolomics for derivatization, vaporization, chromatography, and ionization, especially in gas chromatography mass spectrometry (GC/MS). An optimized derivatization protocol has been successfully applied using multiple isotope labelled analytical internal standards of selected deuterated and C selected compounds, covering a range of different groups of metabolites for non-automated GC metabolomics (off-line). Moreover, the study was also realized in a pooled urine sample, following metabolic profiling.

A fast SALLE GC-MS/MS multi-analyte method for the determination of 75 food packaging substances in food simulants.

A simple and fast method was developed for the simultaneous determination of 75 plastic food contact material (FCM) in liquid food simulants, at levels of a few ng g. The method employs an optimised salt-assisted liquid-liquid extraction for all EU-regulated ethanol/HO food simulants, in the presence of 10% NaCl (simulants A and C) or 5% NaCl (simulant D1), and dichloromethane as the extracting solvent. Gas chromatography with triple-quad MS operating in multiple reaction monitoring acquisition was used, applying isotope dilution with selected deuterated compounds.

Food Contact Materials: Migration and Analysis. Challenges and Limitations on Identification and Quantification.

Food contact materials (FCM) are defined as the objects and materials intended to come into direct or indirect contact with foodstuff, while food contact articles are defined as objects, being equipment, containers, packaging and various utensils which are clearly intended to be used for the manufacture, preparation, conservation, flow, transport or handling of foodstuffs [...

Identification and Analytical Characterization of a Novel Synthetic Cannabinoid-Type Substance in Herbal Material in Europe.

The rapid diffusion of new psychoactive substances (NPS) presents unprecedented challenges to both customs authorities and analytical laboratories involved in their detection and characterization. In this study an analytical approach to the identification and structural elucidation of a novel synthetic cannabimimetic, quinolin-8-yl-3-[(4,4-difluoropiperidin-1-yl) sulfonyl]-4-methylbenzoate (2F-QMPSB), detected in seized herbal material, is detailed. An acid precursor 4-methyl-3-(4,4-difluoro-1-piperidinylsulfonyl) benzoic acid (2F-MPSBA), has also been identified in the same seized material.

Development and validation of an UHPLC-qTOF-MS method for the quantification of cyclic polyesters oligomers in pasta by applying a modified QuEChERS clean-up.

An Ultra High-Performance Liquid chromatography method quadruple time-of-flight mass spectrometry has been developed for the analysis of 11 cyclic polyesters oligomers, following a modified QuEChERS clean-up with alumina/primary secondary amine, in pasta. Target analytes were polyethylene terephthalate (PET) 1 series cyclic dimer to heptamer, polybutylene terephthalate (PBT) dimer to pentamer and a polyurethane oligomer. Standard addition method was applied for the calibration, and the limits of quantification ranged from 3.

Analysis of PBT and PET cyclic oligomers in extracts of coffee capsules and food simulants by a HPLC-UV/FLD method.

A HPLC-UV/FLD method was validated for the quantification of six polyethylene terephthalate (PET) and four polybutylene terephthalate (PBT) oligomers. PBT oligomers are EU regulated, while the PET ones are considered non-intentionally added substances (NIAS). LOQs were higher than 0.

Development and validation of a fast gas chromatography mass spectrometry method for the quantification of selected non-intentionally added substances and polystyrene/polyurethane oligomers in liquid food simulants.

A simple, fast, sensitive and reliable method was developed for the simultaneous determination of 13 food contact materials (FCM) regulated substances and non-intentionally added substances (NIAS) migrating into official food simulants. The method has been optimized to quantify the monomers styrene and α-methyl styrene, selected polystyrene oligomers (dimers, trimers) and polyester urethane-based oligomers (PU) cyclic oligomers, as well as cyclic NIAS originating from food packaging such as 2,6-Di-tert-butylbenzoquinone and 7,9-Di-tert-butyl-1-oxaspiro(4,5)deca-6,9-diene-2,8-dione. The method employs liquid-liquid extraction of aqueous ethanol food simulants with dichloromethane, and analysis with gas chromatography coupled to mass spectrometry (GC-MS) with a total analysis time of less than 16 min, with limits of detections ranging from 0.

A Salting-out Liquid-Liquid extraction (SALLE) for the analysis of caprolactam and 2,4-di-tert butyl phenol in water and food simulants. Study of the salinity effect to specific migration from food contact materials.

Caprolactam and 2,4-di-tert-butyl phenol (2,4-DTBP) are substances typically found in some food contact materials (FCMs). They are known to often migrate into food, and are difficult to analyse in liquid food simulants using GC. In this work a simple salting-out Liquid-Liquid Extraction (SALLE) for the analysis of both substances in water and the official food simulant A (10 % v/v ethanol, Regulation (EU) No.

Development and validation of a multi-analyte GC-MS method for the determination of 84 substances from plastic food contact materials.

Chemical substances shall not migrate from food contact materials (FCM) at levels that are potentially harmful for the consumers. Each of the current analytical methods applied to verify the migration of substances from FCM covers only one or few substances. There is a very limited number of publications on the development of analytical methods allowing the simultaneous determination of several classes of FCM substances, and almost none of them reported methods entirely dedicated to the ones in the positive list of Commission Regulation (EU) No.

Proficiency test on the determination of polyethylene and polybutylene terephthalate cyclic oligomers in a food simulant.

The outcome of a proficiency test (PT) organised by the European Union Reference Laboratory for Food Contact Materials (EURL-FCM) is presented. The PT was set up to assess the analytical performance of National Reference Laboratories (NRLs) and Official Control Laboratories (OCLs) in the determination of mass fractions of polyethylene terephthalate (PET) and polybutylene terephthalate (PBT) cyclic dimers and trimers in the official food simulant D1 containing ethanol and water (50:50 v/v). The EURL-FCM had developed and validated an analytical method based on HPLC-UV to monitor the homogeneity and stability of the target oligomers in the PT test items and to determine the respective assigned values, as prescribed in ISO 17043, 2010ISO 17043, 2010.

Quantification of PET cyclic and linear oligomers in teabags by a validated LC-MS method - In silico toxicity assessment and consumer's exposure.

Determination of polyethylene terephthalate (PET) dimer up to heptamer 1st series cyclic oligomers, applying an LC-qTOF-MS method, has been developed and validated. Recoveries ranged between 80 and 112% with RSDs lower than 15%. An innovative semi-quantitative approach has been applied for 2nd and 3rd series cyclic oligomers, using the closest structural-similar 1st series cyclic oligomer standard as analytical reference.

Influence of pre-heating of food contact polypropylene cups on its physical structure and on the migration of additives.

Laboratories unexpectedly carried out pre-heating of polypropylene beverage cups prior to performing a migration test in a proficiency test. Principal component analysis of the data collected showed that the preheating temperature of the cups contributed to an increased variance of the data and distinguishing pre-heating and non-pre-heating groups. This triggered to study the effect of applying such pre-heating on the physical structure of the material and on the migration of additives to food simulant D1 (ethanol 50% v/v).

Isolation, Characterization and Structural Elucidation of Polybutylene Terephthalate Cyclic Oligomers and Purity Assessment Using a ¹H qNMR Method.

The use of polybutylene terephthalate (PBT) as a food contact material is increasing over the last years. Typical contaminations in the final PBT product include its cyclic oligomers, which are allowed as additives in food contact plastics according to Regulation (EU) No. 10/2011.

Development and validation of an HPLC method with fluorescence detection for the determination of fluorescent whitening agents migrating from plastic beverage cups.

An HPLC method with fluorescence detection has been developed and validated for the quantification of six fluorescent whitening agents (FWA) in plastic beverage cups after extraction and in food simulants after migration at 70°C for 2 h. The sensitivity of the method was high with LODs ranging from 0.053 to 0.

Analytical Methodologies for the Assessment of Phthalate Exposure in Humans.

Screening and quantification of phthalate metabolites in biological matrices provide information on the phthalate exposure. The preferred tool for the determination of phthalate metabolites is liquid chromatography-mass spectrometry, typically preceded by a sample extraction step. Method development for the determination of phthalate metabolites by hyphenated techniques faces challenges due to the widespread occurrence of phthalates in the laboratory and sample collection materials that impairs their accurate quantification.

A hydrophilic interaction chromatography-tandem mass spectrometry method for amino acid profiling in mussels.

A UHPLC-HILIC-tandem MS method has been developed and validated for the quantification of 21 amino acids (20 protein amino acids and cystine) in their free form (FAA) and as protein constituents (total amino acids, TAA) in a rich protein food matrix such as lyophilized mussels (Mytilus galloprovincialis) samples. FAA were analyzed after suspending the samples in the presence of trichloroacetic acid in order to prevent dissolving the proteins, while TAA were determined after acid hydrolysis with 6M HCl in the presence of 4% v/v thioglycolic acid as a reducing agent. In hydrolysed samples 17 amino acids could be determined since tryptophan, cysteine, cystine and asparagine were degraded during acid hydrolysis.

Determination of tocopherol and tocotrienol content of Greek barley varieties under conventional and organic cultivation techniques using validated reverse phase high-performance liquid chromatography method.

Background: Tocotrienols and tocopherols (tocols) are important phytochemical compounds with antioxidant activity and potential benefits for human health. Among cereals, barley is a good source of tocols. In the present study the effect of two cultivation methods, organic and conventional, on the tocol content in 12 Greek barley varieties was investigated.

A multi-residue method for pesticide residue analysis in rice grains using matrix solid-phase dispersion extraction and high-performance liquid chromatography-diode array detection.

Pesticides are widely used in rice cultivation, often resulting in detection of their residues in rice grains. So far, no analytical method has been available for the simultaneous determination of most rice pesticides in rice grains. This paper reports the development and validation of such a method for the determination of eight rice pesticides (penoxsulam tricyclazole, propanil, azoxystrobin, molinate, profoxydim, cyhalofop-butyl, deltamethrin) and 3,4-dichloroaniline, the main metabolite of propanil.