•Evaluation of egg products freshness by instrumental solutions is a relevant industrial need.•Ion Mobility Spectrometry coupled to Gas Chromatography (GC-IMS) provides a rapid, sensitive, ...cost-effective tool.•Developed correspondent chemometric model correctly predicts egg products freshness condition.•Freshness-related selected chemical marker compounds were identified by parallel SPME-GC-MS.•GC-IMS fingerprinting approach could be applied to detect other fraud issues within egg products chain.
Display omitted
Egg products freshness is a crucial problem for the production of safe and high quality food. Ion Mobility Spectrometry (IMS) coupled to Gas Chromatography (GC), provides a rapid, sensitive, cost-effective tool for the detection of freshness issues. A chemometric model was created recording the volatile fingerprints of the different egg products batches, analyzed as fresh, then left at room temperature and daily controlled: 97% was correctly predicted by the model. Beside this, a selection of chemical marker compounds, coherently related with eggs thermal degradation processes, was also identified through the exploitation of Solid-Phase Micro Extraction Gas Chromatography (SPME-GC-MS) technique and associated to the parallel IMS volatile fingerprinting. The GC-IMS system was successfully challenged with the analysis of mixtures in which the predominant component was fresh egg product and different aged eggs were progressively added as adulterants, certifying the reliability of the method also for the detection of sharper fraudulent activities.
Detecting and measuring food fraud is a challenging analytical task since a very wide range of food ingredients and types may be adulterated by numerous potential adulterants, many of which are yet ...unknown. To date most of the methods applied for the control of food fraud are targeted methods, which are focused on the detection of one or a few classes of known compounds.
There is an increasing availability of solutions and applications based on high resolution mass spectrometry (HRMS), allowing parallel non-targeted approaches, novel compound identification and retrospective data analysis. For these types of methods sample-handling must be minimal to allow the inclusion of as many as possible chemical categories. However data-handling of such methods is much more demanding, together with the potential requirement to integrate multiplatform data as well as conducting data fusion. To allow the processing of massive amounts of information based on the separation techniques and mass spectrometry approaches employed, effective software tools capable of rapid data mining procedures must be employed and metabolomics based approaches does appear to be the correct way forward.
To verify the relevance of modelling results, appropriate model validation is essential for non-targeted approaches, confirming the significance of the chemical markers identified.
The present paper is devoted to review and assess the current state of the art with regards non-targeted mass spectrometry in food fraud detection within many food matrices and to propose a harmonized workflow for all such applications.
•There is a increasing availability of High Resolution Mass Spectrometry non-targeted approaches to face food fraud issues.•Diversity in experimental design/data handling in scientific literature makes evaluation of method performance challenging.•Appropriate model validation is therefore a crucial step to assess reliability for quantitative or confirmatory purposes.•Present review assesses the state of the art and proposes a harmonized workflow for all such applications.•Additionally, global considerations on the applicability of these methods for legal scenarios are provided.
Food enzymes are used for technical purposes in the production of food ingredients or foods‐as‐consumed. In the European Union, the safety of a food enzyme is evaluated by EFSA on the basis of a ...technical dossier provided by an applicant. Dietary exposure is an integral part of the risk assessment of food enzymes. To develop exposure models specific to each food manufacturing process in which food enzymes are used, different input data are required which are then used in tandem with technical conversion factors. This allows the use levels of food enzyme to be related to food consumption data collected in dietary surveys. For each food manufacturing process, EFSA identified a list of food groups (FoodEx1 classification system) and collated technical conversion factors. To ensure a correct and uniform application of these input data in the assessment of food enzyme dossiers, stakeholders were consulted via open calls‐for‐data. In addition to publishing and updating the identified input parameters on an annual basis, single‐process‐specific calculators of the Food Enzyme Intake Models (FEIMs) have been developed. These calculators have been deposited at https://zenodo.org/ since 2018 for open access. By 2023, EFSA had compiled the input data for a total of 40 food manufacturing processes in which food enzymes are employed. In this document, the food manufacturing processes are structured, food groups classified initially in the FoodEx1 system are translated into the FoodEx2 system, and technical factors are adjusted to reflect the more detailed and standardised FoodEx2 nomenclature. The development of an integrated FEIM‐web tool using this collection of input data is carried out for a possible release in 2024. This tool will be able to estimate the exposure to the food enzyme–total organic solids (TOS) when employed in multiple food manufacturing processes.
The food enzyme α‐amylase (4‐α‐d‐glucan glucanohydrolase; EC 3.2.1.1) is produced with the non‐genetically modified microorganism Bacillus licheniformis strain AE‐TA by Amano Enzyme Inc. The food ...enzyme is intended to be used in eight food manufacturing processes. Since residual amounts of food enzyme‐total organic solids (TOS) are removed in two food manufacturing processes, dietary exposure was calculated only for the remaining six processes. It was estimated to be up to 0.056 mg TOS/kg body weight per day in European populations. The production strain of the food enzyme fulfils the requirements for the qualified presumption of safety approach to safety assessment. Consequently, in the absence of other concerns, the Panel considered that toxicological studies were not needed for the safety assessment of this food enzyme. A search for the similarity of the amino acid sequence of the food enzyme to known allergens was made and two matches with respiratory allergens were found. The Panel considered that the risk of allergic reactions upon dietary exposure to this food enzyme cannot be excluded (except for the production of distilled alcohol), but the likelihood is low. Based on the data provided, the Panel concluded that this food enzyme does not give rise to safety concerns under the intended conditions of use.
Forensic investigations involving acute or lethal intoxication, drug-facilitated sexual assault, driving or workplace impairment frequently require the analysis of fresh or postmortem blood samples ...to check out a wide variety of pharmaceutical and illicit drugs, even after single-dose consumption. A sensitive and selective ultrahigh-performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) screening method was developed for fast screening of 88 psychoactive drugs and metabolites in blood samples, including the ones most frequently involved in acute intoxications and forensic investigations in Italy. The new method allows short sample processing and analysis time (the whole procedure can be accomplished in less than 30 min) together with the simultaneous monitoring of a large number of pharmaceutical substances. These features represent crucial factors in the approach of acute intoxications, when the patient requires urgent and appropriate therapy. Blood sample treatment was limited to protein precipitation. Two UHPLC–MS/MS runs in positive and negative electrospray ionization modes were performed. The data were acquired at unit mass resolution in the selected reaction monitoring mode. According to international guidelines, linearity range, precision, trueness, detection and quantification limits, recovery, selectivity, specificity, carryover, and matrix effect phenomena were determined. Despite the limited sample purification and the inherent decreased chance of eliminating any potential interference, the present multiresidue screening method proved extremely effective and sensitive, allowing the detection of all tested drugs, even those belonging to structurally different classes of substances. Moreover, the developed method is easily susceptible to further expansion to encompass more drugs, either new or those becoming important for criminal investigation. This protocol was also applied to the analysis of authentic blood samples collected from victims of various crimes in routine casework, whose relevance in forensic investigations is presented in five cases.
The food enzyme thermolysin (EC. 3.4.24.27) is produced with the non‐genetically modified Anoxybacillus caldiproteolyticus strain AE‐TP by Amano Enzyme Inc. A safety evaluation of this food enzyme ...was made previously, in which EFSA concluded that this food enzyme did not give rise to safety concerns when used in eight food manufacturing processes. Subsequently, the applicant has requested to extend its use to one additional process, to withdraw two processes and to revise the use levels. In this assessment, EFSA updated the safety evaluation of this food enzyme for use in a total of seven food manufacturing processes. The dietary exposure to the food enzyme–total organic solids (TOS) was calculated to be up to 0.989 mg TOS/kg body weight (bw) per day in European populations. When combined with the no observed adverse effect level reported in the previous opinion (700 mg TOS/kg bw per day, the mid‐dose tested), the Panel derived a revised margin of exposure of at least 708. Based on the data provided for the previous evaluation and the revised margin of exposure in the present evaluation, the Panel concluded that this food enzyme does not give rise to safety concerns under the revised intended conditions of use.
The food enzyme triacylglycerol lipase (triacylglycerol acylhydrolase; EC 3.1.1.3) is produced with the non‐genetically modified Rhizopus arrhizus strain AE‐TL(B) by Amano Enzyme Inc. A safety ...evaluation of this food enzyme was made previously, in which EFSA concluded that this food enzyme did not give rise to safety concerns when used in two food manufacturing processes. Subsequently, the applicant requested to extend its use to include four additional processes and to revise the use levels. In this assessment, EFSA updated the safety evaluation of this food enzyme when used in a total of six food manufacturing processes. As the food enzyme‐total organic solids (TOS) are removed from one food manufacturing process, the dietary exposure to the food enzyme‐TOS was estimated only for the remaining five processes. Dietary exposure was calculated to be up to 0.086 mg TOS/kg body weight (bw) per day in European populations. When combined with the no observed adverse effect level reported in the previous opinion (1960 mg TOS/kg bw per day, the highest dose tested), the Panel derived a margin of exposure of at least 22,791. Based on the data provided for the previous evaluation and the revised margin of exposure in the present evaluation, the Panel concluded that this food enzyme does not give rise to safety concerns under the revised intended conditions of use.
The food enzyme α‐amylase (4‐α‐d‐glucan glucanohydrolase i.e. EC 3.2.1.1) is produced with the non‐genetically modified Cellulosimicrobium funkei strain AE‐AMT by Amano Enzyme Inc. A safety ...evaluation of this food enzyme was made previously, in which EFSA concluded that the food enzyme did not give rise to safety concerns when used in seven food manufacturing processes. Subsequently, the applicant has requested to extend its use to include three additional processes. In this assessment, EFSA updated the safety evaluation of this food enzyme when used in a total of ten food manufacturing processes. As the food enzyme‐total organic solids (TOS) are removed from the final foods in one food manufacturing process, the dietary exposure to the food enzyme‐TOS was estimated only for the remaining nine processes. The dietary exposure was calculated to be up to 0.049 mg TOS/kg body weight (bw) per day in European populations. When combined with the no observed adverse effect level previously reported (230 mg TOS/kg bw per day, the highest dose tested), the Panel derived a margin of exposure of at least 4694. Based on the data provided for the previous evaluation and the revised margin of exposure in the present evaluation, the Panel concluded that this food enzyme does not give rise to safety concerns under the intended conditions of use.
The food enzyme oryzin (EC 3.4.21.63) is produced with the non‐genetically modified Aspergillus ochraceus strain AE‐P by Amano Enzyme Inc. A safety evaluation of this food enzyme was made previously, ...in which EFSA concluded that this food enzyme did not give rise to safety concerns when used in nine food manufacturing processes. Subsequently, the applicant has requested to extend its use to one additional process, to withdraw two food processes and to revise the use levels. In this assessment, EFSA updated the safety evaluation of this food enzyme when used in a total of eight food manufacturing processes. The dietary exposure to the food enzyme‐total organic solids (TOS) was calculated to be up to 0.354 mg TOS/kg body weight (bw) per day in European populations. When combined with the no observed adverse effect level reported in the previous opinion (1862 mg TOS/kg bw per day, the highest dose tested), the Panel derived a margin of exposure of at least 5260. Based on the data provided for the previous evaluation and the revised margin of exposure in the present evaluation, the Panel concluded that this food enzyme does not give rise to safety concerns under the revised intended conditions of use.
This work presents a non-targeted high-resolution mass spectrometry inter-laboratory study for the detection of new chemical markers responsible of soft refined oils addition to extra virgin olive ...oils. Refined oils (soft deodorized and soft deacidified) were prepared on a laboratory scale starting from low-quality olive oils and analyzed together with a set of pure extra virgin olive oil (EVOO) samples and with mixtures of adulterated and pure EVOO at different percentages. The same analytical workflow was applied in two different laboratories equipped with two types of instrumentation (Q-Orbitrap and Q-TOF); a group of discriminant molecules was selected, and a tentative identification of compounds was also proposed. In summary, 12 molecules were identified as markers of this specific adulteration, and seven of them were selected as discriminative in both the laboratories, with a similar trend throughout the samples (i.e., propylene glycol 1 stearate). The results obtained in the two laboratories are comparable, concretely demonstrating the inter-laboratory repeatability of non-targeted studies. As a confirmation, the same markers were detected also in “in-house” mixtures and in suspect commercial deodorized mixtures, reinforcing the robustness of the results obtained and proving that, thanks to these molecules, mixtures containing at least 40% of adulterated oils can be detected.
PDF
