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HS-SPME Gas Chromatography Approach for Underivatized Acrylamide Determination in Biscuits.

ABSTRACT: Acrylamide (AA) is a food contaminant in thermally processed products that is object of tight control. A simple and easy-to-apply methodology for routine monitoring of AA levels in food products could allow producers to be players in the control of their own products. In this work, a simple methodology for AA quantification without derivatization was developed for biscuits, for which the benchmark levels recommended by EFSA are 350 µg/kg, and 150 µg/kg for biscuits for infants and young children. Headspace-solid phase microextraction (HS-SPME) was used in 120 mL screwed-cap vials with a carboxen/polydimetylsiloxane fiber, 4 g of biscuits, and 10 mL of water during 15 min at room temperature under stirring. The addition of 30 mL of propanol under stirring during 15 min at room temperature and 15 min at 60 °C was used to promote AA transfer to the headspace. The fiber exposure was 45 min. A gas chromatography-mass spectrometry analysis allowed to obtain an external calibration curve at m/z 71, with linearity R² > 0.99 and precision RSD < 9%. The detection and quantification limits were 27.4 µg/kg and 91.5 µg/kg, respectively. The methodology was successfully used in biscuits with lower AA amount, where mitigation strategies (asparaginase or pectate) were applied.

SUBMITTER: Passos CP

PROVIDER: S-EPMC8470632 | biostudies-literature |

REPOSITORIES: biostudies-literature

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Determination of Acrylamide in Biscuits by High-Resolution Orbitrap Mass Spectrometry: A Novel Application.

Project description:Acrylamide (AA), a molecule which potentially increases the risk of developing cancer, is easily formed in food rich in carbohydrates, such as biscuits, wafers, and breakfast cereals, at temperatures above 120 °C. Thus, the need to detect and quantify the AA content in processed foodstuffs is eminent, in order to delineate the limits and mitigation strategies. This work reports the development and validation of a high-resolution mass spectrometry-based methodology for identification and quantification of AA in specific food matrices of biscuits, by using LC-MS with electrospray ionization and Orbitrap as the mass analyser. The developed analytical method showed good repeatability (RSDr 11.1%) and 3.55 and 11.8 ?g kg-1 as limit of detection (LOD) and limit of quantification (LOQ), respectively. The choice of multiplexed targeted-SIM mode (t-SIM) for AA and AA-d3 isolated ions provided enhanced detection sensitivity, as demonstrated in this work. Statistical processing of data was performed in order to compare the AA levels with several production parameters, such as time/cooking temperature, placement on the cooking conveyor belt, color, and moisture for different biscuits. The composition of the raw materials was statistically the most correlated factor with the AA content when all samples are considered. The statistical treatment presented herein enables an important prediction of factors influencing AA formation in biscuits contributing to putting in place effective mitigation strategies.

| S-EPMC6963597 | biostudies-literature

Volatile Profiles of Five Variants of Abeliophyllum distichum Flowers Using Headspace Solid-Phase Microextraction Gas Chromatography-Mass Spectrometry (HS-SPME-GC-MS) Analysis.

Project description:Abeliophyllum distichum (Oleaceae), which is the only species in the monotypic genus and is grown only on the Korean peninsula, has a high scarcity value. Its five variants (white, pink, round, blue, and ivory) have different morphological characteristics in terms of the color of petals and sepals or shape of the fruits. Despite its high value, there has been no study on variant classification except in terms of their morphological characteristics. Thus, we performed a volatile component analysis of A. distichum flowers and multivariate data analyses to reveal the relationship between fragments emitted from five variants of A. distichum flowers with their morphological characteristics. As a result, 66 volatile components of this plant were identified by headspace solid-phase microextraction gas chromatography-mass spectrometry (HS-SPME-GC-MS), showing unique patterns for each set of morphological characteristics, especially the color of the petals. These results suggest that morphological characteristics of each variant are related to the volatile composition.

| S-EPMC7912044 | biostudies-literature

Chemical Diversity between Three Graminoid Plants Found in Western Kenya Analyzed by Headspace Solid-Phase Microextraction Gas Chromatography-Mass Spectrometry (HS-SPME-GC-MS).

Project description:In recent work, it was shown that the graminoid plants Cynodon dactylon (Poaceae), Cyperus exaltatus (Cyperaceae), and Panicum repens (Poaceae) have an ovipositional effect on the malaria vector Anopheles gambiae in olfactometric bioassays. In order to get a view of the diversity of semiochemicals present in the environment of the vector during olfactometric trials, in the present work, the volatile profiles of these graminoid plants were analyzed using headspace solid-phase microextraction (HS-SPME) together with gas chromatography-mass spectrometry (GC-MS). In addition, one-way ANOVA comparison of compounds detected in two or more headspace samples are presented in order to provide a basis for comparison of compounds that could constitute a starting point for novel blends of volatile organic compounds to be tested as oviposition attractants.

| S-EPMC8617917 | biostudies-literature

Headspace solid-phase microextraction comprehensive 2D gas chromatography-time of flight mass spectrometry (HS-SPME-GC × GC-TOFMS) for origin traceability of the genus <i>Hymenaea</i> resinites.

Project description:Differentiating the chemical compositions of resinite (amber, copal, and resin) is very crucial for determining the botanical origin and chemical compositions of the fossilised amber and copal. This differentiation also assists in understanding the ecological functions of resinite. Headspace solid-phase microextraction-comprehensive two-dimensional (2D) gas chromatography-time-of-flight mass-spectroscopy (HS-SPME-GC × GC-TOFMS) was firstly proposed and utilised in this research to investigate the chemical components (volatile and semi-volatile compositions) and structures of Dominican amber, Mexican amber, and Colombian copal for origin traceability, which were all produced by trees belonging to the genus Hymenaea. Principal component analysis (PCA) was used to analyse the relative abundances of each compound. Several informative variables were selected, such as caryophyllene oxide, which was only found in Dominican amber, and copaene, which was only found in Colombian copal. 1H-Indene, 2,3-dihydro-1,1,5,6-tetramethyl- and 1,1,4,5,6-pentamethyl-2,3-dihydro-1H-indene were abundantly present in Mexican amber, which were the critical fingerprints for the origin traceability of amber and copal produced by trees from the genus Hymenaea of various geological places. Meanwhile, some characteristic compounds were closely related to the invasion of fungi and insects; their links with ancient fungi and insect categories were also decoded in this study and these special compounds could be used to further study the plant-insect interactions.

| S-EPMC10168135 | biostudies-literature

Profiling Volatile Constituents of Homemade Preserved Foods Prepared in Early 1950s South Dakota (USA) Using Solid-Phase Microextraction (SPME) with Gas Chromatography⁻Mass Spectrometry (GC-MS) Determination.

Project description:An essential dimension of food tasting (i.e., flavor) is olfactory stimulation by volatile organic compounds (VOCs) emitted therefrom. Here, we developed a novel analytical method based on solid-phase microextraction (SPME) sampling in argon-filled gas sampling bags with direct gas chromatography⁻mass spectrometry (GC-MS) determination to profile the volatile constituents of 31 homemade preserves prepared in South Dakota (USA) during the period 1950⁻1953. Volatile profiles varied considerably, but generally decreased in detected compounds, complexity, and intensity over three successive 2-h SPME sampling periods. Volatile profiles were generally predominated by aldehydes, alcohols, esters, ketones, and organic acids, with terpenoids constituting much of the pickled cucumber volatiles. Bisphenol-A (BPA) was also serendipitously detected and then quantified in 29 samples, at levels ranging from 3.4 to 19.2 μg/kg, within the range of levels known to induce endocrine disruption effects. Absence of BPA in two samples was attributed to their lids lacking plastic liners. As the timing of their preparation coincides with the beginning of BPA incorporation into consumer products, these jars may be some of the first BPA-containing products in the USA. To the best of our knowledge, this is the first effort to characterize BPA in and volatile profiles of rare historical foods with SPME.

| S-EPMC6413207 | biostudies-literature

Determination of volatile organic compounds (VOCs) from wrapping films and wrapped PDO Italian cheeses by using HS-SPME and GC/MS.

Project description:Nowadays food wrapping assures attractive presentation and simplifies self-service shopping. Polyvinylchloride (PVC)- and polyethylene (PE)-based cling-films are widely used worldwide for wrapping cheeses. For this purpose, films used in retail possess suitable technical properties such as clinginess and unrolling capacity, that are achieved by using specific plasticizers during their manufacturing process. In the present study, the main VOCs of three cling-films (either PVC-based or PE-based) for retail use were characterized by means of Solid-Phase Micro-Extraction and GC/MS. In addition, the effects of cling film type and contact time on the migration of VOCs from the films to four different PDO Italian cheeses during cold storage under light or dark were also investigated. Among the VOCs isolated from cling-films, PVC released 2-ethylhexanol and triacetin. These compounds can likely be considered as a "non-intentionally added substance". These same compounds were also detected in cheeses wrapped in PVC films with the highest concentration found after 20 days storage. The PE cling-film was shown to possess a simpler VOC profile, lacking some molecules peculiar to PVC films. The same conclusions can be drawn for cheeses wrapped in the PE cling-film. Other VOCs found in wrapped cheeses were likely to have been released either by direct transfer from the materials used for the manufacture of cling-films or from contamination of the films. Overall, HS-SPME is shown to be a rapid and solvent free technique to screen the VOCs profile of cling-films, and to detect VOCs migration from cling-films to cheese under real retail storage conditions.

| S-EPMC6271448 | biostudies-literature

Development of the Method for Determination of Volatile Sulfur Compounds (VSCs) in Fruit Brandy with the Use of HS-SPME/GC-MS.

Project description:Volatile sulfur compounds (VSCs) play an important role in the aroma profile of fermented beverages. However, because of their low concentration in samples, their analysis is difficult. The headspace solid-phase microextraction (HS-SPME) technique coupled with gas chromatography and mass spectrometry (GC-MS) is one of the methods successfully used to identify VSCs in wine and beer samples. However, this method encounters more obstacles when spirit beverages are analyzed, as the ethanol content of the matrix decreases the method sensitivity. In this work, different conditions applied during HS-SPME/GC-MS analysis, namely: ethanol concentration, salt addition, time and temperature of extraction, as well as fiber coating, were evaluated in regard to 19 sulfur compounds. The best results were obtained when 50/30 μm Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS) was used to preconcentrate the analytes from the sample at 35 °C for 30 min. The dilution of samples to 2.5% v/v ethanol and the addition of 20% w/v NaCl along with 1% EDTA significantly improves the sensitivity of extraction. The optimized method was applied to three fruit brandy samples (plum, pear, and apple) and quantification of VSCs was performed. A total of 10 compounds were identified in brandy samples and their concentration varied greatly depending on the raw material used from production. The highest concentration of identified VSCs was found in apple brandy (82 µg/L).

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Characterization of Volatile and Flavonoid Composition of Different Cuts of Dried Onion (Allium cepa L.) by HS-SPME-GC-MS, HS-SPME-GC×GC-TOF and HPLC-DAD.

Project description:Onion is widely used worldwide in various forms for both food and medicinal applications, thanks to its high content of phytonutrients, such as flavonoids and volatile sulfur compounds. Fresh onion is very perishable and drying is widely applied for extending shelf-life, thus obtaining a very easy-to-use functional food ingredient. The flavonoid and volatile fractions of different onion cuts (flakes, rings) prepared through different drying cycles in a static oven, were characterized by high-performance liquid chromatography with a diode-array detector HPLC-DAD, Head Space-Solid Phase Micro Extraction followed by Gas Chromatography coupled with Mass Spectrometry (HS-SPME-GC-MS) and Head-Space Solid Phase Micro Extraction followed by comprehensive two-dimensional Gas-Chromatography (HS-SPME-GC×GC-TOF). Onion flakes showed a significantly higher flavonoid content (3.56 mg g-1) than onion rings (2.04 mg g-1). Onion flakes showed greater amount of volatile organic compounds (VOCs) (127.26 mg g-1) than onion rings (42.79 mg g-1), with different relative amounts of di- and trisulfides-disulfides largely predominate the volatile fraction (amounts over 60% on the total volatile content), followed by trisulfides and dipropyl disulfide and dipropyl trisulfide were the most abundant VOCs. HS-SPME-GC×GC-TOF allowed for the detection of the presence of allylthiol, diethanol sulfide, 4,6-diethyl1,2,3,5-tetrathiolane, not detected by HS-SPME-GC-MS, and provided a fast and direct visualization and comparison of different samples. These results highlight different nutraceutical properties of dried onion samples processed otherwise, only differing in shape and size, thus pointing out potentially different uses as functional ingredients.

| S-EPMC7024371 | biostudies-literature

Advancement in Determination of Phthalate Metabolites by Gas Chromatography Eliminating Derivatization Step.

Project description:A gas chromatography-mass spectrometry (GC-MS) method to determine polar and thermally unstable phthalate metabolites [monomethyl phthalate-MMP, monoethyl phthalate-MEP, mono-n-butyl phthalate-MnBP, mono-(2-ethylhexyl) phthalate-MEHP] has been developed. This is the first report presenting the separation of monophthalates without derivatization step and any additional equipment or special injection port. Injection parameters (temperature, pressure, time, and volume of injection), chromatographic separation (retention gap, temperature program), and MS detection/identification (working parameters, ion selection) were investigated. Mechanisms and phenomena occurring under different conditions in the GC injector were evaluated and discussed. The limits of detection (LODs) of MMP, MEP, MnBP, MEHP in the protocol were 0.049, 0.036, 0.038, and 0.029 ng (per 2 ?L of injection), respectively. The response of the monophthalates was found to be linear in the tested concentration range (for MMP: 0.15-100 ng, MEP and MnBP: 0.11-100 ng, MEHP: 0.087-100 ng per 2 ?L) with the coefficient of determination higher than 0.9817 and inter-day precision in the range of 1.4-5.4%. The developed method is fast, easy and repeatable. Moreover, it allows for the elimination of derivatization agents, reduction of toxic waste production and simplification of analytical procedure.

| S-EPMC6974799 | biostudies-literature

The determination of methionine in proteins by gas-liquid chromatography.

Project description:Intact methionine residues in proteins were rapidly and precisely determined by measuring methyl thiocyanate released during the reaction with CNBr and separated by g.l.c. Conditions for the reaction and for chromatography on columns of Porapak P-S are described. The recovery of methyl thiocyanate from several methionine derivatives and analogues were examined. Carbamoylmethionine was adopted as a stable primary standard and ethyl thiocyanate as internal standard. The measured methionine content of several isolated proteins was close to the theoretical value indicated by previous work and the results for these and a range of food proteins agreed well with results obtained by ion-exchange chromatography after performic acid oxidation. Since CNBr does not react with methionine sulphoxide and a preliminary hydrolysis is not required, the method discriminates between methionine and any methionine sulphoxide that may be present. It could be useful in studies on the nutritional availability of methionine in processed foods.

| S-EPMC1172884 | biostudies-other

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