A gas chromatography tandem mass spectrometry has been developed and validated for the separation, detection, identification and quantification of acrylamide in bread, biscuits and similar products. The method showed good precision with values lower than 6%. A good sensitivity was achieved for bread with 2.41 and 7.23 µg kg -1 limit of detection (LOD) and limit of quantification (LOQ), respectively, while for biscuits, LOD and LOQ were 4.63 and 13.89 µg kg -1 , respectively. Accuracy obtained through the bias of 2 certified reference materials ("crisp bread -ERM ® -BD272" and "rusk -ERM ® -BD274") gave a value below 1.68-2.52%. The method was applied by analyzing 49 types of bread, biscuits and other similar products. The results showed different levels of acrylamide in bread (values ranged between 7.6 and 165.6 µg kg -1 ), biscuits (between LOD and 2405.0 µg kg ).

The aim of this work was to develop an analytical method for determining acrylamide in potato-based products by gas chromatography and tandem mass spectrometry analysis (GC-MS/MS) using solid-phase extraction (SPE) clean-up. Different conditions for extraction and clean-up of AA extracts were studied on a potato crisps reference material (RM) with the value of 625 ± 45 μg/kg: the solvent volume used for AA elution, the extraction water temperature, the volume of hexane used, and also the addition of Carrez solutions. The SPE cartridge sorbents contain silica-based C-18 groups (anion and cation exchangers) and polymers (polystyrene-divinylbenzene). After SPE clean-up, extracts were derivatized with bromine compounds. A good efficiency for AA extraction and a cleaned-up extract from this matrix were obtained when the SPE procedure was carried out with water at room temperature, simultaneous with hexane, without Carrez solutions, by using two types of SPE cartridges (Isolute Multimode; Isolute ENV+), and 5 mL of elution solvent. The SPE clean-up procedure functionality was demonstrated by the results obtained in the Food Analysis Performance Assessment Scheme proficiency test (z-score: −0.8) on French fries (precooked) matrix and also by comparative analysis with a laboratory procedure, validated and accredited on cereal-based food matrices, in which liquid–liquid extraction and clean-up through a florisil column were realized (RSD(R) = 2.23–5.10%).

For simultaneous separation, detection, identification and quantification of fatty acid methyl esters from oils/fats, a GC-MS method was developed and validated. The method is based on fat extraction and transesterification of fatty acids to fatty acid methyl esters. Samples of sunflower oil, refined non-hydrogenated palm oil, fish oil and lard, demonstrated the applicability of the proposed method. Fatty acid methyl esters determination and quantification was realized by using internal standards, and applying relative response factors, and without using internal standards by applying correction factors. Linearity, sensitivity, precision, accuracy, recovery and robustness were determined. The method is sensitive enough to simultaneously quantify 26 compounds, when using internal standard (absolute concentration), and 40 fatty acids without using internal standard (relative concentration). Accuracy was achieved by using a reference material, peanut butter (SRM ® 2387). The results have shown that the proposed method could be considered an effective tool for analyzing the fatty acid profile of food.

In the recent years, evidence has been accumulated about the beneficial effects on consumers' health of oat in daily diets, respectively: maintaining blood cholesterol, lowering postprandial glucose, cardiovascular risk reduction, reducing oxidative stress and so on. The increase of oat content in bakery products, such as bread was generally associated with a decrease in volume and a worsening of sensorial characteristics, features that are guiding the consumer's decision to buy a particular product. Researchers have aimed to achieve a bakery product that contains a sufficient amount of whole oat flour, without affecting the quality characteristics of bread (volume, porosity, elasticity). Our results have shown that the ideal proportion between the oat flour and wheat flour was 30:70, in order to obtain a functional product attractive to the consumer. We have also analyzed the main rheological changes (by farinographic and alveographic methods) of dough obtained from wheat-oat composite flours (10, 20, 30, 40, 50% oat flour). Our findings have shown that the addition of oat flour significantly increased the water absorption and decreased water retention capacity under mechanical stress. Generally, the rheological parameters in wheat-oat composite flours were affected by a more than 20% oat flour content.

Nine essential oils from fennel (seeds and herbs) and anise (seeds) from different origins were analysed for density, refractive index and for a complete composition through GC-MS and 1H-NMR-spectroscopy. Anethole was the main compound identified in fennel and anise essential oils. Anethole content varied between 30 – 90% in fennel oils and between 80 – 99% in anise oils; anethole is often used as flavouring substance in foods with a good antimicrobial activity also. A positive correlation was found between anethole content determined by GC-MS and 1H-NMR (r = 0.8567 for fennel oils and r = 0.6986 for anise oils). The results showed different levels of anethole in oils (values ranged between 30.66 % and 99.24 %). Electronic nose was a very good and rapid method for discrimination of essential oils based on PCA (Principal Component Analysis) with discrimination index above 90 for both essential oils.

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This study reports the acrylamide (AA) content of some cereal-based products purchased from different Romanian suppliers. The AA level was determined by using gas chromatography tandem mass spectrometry (GC-MS/MS) in SRM mode. The analytical method was characterized by a high degree of sensitivity (limit of detection (LOD) = 1.23 μg/kg, and limit of quantification (LOQ) = 3.70 μg/kg). A total of 46 food samples of bread, biscuits, and similar products (doughnuts, cakes, cookies etc.) were analysed. The results showed that the AA level varied between food samples, for soft bread (5.63-85.05 µg/kg), biscuits (8.55-548.80 µg/kg), crackers (13.92-167.58 µg/kg) and for similar products (12.57-99.01 µg/kg) which were lower than the benchmark levels set by the Commission Regulation (EU) 2017/2158. The highest AA content (548.80 µg/kg) was found for biscuits, while the lowest AA content (5.63 µg/kg) was obtained for wheatbased bread. From the analysed products, 4 biscuit samples exceeded the benchmark levels of 350 µg/kg established by European Union.

Cereal products are the most consumed in Romania being the main contributors to daily acrylamide exposure. The paper aims to present for the first time a general situation regarding the evolution of the acrylamide levels content from cereal products, on the Romanian market, during 2017-2018 periods, as a result of legislative measures imposed by the European Union (EU). For this purpose, the levels of acrylamide in 55 selected cereal products samples were evaluated. The cereal products analyzed were grouped in biscuits, confectionery, expanded cereals, bakery products and specialties. The acrylamide content from the cereal products were detected using GC-MS/MS method. The highest level of acrylamide was found in biscuits, whereas the lowest level was determined in bakery products. The most of the cereal products samples analyzed (90.9%) was below the reference levels established by the EU Regulation for the acrylamide level from 2017 EC (2013/647/EU) and 2018 EC (2017/2158/ EU). From the 55 cereal products analyzed, only 5 biscuits samples exceeded the reference levels established by the European Commission, one in 2017 and four in 2018 period.