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N. Olluyn, E. Verleysen, L. Siciliani, D. A. Esteban, S. Mathioudaki, S. Bals, S. Sharma, J. Mast, J. Van Loco
Identification and characterization of inorganic food additives and pearlescent pigments in sprays for food decoration by STEM-EDX

Food colorants are applied in commercial products and domestic cooking to enhance the appearance of food. To obtain specific hues, inorganic food additives containing (nano)particles are mixed in varying concentrations, and pearlescent pigments consisting of mica platelets coated with a layer of titanium dioxide and/or iron oxide particles, are applied to provide glitter effects1 . For assessing potential risks of multi-constituent substances and mixtures, characterisation of the fraction of small particles, including the particle size distribution, is needed for each single constituent or each component in the mixture2 . This is challenging for control laboratories and only limited guidance is currently available3 . This study developed electron microscopy-based methods to identify and characterize the particles of individual components in eight commercially available food-decoration sprays of different colours, containing mixtures of food additives and pearlescent pigments. No dispersion protocols or purifications steps were applied so as to faithfully reproduce the properties of the particles consumers are exposed to. Samples were prepared by spraying 5 mL in a glass vial and coated on EM-grids using the grid-on-drop method. Scanning transmission electron microscopy (STEM) combined with energy dispersive X-ray spectroscopy (EDX) allowed identifying individual components, including potassium aluminium silicate-based pearlescent pigments, vegetable carbon, rutile titanium dioxide, iron oxide and aluminium containing (nano)particles by their elemental composition. Their presence and relative concentration varied among the different spray colours. Often the layer of titanium dioxide particles detached from the mica substrate, and titanium dioxide particles were also observed forming nearspherical aggregates. STEM-EDX tomography allowed identifying particles of overlapping components and examining the structure of the pearlescent pigments in 3D. The presence of a fraction of nanoparticles in each component was demonstrated based on their number-based particle size distributions. The methods and findings support regulatory bodies in assessing potential health risks of mixtures of (nano)particles used in food-related applications.

F. Hernandez, M. Magre, S. Mateus, C. Bourrel, M. Dubernet
Determination of metals content in wine samples by direct ICP-MS analysis

Metal content of wine varies from ng/L to mg/L depending on the element. They should be determined and controlled in wines . Indeed, on one hand some of them are of toxicological concern as Lead, Cadmium and Arsenic which are regulated by OIV and by European regulation (CE 1881/2006) ; on the other hand some others can present technological risks as Iron and Copper that may cause precipitations in wines. A new method for metal content in wines was developed by ICP-MS after on-line dilution of the samples. The method was then validated according to the accuracy profile approach. The aim of this study is to characterize the content of Lithium, Sodium, Magnesium, potassium, Calcium, Titanium, Chromium, Manganese, Iron, Cobalt, Nickel, Copper, Zinc, Arsenic, Selenium, Strontium, Molybdenum, Silver, Cadmium, Tin, Antimony, Baryum, Mercury and Lead in a sampling of wines from South of France.

D. Ghaffour, V. Sirot, M. Champion, A. Leufroy, P. Jitaru
Development & validation of a novel method for Hg speciation analysis in food by HPLCICP-MS and application to the 3rd (French) Total Diet Study

A simple, fast and a robust method for routine speciation analysis of inorganic (Hg2+) and methylmercury (MeHg) by reverse phase (RP) high-performance liquid chromatography coupled to inductively coupled plasma mass spectrometry (HPLC-ICP-MS) was optimized and validated. This novel method is to be applied for the analysis of a large panel of foodstuffs samples within the framework of the 3rd (French) total Diet Study (3rd TDS). TDSs are endorsed by the World Health Organisation (WHO) and Food and Agriculture Organization of the United Nations (FAO) and they are one of the most efficient tools for national assessment of chemical contamination of food prepared as consumed. This allows estimating human dietary exposure after matching contamination data (occurrence) with the consumption patterns based on samples representativeness. TDSs provide valuable scientific information to national authorities in order to address the risk for the general population in terms of food chemical hazards and permitting to protect the public health on a long-term basis. An effective separation of Hg2+ and MeHg species was achieved in less than 7 min using a peptide mapping RP column. The development was carried out using an experimental design for the HPLC separation and the sample extraction. In the latter case, two extraction approaches, employing a closed microwave system and the use of a heating block, respectively, were compared. The method was validated based on the accuracy profile approach according to the NF V03-110 French standard, which takes into account the simultaneous assessment of the accuracy and precision of the method. The accuracy profile is an expression of the combination of the systematic (trueness) and the random error (repeatability and/or intermediate precision) for a series of analyst's levels in various matrices in range of concentrations called validity domain. For this purpose, five measurement series were repeated in duplicate on (5) different days, over a timespan of two months for constructing the accuracy profile. The method was applied to the speciation analysis of MeHg and Hg2+ in a variety of foodstuffs of the 3rd(French) Total Diet Study

G. Barzan, M. Putzu, R. Avolio, G. Berti, S. Squadrone, L. Pinotti, A. M. Giovannozzi, A. M. Rossi, D. Marchis
Evaluation of packaging contamination in animal feed containing former food

Considering the actual population increase and the compelling need of food waste reduction and nutritional resources saving, former food products (FFPs), not more suitable for human consumption, can be recovered and reused in animal feed as sustainable alternative to cereals. However, some packaging residues (paper, aluminum, plastics etc.) may remain in the final product due to mechanical unpackaging and grinding processes and needed to be quantified and characterized to optimize the use of FFPs and reduce the risks involved. In this work, 14 feeds containing FFPs were taken as part of the official control of packaging residues according to the Italian National Feed Plan. Firstly, a quantitative method for the determination of six phthalates (DBP, DEP, BzBP, DMP, DEHP, DnOP) by gas chromatography (GC-TQ-MS/MS) was developed and validated. Three samples containing detectable concentration of phthalates were selected and the packaging contaminants, isolated by subsequent sieving [1] (mesh from 2 to 0.7 mm), were chemically characterized by vibrational spectroscopy (µFTIR and µRaman) to identify possible plastic residues [2]. This non-destructive technique, allowing to rapidly obtain the analyte specific chemical fingerprint, even with very small amount, and avoiding any difficult preparation step, represents the excellence choice for polymers identification [3]. DEHP was detected in 5 samples (0.210 to 0.898 mg/kg), in two of which it was associated to DMP (0.081 mg/kg) and BzBP (0.113 mg/kg). The three most contaminated samples contained up to 0.08% (w/w) of total packaging residues. Vibrational spectroscopy analysis also evidenced the presence of plastic polymers such as PE. A library of the most common plastic polymers (PE, PP, PET etc.) was obtained measuring standards by both µFTIR and µRaman. Further vibrational spectroscopy analysis of these samples, after digesting the organic matrix, are also intended to identify the possible presence of microplastics < 1 µm. Since the presence of phthalates and microplastics that can accumulate in the tissues of animals intended for human consumption represents a severe issue due to their xenogeneic activity, measuring and quantifying their occurrence in feed results fundamental for a risk-based approach.

R. Chekri, M. Saraiva, S. Millour, T. Guérin, L. Noel, J. Sloth, P. Jitaru
Impact of cooking on the fate of elements and species in food: implementation of different analytical approaches

Trace elements can occur in food because of their presence in the environment, due to human activities or contamination during storage and food processing, including cooking.
There are various ways of cooking (boiling, grilling, frying, etc.) and each of them can affect differently the elements' content. This may lead to a decrease or an increase in element concentration, or even to a transformation of the species. Therefore, to better assess people's exposure to these contaminants and avoid or reduce harmful human effects, it is important to know the fate of the elements and their species in food during cooking.
For this work, we conducted various studies and implemented different approaches to evaluate the impact of cooking on (i) arsenic (As), lead (Pb) and cadmium (Cd) in whelks (ii), total arsenic and inorganic arsenic (iAs) in rice and (iii) total chromium (Cr), Cr(III) and Cr(VI) in milk and meat. For the total elements' determination, analyses were carried out by inductively coupled plasma-mass spectrometry (ICP-MS). For the speciation analyses, high performance liquid chromatography (HPLC) coupled to ICP-MS alone or in combination with species-specific isotope dilution (ID) was implemented. This latter technique allows also to assess possible interconversions of Cr species due to foodstuffs cooking. Results obtained show that boiling was the cooking method with the highest impact on the elements' content, especially for As and iAs with a significant concentration decrease in cooked samples (rice and whelks). On the other hand, the culinary treatments employed for meat and milk samples (heating and frying) did not induce significant differences on total Cr and Cr species levels between raw and cooked samples. Thanks to the IDICP-MS approach used, we demonstrated that a total reduction of Cr(VI) to Cr(III) occurred in the samples but that this was due to the sample preparation (extraction) and not to the cooking process.

T. Carsi Kuhangana, K. Cheyns, C. Banza Lubaba Nkulu, E. Smolders, P. Hoet, J. Van Loco, H. Demaegdt, B. Nemery
Unprecedentedly migration of lead and other metals from artisanal cookware to simulants and foods

Wold wide, studies have been carried out on the contact of food with stainless steel kitchen utensils and most of them showed a releasing of several metals in "similants" or in a representative food. Kitchen utensils, as unrecognized exposure sources, can cause significant public health risks throughout the developing world. The objective of this study was to investigate the releasing of metals in similants and in some representative foods from artisanal cookwares. We conducted an experimental study on 9 samples of cookware collected in six cookware manufacturing workshops located in Lubumbashi city. three samples of cookwares for each type of samples (Artificial tape water, citric acid and food cooked in the local context) were used for migration test, one cookware of food was excluded because of unsaficiant data. The preparation and the migration test of smilants were done according to the pratical guide for manufacturers and regulators published by the European Directorate for the Quality of Medicines & HealthCare of the Council of Europe (1st Edition) and the Practical Guidelines for Performing FCM Metal/Alloy, Ceramic and Plastic Migration Testing for Metal Migration and Reporting of Results of Sciensano [SRL(µg/kg): Al(5000), V(10), Cr(250), Ni(140), Zn(5000), Tl(0.1) et le Pb(10)]. Two normes of Specific Release Limit (SRL) ((3rd MT > SLR and 1st + 2nd MT > 7.SLR); MT: concentration of migration test) were considered. We also collected randomly on the workspace of 4 workshops 4 samples of alloys,obtained after cookware polishing, and one maleable metal used to plug cookware's holes, for chemical comosition analysis. Metal determination was performed using Inductively Coupled Plasma Mass Spectrometry (ICP-MS). The alloys collected showed concentration mean (g/kg) of Mg(3.5), Al(521.9), V(0.34), Cr(0.16), Mn(1.3), Fe(12.8), Co(0.02), Ni(0.5), Cu(11.1), Zn(4.2), As(4.10-6), Cd(15.10-4) and Pb(0.5), and the one sample of maleable metal showed (g/kg) Mg(0.752), Fe(0.624), Co(0.002), Ni(0.091), Cu(2.201), As(13.10-3), Cd(523.10-4), Tl (816.10-4) and Pb(1015.8). In regard to experience of migrations, for each type of similiant and food sample used for the eight cookwares, only seven elements (Al, V, Cr, Ni, Zn, Tl and Pb) showed concentrations above the standards. For citric acid, the aluminum concentrations obtained after the migration tests were above the required safe standards (3rd MT > SLR and 1st + 2nd MT > 7.SLR), whereas for ATW, one of the two standards were not met (3rd MT > SLR) . The vanadium concentrations in the AC samples collected after testing met only one standard (3rd MT > SLR), whereas for the ATW, the migration standards were met. With regard to lead, two cookwares out of the three collected showed concentrations higher than the two standards (3rd MT > SLR and 1st + 2nd MT > 7.SLR) and the other one did not met one of the standards (1st + 2nd MT > 7. SLR). For the migrations in the ATW, only one cookware showed concentrations above a standard (3rd MT > SLR). Concerning beans, the migrations were beyond the norms for Pb only (3rd MT > SLR and 1st + 2nd MT > 7.SLR), as for sorrel, Al, V, Cr, Ni, Zn, Tl and Pb migrated beyond the standards (3rd MT > SLR and 1st + 2nd MT > 7.SLR). These findings support that consumers using atisanal cookwares in developing countires are exposed to metals, especialy to lead and warns on the use of pure lead in the manufacture process of some cookwares. Studies on the types of row materials used for cookware manufacture are needed to identfy the factors influencing the composition of cookware, consequently the relesing of metals in food.

Y. Devriendt-Renault, F. Massat, T. Guérin, J. Parinet
Impact of food cooking on chlordecone contents in animal matrices identification of elimination mechanisms

Chlordecone (CLD) was an organochlorine pesticide frequently used in the French West Indies between 1972 and 1993 to control the banana weevil (Cosmopolites sordidus). The CLD has impregnated the whole ecosystem at all trophic levels, and contaminated the local population through the consumption of locally produced food, raising a major issue of sanitary safety and public health. Self-production is a major route of CLD exposure. These foodstuffs, of vegetal or animal origin, may be consumed by the producer or offered for sale at the roadside and can far exceed the current CLD maximum residue limit of 20 µg.kg-1. Consumption recommendations of these matrices have been proposed to local populations to limit the ingestion of CLD.A method of analysis of CLD and chlordecol (CLDOH), using QuEChERS extraction salts and tandem mass spectrometry (LC-MS/MS) in MRM mode with isotopic dilution, was developed and used to assess the effects of cooking (Saint-Hilaire et al., 2018; Martin et al., 2020). The aim of this study is to analyze a wide variety of animal matrices (i.e. fish, lobster, crayfish, chicken, egg and pork) and identify the CLD elimination mechanisms occurring during a cooking process. These new matrices were pan-fried, oven-fried and microwaved, with adapted cooking conditions. CLD levels were measured before and after cooking for each matrix, and processing factors (PF) representing the proportion of CLD remaining in a matrix were calculated for each pair of matrix/cooking conditions (Devriendt-Renault et al., 2023). CLD Transformation hypothesis was investigated using high-resolution mass spectrometry coupled with liquid chromatography (LC-HRMS) for the search of chlorinated by-products, possibly generated during the cooking process.

L. Ruggiero, R. Ofano, D. Agrelli, C. Amalfitano, P. Adamo
Multielement fingerprinting of soils and agriproducts as tracer of food geographical provenience: the case of Vesuvian Piennolo Tomato PDO

Multielement fingerprinting is one of the most widely used technique to discriminate the geographical origin of food. It takes advantage of the fact that mineral elements can be transferred from soil to agricultural products and thus any difference in element distribution between different geographic regions are reflected in agriproducts. The Vesuvian Piennolo Tomato (VPT) is a traditional variety, grown in the Campania (Italy) on the SommaVesuvius volcano slopes, sold assembled in bunches and characterized by long shelf-life. VPT was awarded by Protect Designation Origin (PDO) in 2009. Local "custodian farmers" play an important role in conserving traditional cultivation management and biodiversity, as well as organoleptic properties deriving from Vesuvian environment. Due to the high typicity and higher selling value, VPT is susceptible to origin fraud. Thus, main aim of our study is to valorise VPT strengthening the traceability system. A way to achieve this is to link the tomato to the soil characteristics by multielement fingerprinting. In this work, the multielement profiles of VPT (three ecotypes) from five PDO and two not PDO farms were investigated in two production years. In addition, the multielement profile of cultivation soils (total and bioavailable elements) was investigated to evidence the variability of the PDO or not PDO soils and relationships with related tomatoes. The exploratory PCA analysis of multielement profiles evidenced a tendency to a natural grouping of tomato and soil according to provenance farms. By contrast any tendency to a natural grouping of tomatoes according to ecotypes was observed. S-LDA model applied on tomato multielement profiles grouped by farms gave 100% of correct classification and external validation, demonstrating a great discriminating power of multielement fingerprinting. The good correlation between elements in soil and tomatoes reinforced the reliability of the discriminant variables. Work carried out in the framework of METROFOOD-IT (NextGenerationEU, PNRR - M4C2, Investment 3.1: Fund for the realisation of an integrated system of research and innovation infrastructures - IR0000033 (D.M. Prot. n.120 del 21/06/2022) and Tomato Trace 4.0 (Campania Region Rural Development Programme) projects.

Y. Pieracci, I. Korbi, N. Omri, F. Seby, O. F. X. Donard, V. Vacchina
Potential of a new multi-isotopic dilution method for geographical origin discrimination: application to wine

Wine traceability has become of primary important for consumers as well as for producers. One of the most powerful tools to link wines to their geographical origin is the use of isotopic ratios of three non-traditional elements (Sr, Pb and B) mainly thanks to its very high precision. However, this approach is long and expensive which makes it difficult to use on a daily basis. In this study, a mix of 22 major and trace elements measurable by ICP-MS and proved to be relevant for geographical discrimination purpose have been selected to replace this triple isotopic system. A new method has been developed to measure simultaneously these 22 elements. It involves: (1) a quantification by isotopic dilution whenever possible to improve the precision of the measurements (one of the key factors achieve a good discrimination) and (2) the use of a triple quadrupole ICP-MS to eliminate the potential interferences and allow the analysis of the 22 elements all at once to save time. The potential of this new method comes from the range of elements precisely measured that allow the selection of the relevant ones depending on the application aimed. The presentation will introduce the development of this new method, its analytical performances, and its application to discriminate the geographical origin of wines. In particular, the potential of the method will be illustrated at different scales: from the country level to almost the farm level.

A. Ochem, L. Delaire, C. Marc, C. Dutfoy, A. Diby
Analytical strategy for food authenticity and characterization of food frauds

The Joint Laboratories Service is a governmental agency working mainly for the French Customs and the French Fraud Repression administrations. It is constituted of 11 labs, in France mainland and overseas, of different sizes and specialities working together in network. Among this network, the laboratory of Paris is particularly in charge of analysis of various food products to detect some frauds. Those frauds may have for consequences some economic losses for the French administration as well as some consequences on the health safety of population. The purpose of the lecture will be to present our analytical strategy in front of a potential fraud involving food products such as fruits, vegetables, eggs and so on. In particular, different examples of recent caseworks and the analytical ways to face them will be developped. The first one will be the use of etephon on pineapples or bananas to mature them quicker. The second one will deal with the use of additives in egg white in the industry. And finally, an illustration of how analytical chemistry allows us to show that the mention « grow in France » may be abusivelly used. The main analytical techniques presented will be LC-QToF, LC-MS-MS and viscosimetry.

Page 37 of 977 Results 361 - 370 of 9762