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Two sample preparation methods were developed (graphitised carbon and C18 solid phase extraction clean-up) and validated in house using liquid chromatography and tandem mass spectrometry (MS/MS) for the determination of 30 pyrrolizidine alkaloids (PAs) in salads, herbs, tea, herbals teas as well as tea infusion and ice-tea beverages. Total PAs concentration of samples purchased on the Belgian market varied greatly with matrix type ranging from

The aim of the present study was to monitor the consumption of foods containing intense sweeteners present on the Italian food market and to investigate whether the Italian general population (aged >3-65+) was at risk for exceeding the Acceptable Daily Intake (ADI) of 10 intense sweeteners. A food label survey was performed in Rome (Italy), using market share data to identify the brands more representative of the market. A sample of 326 foods (table-top sweeteners included), beverages and food supplements containing intense sweeteners was collected and analyzed in order to establish the concentration levels. Intense sweeteners were only found in foods belonging to 8 sugar-free food categories out of 37 regulated. The dietary exposure was estimated using the tiered approach. Food consumption data from the last Italian national survey (INRAN-SCAI 2005-06) were combined with Maximum Levels at Tier 2, and with the actual concentration of sweeteners in the collected food products at Tier 3. The estimated exposure among consumers of sweeteners in Italy was well below the ADIs, in both tiers; non-alcoholic beverages, table-top sweeteners and food supplements were main contributors to exposure., (Copyright © 2017 Elsevier Ltd. All rights reserved.)

2-Methylimidazole, 4-methylimidazole (2-MI and 4-MI), 2-acetyl-4-(1,2,3,4-tetrahydroxybutyl) imidazole (THI) and 5-hydroxymethylfurfural (5-HMF) are neo-formed compounds generated during the manufacture of caramel colours and are transferred to the processed food. These contaminants are known to have a toxicological profile that may pose health risks. Hence, to characterise THI, 2- and 4-MI and 5-HMF levels in liquid foods, an ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed and sample preparation was divided into two analytical strategies depending on the concentration range expected in the type of foods targeted. For the determination of the imidazole substitutes (THI, 2- and 4-MI), a sample enrichment and clean-up step by strong cation solid-phase extraction was developed. This method is capable of quantifying over a range of 5 ng ml⁻¹ (LOQ) to 500 ng ml⁻¹ with recoveries of 75.4-112.4% and RSDs of 1.5-15%. For determination of 5-HMF, a standard addition method was applied covering the linear range of 0.25-30 µg ml⁻¹ with RSDs from 2.8% (for intraday precision) to 9.2% (for intermediate precision). The validated analytical methods were applied to 28 liquid food samples purchased from local markets. THI was found only in the beer samples at levels up to 141.2 ng ml⁻¹. For 2-MI, non-quantifiable traces were observed for all samples, while 4-MI was observed in all samples with large concentration variations (from < LOQ to 563.9 ng ml⁻¹). 5-HMF was found at expected concentrations, except for a sherry vinegar sample (113 µg ml⁻¹), which required a high level of dilution before following the standard addition protocol.

Food additives are used in numerous food products and are characterised by various physicochemical properties. In European member states, their use in food is regulated by the European Union. This work aimed to develop an accurate and high-throughput analytical method enabling the simultaneous determination of additives from different functional classes to facilitate controls and generate occurrence data for exposure assessments. The QuEChERS principle was applied due to its ease of implementation and flexibility to adjust to various food matrices. However, very polar substances could not be extracted with sufficient recoveries. Consequently, an alternative basic methanol sample-preparation methodology was developed. After sample preparation, the obtained extracts were analysed using ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). Overall, the developed methodology allowed the quantification of 27 additives from the functional classes of colours, sweeteners, preservatives, and antioxidants in various foods (e.g. beverages, dairies, processed meals). The methods were also validated in terms of selectivity, linearity, matrix effect, limit of quantification, accuracy, repeatability, and intra-laboratory reproducibility. Finally, the methods were successfully applied to eighty-four actual samples. All additives were found below authorised levels. However, irregularities were spotted in labelling. [ABSTRACT FROM AUTHOR]