BACKGROUND:Pyrrolizidine alkaloids (PAs) are natural toxins produced by >6000 flowering plant species. Some PAs are hepatotoxic and genotoxic carcinogens. Reported cases of direct poisoning in humans have already been documented, but the highest risk of human exposure occurs through the consumption of crops contaminated with PA-producing weeds. The European Commission Regulation EU 2023/915 set maximum levels (MLs) for the sum of 35 PAs in tea, herbal teas, herbs, and spice seeds at levels ranging from 75 to 1000 µg/kg (dry matter basis). OBJECTIVE:The study describes the performance characteristics of a quantitative liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination of the 35 PAs mentioned in AOAC INTERNATIONAL Standard Method Performance Requirement (SMPR®) 2023.002 in tea, herbal infusions, herbs, seed spices, cereals, and honey. The analyte scope also comprised nine additional PAs along with two tropane alkaloids (TAs; namely, atropine and scopolamine) for which MLs are also set in plant-based products in the European Union (EU 2023/915). METHOD:The protocol involves an extraction of toxins from food using aqueous sulfuric acid followed by solid-phase extraction purification. After elution and evaporation to dryness, the residue is reconstituted in a water-methanol solution before LC-MS/MS analysis. Alkaline mobile phases are used to favor the separation of isomers. Identification of the analytes is conducted according to the confirmation criteria defined in EU 2023/2783 and SANTE 11312/2021v2 documents. Quantification is performed by isotopic dilution using four isotopically labeled PAs and two isotopically labeled TAs as internal standards. RESULTS:Method validation workload was shared by three different laboratories on representative matrixes from the following commodities: dried herbs, dried tea, dried herbal infusions, seed spices, cereals, and honey. The 35 target analytes specifically listed in the AOAC SMPR 2023.002 have been successfully validated (recovery 70-120%, repeatability <20%, intermediate reproducibility <20%), allowing LOQs down to 1 µg/kg. CONCLUSIONS:The performances of the method are in agreement with criteria defined in AOAC SMPR 2023.002. HIGHLIGHTS:The Expert Review Panel for Pyrrolizidine Alkaloids approved the present method as AOAC Official First Action 2025.02.

BACKGROUND:Per- and Polyfluoroalkyl Substances (PFAS) are synthetic compounds widely used due to their water, grease, and dirt repellent properties. They are persistent and resistant to degradation, therefore they can be found in the environment, the food chain, and in human fluids. The European Union (EU) has established limits of quantification (LOQs) for four PFAS in produce, seafood, meat, eggs, fish oil, milk, and ready-to-eat food for infants and young children and set maximum levels (MLs) for the same analytes in eggs, fish, and meat products. OBJECTIVE:The study describes a quantitative LC-MS/MS method for the determination of 57 PFAS in food. The 55 analytes are quantified by isotopic dilution while two of the compounds, namely Capstone A and Capstone B are quantified using 2-level standard addition. Seven of the compounds have only one transition, which need another technique for their confirmation in case of a positive result in a sample. The scope comprises analytes included in the AOAC INTERNATIONAL Standard Method Performance Requirements (SMPRs®) 2023.003, cited in the EU Recommendation 2022/1431, and analytes surveyed by service laboratories in Europe or mentioned in the literature.Representative samples from several food categories (baby food puree, milk-based infant formula (powder), full cream milk powder, fish meat and fish oil, whole egg, soluble coffee, pet food and edible offal) were validated. Targeted performance requirements for LOQ, recovery and precision were as defined per AOAC SMPR 2023.003. METHOD:The protocol involves an acetonitrile/water extraction. For 55 PFAS analysis in all matrices, a solid phase extraction (SPE) method is applied. Detection is conducted by LC-MS/MS and isotopic dilution is applied for quantification. Confirmation for single-transition analysis is performed by LC-HRMS. For infant formula and baby food, the extract is diverted to two workflows, one for the 55 PFAS and one for Capstone A & Capstone B, where a diluted aliquot is analyzed by LC-MS/MS and quantified by the standard addition procedure. RESULTS:The method was single laboratory validated in the nine food matrices with results generally in agreement with the criteria of the AOAC SMPR 2023.003, in terms of LOQs, recovery and precision. LOQs were generally in the low ng/kg range, and recoveries typically fell within 70-120%, with acceptable repeatability and intermediate precision. The performance of the method was further demonstrated by analyzing 27 additional food matrices. CONCLUSIONS:The method described covers a wide range of food matrices and analytes compares favorably with most of the requirements of the SMPR 2023.003, it contains as well a larger scope of analytes compared to the SMPR 2023.003, giving an advantage of searching other potential sources of PFAS contamination. Following independent scientific review, the AOAC Expert Review Panel for PFAS in Food Methods determined that the method met the requirements of AOAC SMPR 2023.003 and approved it for First Action status as AOAC Official Method 2025.10. HIGHLIGHTS:This work presents a validated LC-MS/MS method for 57 PFAS across diverse food matrices, meeting or exceeding most of the AOAC SMPR 2023.003 performance requirements and demonstrating broad applicability for routine monitoring. The method includes additional PFAS of emerging interest and was approved for AOAC First Action status, designated AOAC Official Method 2025.10.

Background: The presence of veterinary drug residues in food-producing animals and animal products is regulated through the enforcement of maximum residue limits (MRLs). To answer the need of the food sector to monitor these substances in a wide range of food commodities, stakeholders at AOAC INTERNATIONAL identified the need for a reliable confirmatory screening method. Such a qualitative approach is required for compliance checking and to support product release in manufacturing. Objective: Data were collected from five independent laboratories that applied the First Action Official Method 2020.04 to demonstrate adequate performance under reproducibility conditions. The probability of detection (POD) was calculated in blank test samples and test samples spiked at the screening target concentration (STC) level, with the objective to achieve PODs <= 10% and >= 90%, respectively. Additionally, the effectiveness of the screening method was evaluated by participating in 92 proficiency tests. Methods: Four streams were optimized to screen for 152 veterinary drug residues by LC-MS/MS in a wide variety of food commodities including milk-based ingredients and related products (e.g., milk fractions, infant formula, infant cereals, and baby foods), meat- and fish-based ingredients and related products (fresh, powdered, cooked, infant cereals, and baby foods), and other ingredients based on eggs, animal fat, and animal byproducts. The four streams covered 105 antibiotic residues, anti-inflammatory and antiparasitic agents (stream A), 23 beta-lactams (stream B), 14 aminoglycosides (stream C), and 10 tetracyclines (Stream D). Results: The multilaboratory validation led to PODs at the STC >= 94% and PODs in the blank <= 9%. Further application of the multilaboratory validated method to 92 proficiency tests provided more than 99% satisfactory submitted results (n = 784). Conclusion: The interlaboratory reproducibility determined for this method met the acceptance criteria defined in AOAC Standard Method Performance Requirement (SMPR) 2018.010.

BACKGROUND:Chlorate is an effective herbicide, but also a byproduct of chlorinating agents used to disinfect water, which is one of the reasons why it is regularly found in food. Perchlorate is a ubiquitous contaminant, which is naturally occurring in the environment but also released from anthropogenic sources such as the industrial use of certain natural fertilizers. Chlorate affects the hematological system, and perchlorate the thyroid.OBJECTIVE:Implement and validate a simple and robust analytical method for the accurate determination of chlorate and perchlorate in baby food, infant and adult formulas, and ingredients thereof, which is suited for its application in routine environments where a broad variety of food commodities must be analyzed simultaneously.METHOD:Typically, analytes are extracted with a mixture of water, acidified methanol, and dichloromethane. Optionally, for dairy products and byproducts, extraction can be performed with water, acidified methanol, and EDTA, followed by two steps of cleanup (freezing out and dispersive solid-phase extraction with C18 in acetonitrile). Quantitative determination is carried out by isotopic dilution liquid chromatography tandem mass spectrometry (LC-MS/MS).RESULTS:The method was single-laboratory validated in five Nestlé Quality Assurance Centers (NQACs) in a comprehensive range of representative matrixes of different categories such as baby foods, infant/adult formulas, and ingredients, with results generally in agreement with the acceptance criteria of the Standard Method Performance Requirement (SMPR®) 2021.001 defined by AOAC INTERNATIONAL, in terms of representative matrixes validated, LOQs, trueness, and precision.The data generated during validation show that the method proposed is simple, accurate and robust enough to be implemented and applied in routine environments.CONCLUSION:The data generated during validation show that the method proposed is simple, accurate and robust enough to be implemented and applied in routine environments.HIGHLIGHTS:The AOAC Expert Review Panel approved the present method as AOAC Official First Action 2022.06.

To enable the monitoring of a wide scope of per- and polyfluoroalkyl substances (PFAS) in the ng/kg level in foodstuffs, an LC-MS/MS method comprising 57 analytes was developed and validated in seven different matrices (milk powder, milk-based infant formula, meat-based baby food puree, fish and fish oil, fresh egg, and soluble coffee). The analytical approach was based on an acetonitrile:water extraction followed by solid phase extraction clean-up with subsequent quantification of the extracted analytes either by isotope dilution (55 compounds) or by standard addition (2 compounds) mass spectrometry. The validation criteria followed the guidance document for the analysis of PFAS issued by the European Union Reference Laboratory for Halogenated Persistent Organic Pollutants. The lowest limits of quantification (LOQs) for the four recently regulated compounds (L-PFOS, PFOA, PFNA, L-PFHxS) were set at 0.010 µg/kg in baby and infant foods (as sold) but also in dairy ingredients. Exception was for PFOA in milk powder due to too large variability in the repeatability. Applicability of the method was further demonstrated in 37 commodity check matrices. Overall validation data demonstrated the robustness of the method for most of the compounds and the LOQs achieved were low enough to ensure compliance with Commission Regulation EU 2022/2388 but also to support future collection of occurrence data in ng/kg level in food.

Liquid chromatography-tandem mass spectrometry (LC-MS/MS) is a widespread technology used for the quantitative determination of per- and polyfluoroalkyl substances (PFAS) in foodstuff. Specifically, LC-MS/MS offers an attractive performance by combining the sensitivity and selectivity required by the European Union for testing perfluorooctane sulfonic acid, perfluorooctanoic acid, perfluorononanoic acid, and perfluorohexane sulfonic acid with maximum limits of quantification (LOQ) in the sub-parts-per-billion (μg/kg) or the parts-per-trillion (ng/kg) domains. In this article, we highlight the important diversity in LOQ definitions applied in LC-MS/MS methods described in the literature that raise concerns about the capability of some of those to generate reliable data requested by the European regulation. Here, we point out the risk of false response or misquantification if the criteria for assessing LOQ suffer from a lack of rigor. We emphasize the need to use PFAS-free samples spiked with the analyte(s) of interest and the application of identification criteria according to official documents for a sound measurement of the LOQ.

This study describes the extension of a gas chromatography mass spectrometry (GC-MS) method, initially devoted to the analysis of ethylene oxide (EO) in ice cream, to a larger range of food items including herbs, spices, vegetables, inorganic salts, food supplements, thickeners, etc. Results are reported as EOTotal according to EC 2015/868 definition (expressed as EO equivalents as the sum of native EO and 2-chloroethanol (2-CE) after acidic hydrolysis) with a limit of quantification at 0.01 mg/kg regardless of the food item. Its ruggedness was demonstrated through fortification experiments on hundreds of samples. Re-analysis of 146 positive food samples without hydrolysis demonstrated that not EO but 2-CE is the predominant analyte detected in the different processed ingredients suspected to have been previously treated with EO. A series of eight contaminated dried herbs and spices were also re-analysed by four ISO 17025 accredited commercial laboratories making use of different analytical strategies for EO determination in foods. Each laboratory reported EOTotal levels within the same concentration range, but the resulting reproducibility ranged from 23% to 41% depending on the sample. Additionally, we show that results of free EO from methods based on conversion to 2-iodoethanol may lead to artefactual detection of native EO (false positive). An official method of analysis applicable for different food matrices would be useful to avoid discrepancies of results. Altogether, these data re-enforce the fact that in absence of native EO in food items, risk assessment of EO in foodstuffs should consider the predominance of 2-CE. A toxicological risk assessment using the food additive xanthan gum as a case study is discussed.

ADVERTISEMENT RETURN TO ISSUEViewpointNEXTDetermination of Poly- and Perfluoroalkylated Substances in Food: How Consistent Are Results across Laboratories?Thierry Delatour*Thierry DelatourSociété des Produits Nestlé S.A., Nestlé Research, Vers-chez-les-Blanc, CH-1000 Lausanne 26, Switzerland*E-mail: [email protected]More by Thierry Delatourhttps://orcid.org/0000-0003-1540-9645, Xanthippe TheurillatXanthippe TheurillatSociété des Produits Nestlé S.A., Nestlé Research, Vers-chez-les-Blanc, CH-1000 Lausanne 26, SwitzerlandMore by Xanthippe Theurillat, Claudia MujahidClaudia MujahidSociété des Produits Nestlé S.A., Nestlé Research, Vers-chez-les-Blanc, CH-1000 Lausanne 26, SwitzerlandMore by Claudia Mujahid, Bjo̷rn EriksenBjo̷rn EriksenSociété des Produits Nestlé S.A., Nestlé Research, Vers-chez-les-Blanc, CH-1000 Lausanne 26, SwitzerlandMore by Bjo̷rn Eriksen, and Pascal MottierPascal MottierSociété des Produits Nestlé S.A., Nestlé Research, Vers-chez-les-Blanc, CH-1000 Lausanne 26, SwitzerlandMore by Pascal MottierCite this: J. Agric. Food Chem. 2023, 71, 12, 4767–4768Publication Date (Web):March 14, 2023Publication History Received2 March 2023Published online14 March 2023Published inissue 29 March 2023https://pubs.acs.org/doi/10.1021/acs.jafc.3c01306https://doi.org/10.1021/acs.jafc.3c01306article-commentaryACS PublicationsCopyright © 2023 American Chemical Society. This publication is available under these Terms of Use. Request reuse permissions This publication is free to access through this site. Learn MoreArticle Views1314Altmetric-Citations-LEARN ABOUT THESE METRICSArticle Views are the COUNTER-compliant sum of full text article downloads since November 2008 (both PDF and HTML) across all institutions and individuals. These metrics are regularly updated to reflect usage leading up to the last few days.Citations are the number of other articles citing this article, calculated by Crossref and updated daily. Find more information about Crossref citation counts.The Altmetric Attention Score is a quantitative measure of the attention that a research article has received online. Clicking on the donut icon will load a page at altmetric.com with additional details about the score and the social media presence for the given article. Find more information on the Altmetric Attention Score and how the score is calculated. Share Add toView InAdd Full Text with ReferenceAdd Description ExportRISCitationCitation and abstractCitation and referencesMore Options Share onFacebookTwitterWechatLinked InRedditEmail PDF (2 MB) Get e-AlertscloseSUBJECTS:Animal derived food,Composites,Food,Testing and assessment,Toxins Get e-Alerts

Liquid chromatography-high resolution mass spectrometry (LC-HRMS) is considered an unavoidable extension of low-resolution LC-MS/MS that stretches the capabilities of multi-residue analysis of chemical contaminants in food. However, LC-HRMS acquisitions generate a massive amount of information available for data processing with supplier software that still miss critical calculation features and adapted reporting tools. Consequently, routine laboratories are still reluctant to switch from LC-MS/MS to LC-HRMS, the latter is still perceived as a cumbersome and demanding technology. In that context, we propose a four-step LC-HRMS workflow to speed-up data processing in situations of multi-residue multi-matrix analysis with the goal to maximize the time spent on data interpretation rather than on data formatting. The first three steps of the workflow imply specific settings on the Orbitrap HRMS associated software (TraceFinderTM) while the fourth step is the novelty i.e. a newly coded R-script capable to translate a raw export file into a comprehensive .xlsx report file in a few seconds. As recommended by various international guidelines and in some official methods, standard addition-based applications are fully embedded in this reporting tool whilst still being the main bottleneck of supplier's software. The reporting tool also allows appropriate data formatting, filtering, and color-coding options to provide a clear picture of compounds being detected or not, and those requiring specific attention due to unmet quality control criteria as required by European legislation (European Commission SANTE 11312/2021). It is hoped that additional functionalities compatible with R scripts will be soon fully embedded in the supplier's software for easier data interpretation and reporting.

In this study an analytical procedure, based on a modification of the so-called QuPPe-method (quick method for the analysis of numerous highly polar pesticides in food), has been evaluated for routine monitoring of chlorate and perchlorate in a broad range of food matrices. Analytes were extracted with a mixture of water, acidified methanol and dichloromethane, followed by liquid chromatography tandem mass spectrometry (LC-MS/MS) determination. For LC separation HILIC stationary phase provided best results in terms of robustness and column durability. Quantification was performed by isotopic dilution, using the respective 18O isotopically labelled analogues as internal standards. The method was validated in four Nestle Quality Assurance Centres (NQACs) according to the current EU guidelines for pesticides method validation (SANTE/12682/2019). Trueness of the method ranged from 91.3 to 110.1 %, and intermediate precision was lower than 20 %, except for slight deviations observed in two matrices. Limits of quantification (LOQs) of the method were 0.010 mg/kg for chlorate and perchlorate in all matrices, except for perchlorate in food intended for infants for which the LOQ was 0.002 mg/kg, thus equal or below the maximum residue levels (MRLs) specified on the current EU regulations and recommendations. Therefore, the method fits for monitoring in high routine environments at those decision levels.

This study investigated the feasibility to monitor ca. 400 veterinary drug residues in various foodstuffs by a single method. For this, a generic QuEChERS-based approach was applied for sample preparation while liquid chromatography-high resolution mass spectrometry (LC-HRMS) was considered as detection technique. The LC-HRMS based method was eventually found suitable to screen for 353 parent compounds and marker residues in raw materials of animal sources (dairy-, meat-, fish-, egg-, and animal by-products), but also in related processed ingredients and end commercialized items. The screening approach was fully validated according to the Euro-pean Guidelines in 70 samples, ending with false positive-and false negative rates below 5 %. Simultaneously, quantitative method performances were found acceptable in terms of recovery (70-120 % range) and precision (<20 %) for 184 out of the 353 compounds. A set of 114 samples originating from Europe, Asia, USA, Brazil, New Zealand and Australia, were subsequently analyzed to collect occurrence and quantitative data. The survey highlighted a high incidence of Antiparasitics (Benzimidazoles in eggs and Coccidiostats in poultry samples), though only one poultry sample for monensin (22 mu g kg(-1)) exceeded the Maximum Residue Level set at 10 mu g kg(-1) by the European Union. The presented LC-HRMS approach was complemented with a dedicated LC-MS/MS method to improve quantitative measurements of such recurringly found Coccidiostats but also to achieve enhanced sensitivity for Macrocylic lactones.

Residues of ethylene oxide (EO), a banned fumigant in the EU, were found at amounts above the maximum residue limit (MRL) in carob (locust) bean gum (additive E410). The pesticide entered the food chain via stabiliser blends that are used as minor ingredients in the manufacture of ice cream. Consequently, all products that contained the non-compliant ingredient were withdrawn or recalled in several countries across the EU, in most cases irrespective of whether the pesticide residue was detectable or not in the final product. This is the first report of a reliable method to determine EO and its metabolite/marker compound 2-chloroethanol (2-CE), either together or independently in ice cream, with a limit of quantification at 0.01 mg EO/kg and recovery in the range of 87-104% across the levels investigated (0.01, 0.02 and 0.06 mg EO/kg). The method applies QuEChERS extraction and isotope dilution gas chromatography coupled with tandem mass spectrometry (GC-MS/MS). High resolution mass spectrometry (HRMS) confirmed the specificity of low mass ions. Data on the stability of EO and 2-CE under thermal conditions revealed that 2-CE is relatively stable in an ice cream matrix (ca. 80% recovery of spiked material). Importantly, this study also demonstrates that not EO, but 2-CE is the predominant analyte detected in the contaminated samples, which is new information of significance in terms of the overall risk assessment of EO in foodstuffs.

Background: Veterinary drug residues in food are substances (>200 compounds) exhibiting potential health risks for consumers, thus being regulated in national legislations and the Codex Alimentarius. Most of the compounds are regulated based upon a maximum residue limit (MRL) while a few of them are banned in food for humans. The food sector needs a reliable and consensus analytical platform able to monitor these substances in a wide range of food commodities. Objective: Several confirmatory methods based on liquid chromatography-mass spectrometry are available in the literature for either screening or quantification of veterinary drug residues in food, but usually applicable to limited scope of matrices. The current work describes the single-laboratory validation (SLV) of a method for screening 154 veterinary drug residues in several food categories. Methods: This work describes a streamlined platform making use of liquid chromatography-tandem mass spectrometry (LC-MS/MS) for screening 105 antibiotics, 41 antiparasitics, 5anti-inflammatory agents, and 3 tranquilizers in foods of animal origin. For the best performance across the commodities (dairy-, meat-, fish-, and egg-based materials), four method streams were established. As a screening tool, probabilities of detection (PODs) were assessed at the screening target concentration (STC < MRL) and the blank. Results: The SLV led to PODs at the STC >94% and PODs in the blank < 4%. Conclusion: Performance is in agreement with the acceptance criteria defined in SMPR 2018.010. Highlights: The Expert Review Panel approved the present method as AOAC Official First Action2020.04.

In this study, the occurrence of cannabinoids in hemp-based food products was investigated. For that purpose, a new liquid chromatography tandem mass spectrometry method for the quantification of fifteen cannabinoids was developed and validated for multiple matrices. Method performances were good, fulfilling the SANTE/11813/2017 requirements, and allowing for products compliance testing with various national legislations on cannabinoids levels in food products. The limit of quantification of each analyte was 0.15 mg/kg for hemp seed and hemp protein, 0.6 mg/kg for hemp seed oil, and 0.005 mg/kg for raw milk and milk powder. The applicability of the method was further demonstrated by conducting a limited survey on twenty hemp-based food products. The survey revealed that products from the same category can have very different cannabinoids profiles and levels. These results highlighted the importance of cannabinoids testing of food products in view of the current heterogeneous and fast evolving regulatory landscape worldwide.

Alternaria toxins are emerging mycotoxins, candidates for regulation by European Authorities. Therefore, highly sensitive, confirmatory, and reliable analytical methodologies are required for their monitoring in food. In that context, an isotope dilution LC-MS/MS method was developed for the analysis of five Alternaria toxins (Altenuene, Alternariol, Alternariol monomethylether, Tentoxin, and Tenuazonic Acid) in a broad range of commodities including cereals and cereal-based products, tomato-based products, tree nuts, vegetable oils, dried fruits, cocoa, green coffee, spices, herbs, and tea. Validation data collected in two different laboratories demonstrated the robustness of the method. Underestimation of Tenuazonic Acid level in dry samples such as cereals was reported when inappropriate extraction solvent mixtures were used as currently done in several published methodologies. An investigation survey performed on 216 food items evidenced large variations of Alternaria toxins levels, in line with data reported in the last EFSA safety assessment. The analysis of 78 green coffee samples collected from 21 producing countries demonstrated that coffee is a negligible source of exposure to Alternaria toxins. Its wide scope of application, adequate sample throughput, and high sensitivity make this method fit for purpose for the regular monitoring of Alternaria toxins in foods.

An intercollaborative study was organized to evaluate the performance characteristics of a liquid chromatography tandem mass spectrometry procedure for the simultaneous determination of 12 mycotoxins in food, which were ochratoxin A, aflatoxins B1, B2, G1, G2, and M1, deoxynivalenol, zearalenone, fumonisins B1 and B2, and T-2 and HT-2 toxins. The method combined the simplicity of the QuEChERS (Quick, Easy, Cheap, Efficient, Rugged and Safe) approach with the efficiency of immunoaffinity column cleanup (the step used to enhance sensitivity and sample cleanup for some matrices only). Twenty-three entities were enrolled and were European reference laboratories for mycotoxin analysis, U.S. and European service laboratories, and Nestlé laboratories. Each participant analyzed 28 incurred and/or spiked blind samples composed of spices, nuts, milk powder, dried fruits, cereals, and baby food using the protocol given. Method performances were assessed according to ISO 5725-2. Relative standard deviations of repeatability and reproducibility and trueness values for each of the 115 mycotoxin/sample combinations ranged from 5% to 23%, 7% to 26%, and 85% to 129%, respectively, in line with requirements defined in EC 401/2006. The overall set of data gathered demonstrated that the method offered a unique platform to ensure compliance with EC 1881/2006 and EC 165/2013 regulations setting maximum limits for mycotoxins in food samples, even at low regulated levels for foods intended for infants and young children. The method was applicable regardless of the food, the regulated mycotoxin, and the concentration level, and thus is an excellent candidate for future standardization.

The unauthorised addition of colours to herbs and spices is a recurrent issue affecting food business operators. Such a practice aims at improving food visual attractiveness, masking poor product quality, and/or compensating for natural colour variation with the ultimate goal to increase profits. To detect this fraud, a new LC-MS/MS method was developed for screening 58 dyes in both herbs and spices. This extended list of targets was established based on requirements from international spices organisations, past issues identified by web scouting and by notifications from the European Rapid Alert System for Food and Feed (RASFF). The method is intended to quickly detect fraudulent addition of dyes with Screening Target Concentrations ranging from 0.1 to 2.5 mg/kg. Validation was performed according to the European Community Reference Laboratories Residues Guidelines 20/1/2010. False positive and false negative rates were below 5% for all analytes and applicability of the method was further demonstrated by analysing 117 samples collected worldwide. None of the surveyed dyes was found in herbs (n = 28, 16 varieties) whereas 6% of spice samples (n = 89, 21 varieties) was found contaminated with one or two dyes at levels ranging from 0.12 to 255 mg/kg. Four out of the nine detected compounds have never been reported in the RASFF, thus demonstrating the usefulness of this analytical approach.

An international pilot study involving five laboratories evaluated the performance of a method intended as a joint ISO/IDF international standard for the analysis of fluid milk and powdered dairy products for intact nitrofurazone down to levels of 1 ng g(-1) . After first establishing that nitrofurazone remains stable to heat treatments in excess of pasteurisation conditions, fluid milk samples that were deliberately spiked with nitrofurazone at low ng g(-1) levels were measured by the laboratories, despite the milk containing no preservatives and, in some cases, being stored at ambient temperature for several months. Commercial whole milk powder and milk protein concentrate, deliberately spiked with low ng g(-1) levels of nitrofurazone, were also analysed by the participating laboratories. For both liquid and powdered dairy samples containing nitrofurazone, laboratories could detect and confirm the presence of nitrofurazone. The within-laboratory repeatability and between-laboratory reproducibility estimates were consistent with the Horwitz ratio. (C) 2019 Elsevier Ltd. All rights reserved.

A procedure for screening 105 veterinary drugs in foods by liquid chromatography tandem mass-spectrometry (LC-MS/MS) is presented. Its scope encompasses raw materials of animal origin (milk, meat, fish, egg and fat) but also related processed ingredients and finished products commonly used and manufactured by food business operators. Due to the complexity of the matrices considered and to efficiently deal with losses during extraction and matrix effects during MS source ionisation, each sample was analysed twice, that is 'unspiked' and 'spiked at the screening target concentration' using a QuEChERS-like extraction. The entire procedure was validated according to the European Community Reference Laboratories Residues Guidelines. False-negative and false-positive rates were below 5% for all veterinary drugs whatever the food matrix. Effectiveness of the procedure was further demonstrated through participation to five proficiency tests and its ruggedness demonstrated in quality control operations by a second laboratory.

Formaldehyde (FA) was analyzed in milk powders by isotope dilution LC-MS/MS using 2,4-dinitrophenylhydrazine (DNPH) as the derivatization agent. Analytical conditions (temperature and time) applied for derivatization were shown to strongly impact the levels of FA detected in micronutrient-fortified milk powders. In particular, vitamin C and ferrous iron catalyzed FA formation when derivatization was conducted at 60 degrees C, as described by several authors. Artefact formation of FA was demonstrated in a model study using H-2(2)-glycine and a freeze-dried raw cow's milk with added micronutrients. A limited survey of commercial fortified milk powders showed that FA levels were about 4-fold lower when analyses were conducted at room temperature as compared to 60 degrees C (0.65 +/- 0.25 mg/kg and 2.57 +/- 0.51 mg/kg, respectively). Based on data obtained at room temperature, FA exposure from fortified milk powders does not represent a safety concern even under worst-case assumptions. This study highlights the need and importance of adopting an international standard for FA analysis in foods.