Pitfalls in the Detection of Volatiles Associated with Heated Tobacco and e-Vapor Products When Using PTR-TOF-MS.

We investigated the applicability of proton transfer reaction-time-of-flight mass spectrometry (PTR-TOF-MS) for quantitative analysis of mixtures comprising glycerin, acetol, glycidol, acetaldehyde, acetone, and propylene glycol. While PTR-TOF-MS offers real-time simultaneous determination, the method selectivity is limited when analyzing compounds with identical elemental compositions or when labile compounds present in the mixture produce fragments that generate overlapping ions with other matrix components. In this study, we observed significant fragmentation of glycerin, acetol, glycidol, and propylene glycol during protonation via hydronium ions (H3O+). Nevertheless, specific ions generated by glycerin (m/z 93.055) and propylene glycol (m/z 77.060) enabled their selective detection. To thoroughly investigate the selectivity of the method, various mixtures containing both isotope-labeled and unlabeled compounds were utilized. The experimental findings demonstrated that when samples contained high levels of glycerin, it was not feasible to perform time-resolved analysis in H3O+ mode for acetaldehyde, acetol, and glycidol. To overcome the observed selectivity limitations associated with the H3O+ reagent ions, alternative ionization modes were investigated. The ammonium ion mode proved appropriate for analyzing propylene glycol (m/z 94.086) and acetone (m/z 76.076) mixtures. Concerning the nitric oxide mode, specific m/z were identified for acetaldehyde (m/z 43.018), acetone (m/z 88.039), glycidol (m/z 73.028), and propylene glycol (m/z 75.044). It was concluded that considering the presence of multiple product ions and the potential influence of other compounds, it is crucial to conduct a thorough selectivity assessment when employing PTR-TOF-MS as the sole method for analyzing compounds in complex matrices of unknown composition.

Development of a GC-FID method for quantitative characterisation of polyglycerols in polyglycerol polyricinoleate (PGPR) present in a lipid matrix.

PGPR is an emulsifier (E476) widely used in the food industry. In this study, a gas chromatography-flame ionisation detection (GC-FID) method was developed for the quantitative characterisation of the polyglycerol composition of PGPR. The method was validated to analyse quantitatively the polyglycerol species in neat PGPR products and in PGPR samples present in a lipid matrix. This method consists of saponification, acidification and petroleum ether extraction to remove interfering fatty acids, neutralisation, silylation and finally GC-FID analysis. Phenyl ß-D-glucopyranoside was used as internal standard as sorbitol proved unsuitable due to its susceptibility to interference from Na/K chloride during silylation. The response factors of glycerol and diglycerol towards phenyl ß-D-glucopyranoside were determined using pure standards, while response factors of polyglycerols with a degree of polymerisation of at least 3 could be reliably estimated according to an effective carbon number (ECN) approach. The validity of the method applied to PGPR samples was further supported on the basis of a mass balance considering the experimentally determined polyglycerol and fatty acid content. Moreover, recoveries of di-, tri-, tetra- and pentaglycerol were more than 95% for various PGPR samples added to two different lipid matrices at 2 wt% and 5 wt% concentrations. Furthermore, the method proved to be very repeatable (with relative standard deviation values below 2.2%). On the other hand, the inevitable presence of glycerol in the lipid samples caused fouling of the detector and column overloading, requiring frequent cleaning of the detector and trimming off part of the column.

Conventional and multi-omics assessments of subacute inhalation toxicity due to propylene glycol and vegetable glycerin aerosol produced by electronic cigarettes.

Propylene glycol (PG) and vegetable glycerin (VG) are the most common solvents used in electronic cigarette liquids. No long-term inhalation toxicity assessments have been performed combining conventional and multi-omics approaches on the potential respiratory effects of the solvents in vivo. In this study, the systemic toxicity of aerosol generated from a ceramic heating coil-based e-cigarette was evaluated. First, the aerosol properties were characterized, including carbonyl emissions, the particle size distribution, and aerosol temperatures. To determine toxicological effects, rats were exposed, through their nose only, to filtered air or a propylene glycol (PG)/ glycerin (VG) (50:50, %W/W) aerosol mixture at the target concentration of 3 mg/L for six hours daily over a continuous 28-day period. Compared with the air group, female rats in the PG/VG group exhibited significantly lower body weights during both the exposure period and recovery period, and this was linked to a reduced food intake. Male rats in the PG/VG group also experienced a significant decline in body weight during the exposure period. Importantly, rats exposed to the PG/VG aerosol showed only minimal biological effects compared to those with only air exposure, with no signs of toxicity. Moreover, the transcriptomic, proteomic, and metabolomic analyses of the rat lung tissues following aerosol exposure revealed a series of candidate pathways linking aerosol inhalation to altered lung functions, especially the inflammatory response and disease. Dysregulated pathways of arachidonic acids, the neuroactive ligand-receptor interaction, and the hematopoietic cell lineage were revealed through integrated multi-omics analysis. Therefore, our integrated multi-omics approach offers novel systemic insights and early evidence of environmental-related health hazards associated with an e-cigarette aerosol using two carrier solvents in a rat model.

Qualitative and Quantitative Analysis of Five Indoles or Indazole Amide Synthetic Cannabinoids in Suspected E-Cigarette Oil by GC-MS.

OBJECTIVES: To establish the GC-MS qualitative and quantitative analysis methods for the synthetic cannabinoids, its main matrix and additives in suspicious electronic cigarette (e-cigarette) oil samples. METHODS: The e-cigarette oil samples were analyzed by GC-MS after diluted with methanol. Synthetic cannabinoids, its main matrix and additives in e-cigarette oil samples were qualitatively analyzed by the characteristic fragment ions and retention time. The synthetic cannabinoids were quantitatively analyzed by using the selective ion monitoring mode. RESULTS: The linear range of each compound in GC-MS quantitative method was 0.025-1 mg/mL, the matrix recovery rate was 94%-103%, the intra-day precision relative standard deviations (RSD) was less than 2.5%, and inter-day precision RSD was less than 4.0%. Five indoles or indazole amide synthetic cannabinoids were detected in 25 e-cigarette samples. The main matrixes of e-cigarette samples were propylene glycol and glycerol. Additives such as N,2,3-trimethyl-2-isopropyl butanamide (WS-23), glycerol triacetate and nicotine were detected in some samples. The content range of synthetic cannabinoids in 25 e-cigarette samples was 0.05%-2.74%. CONCLUSIONS: The GC-MS method for synthesizing cannabinoid, matrix and additive in e-cigarette oil samples has good selectivity, high resolution, low detection limit, and can be used for simultaneous qualitative and quantitative analysis of multiple components; The explored fragment ion fragmentation mechanism of the electron bombardment ion source of indole or indoxamide compounds helps to identify such substances or other compounds with similar structures in cases.

Determination of process contaminants 2- and 3-MCPD esters and glycidyl esters in palm-based glycerol by indirect analysis using GC-MS.

Esters of 2- and 3-monochloropropanediol (2-MCPDE, 3-MCPDE) and glycidol (GE) are regarded as process contaminants that are found in refined vegetable oils and oil-based foods. Since glycerol is produced during fat splitting, saponification and biodiesel production, it is important to have methods for determining contaminants that might be formed during these processes. Due to the use of glycerol as a food additive, data on the presence of compounds of toxicological concern, including 3-MCPD, are of interest. This study focuses on modifying the indirect analysis of 2-MCPDE, 3-MCPDE and GE using GC-MS based on the AOCS Official Method Cd 29a-13, validating the modified method, and quantifying 2-MCPDE, 3-MCPDE and GE in glycerol. The AOCS Cd 29a-13 method was modified at the initial stage of sample preparation in which the targeted esters were extracted from glycerol by vortex-assisted extraction before sample analysis. This modification was performed based on the polarity of all compounds involved. The calibration functions for all analytes were fitted to linear regression with R2 above 0.99. Limits of detection (LOD) 0.02, 0.01 and 0.02 mg kg-1 were obtained for 2-MCPDE, 3-MCPDE and GE, respectively. Spiked glycerol with 3-MCPDE and 2-MCPDE (0.25, 0.51 and 1.01 mg kg-1) and GE (0.58, 1.16 and 2.32 mg kg-1) were used for recovery and precision measurements. Recoveries of 100-108%, 101-103%, and 93-99% were obtained for 2-MCPDE, 3-MCPDE and GE, respectively. Acceptable precision levels with relative standard deviations ranged from 3.3% to 8.3% were obtained for repeatability and intermediate precision. The validated method was successfully applied for the analysis of the target compounds in refined glycerol from commercial plants, which showed that 2-MCPDE, 3-MCPDE and GE levels in the analysed samples were below the detection limit.

Detection of the Synthetic Coolant Menthone 1,2-Glycerol Ketal in an e-Liquid and in Electronic Waterpipe Aerosols Therefrom.

The presence and toxicological risks of synthetic coolants in electronic nicotine delivery systems (ENDS) have not been thoroughly studied. We identified the synthetic coolant menthone 1,2-glycerol ketal (MGK) in a menthol-flavored e-liquid at a concentration of ∼170 µg/mL. We also detected MGK in aerosols resulting from heating the e-liquid with an electronic waterpipe. MGK was initially detected in the e-liquid by two-dimensional gas chromatography-time-of-flight mass spectrometry. To avoid potential analytical artifacts that could result from heating samples in the injection port of the gas chromatograph, quantitation of MGK in the e-liquid was accomplished using a liquid chromatography-tandem mass spectrometry method. Following recent reports identifying other synthetic coolants in e-liquids, these results add knowledge about inhalation exposures from ENDS use and suggest the importance of future research to study the potential inhalation toxicity related to the use of MGK-containing e-liquids in ENDS devices. Furthermore, the results demonstrate the ability to quantify ketals in e-liquids using liquid chromatography methods.

A novel online dispersive liquid-liquid microextraction for the spectrophotometric determination of free glycerol in biodiesel.

Biodiesel is an important alternative fuel produced from animal fats or vegetable oils. According to several world regulatory agencies, the acceptable threshold content for free glycerol in biodiesel is 200 mg kg-1. Exceeding concentrations may yield high amounts of acrolein after combustion. The analytical methods for glycerol determination are usually preceded by conventional liquid-liquid extraction that may affect precision and accuracy and impair analytical frequency. In this work, a multi-pumping flow system was proposed for the online dispersive liquid-liquid extraction of free glycerol from biodiesel followed by spectrophotometric determination. The analyte was transferred to the aqueous phase by mixing the sample and water under a pulsed flow regime. The emulsion was directed towards a retention column to remove the organic phase before chemical derivatization. Glycerol was oxidized by NaIO4 to generate formaldehyde, which reacted with acetylacetone in an ammonium acetate medium to yield 3,5-diacetyl-1,4-dihydrolutidine (λMAX = 412 nm). The optimization of the main parameters of the system was carried out by multivariate methods. The screening of variables was performed by fractional factorial design 24-1. The models for free glycerol determination and extraction were refined by central composite and full factorial 23, respectively. In both cases, the validation was carried out by analysis of variance, which yielded a satisfactory F-test value. After optimization, a linear range from 3.0 to 50.0 mg L-1 glycerol was observed. The detection limit, coefficient of variation and determination frequency were estimated to be 2.0 mg L-1 (n = 20; 99.7% confidence level), 4.2-6.0% (n = 20) and 16 h-1, respectively. The efficiency of the process was estimated to be 66%. After each extraction, the retention column (filled with 185 mg of glass microfiber) was washed with 50% ethanol solution to avoid carry-over effects. The comparative analyses of samples by the proposed and reference methods demonstrated the accuracy of the developed procedure at a 95% confidence level. Recoveries between 86 and 101% also indicated that the proposed procedure is accurate, suitable and reliable for online extraction and determination of free glycerol in biodiesel.

Correlation of the presence of acrolein with higher alcohols, glycerol, and acidity in cachaças.

Acrolein is a toxic aldehyde that can be present in various beverages, such as cachaça and other distilled spirits from sugarcane. The objective of this work was to detect and quantify acrolein in samples of cachaça produced by different processes in all regions of Brazil and to evaluate the possible routes of formation of this contaminant from the correlation with other secondary compounds present in the beverage using principal component analysis. Approximately 27.0% of the samples analyzed were outside the limit established by Brazilian legislation for this contaminant, with an average acrolein concentration of 14.01 mg 100 mL-1 anhydrous alcohol (aa). In the other samples, the average concentration was 0.97 mg 100 mL-1 aa. After selecting the variables that most closely correlated with the presence of acrolein in beverages, a positive correlation was found with the presence of butan-2-ol, propan-1-ol and volatile acids, and a slight correlation with the presence of phenolic compounds. Therefore, the presence of acrolein in cachaça can be associated with contamination of the fermentation must by bacteria of the genus Lactobacillus, as a result of the chemical degradation and enzymatic conversion of the glycerol produced during fermentation.

Characterization of Indigenous Non-Saccharomyces Yeast Strains with Potential Use in Winemaking.

BACKGROUND: The vineyard is a great reservoir of autochthonous yeast strains whose composition is defined by different regional (edaphology, orography or climatology) and anthropological factors (cultivation systems or cultural practices). Most of this yeast diversity corresponds to non-Saccharomyces strains, some of which have potential use in winemaking. METHODS: The oenological potential of 29 different native non-Saccharomyces strains belonging to 4 species (Lachancea thermotolerans, Torulaspora delbrueckii, Starmerella bacillaris and Metschnikowia spp.) was evaluated, using the autochthonous Saccharomyces cerevisiae XG3 strain as a control. Microfermentations with pure culture of each strain were performed in duplicate and the basic parameters and major volatiles of wines were analysed following official methodology. The best strain within each species was selected using a quantification matrix including the relevant oenological characteristics. RESULTS: The fermentative ability of non-Saccharomyces was lower than S. cerevisiae in all cases, but with differences among species. L. thermotolerans and T. delbrueckii showed higher fermentation rates than Starm. bacillaris, whereas Metschnikowia spp. presented a low fermentative power. At chemical level all non-Saccharomyces strains reduced the alcoholic content, the higher alcohols and the volatile acidity of wines and increased the content of glycerol, with differences among strains within a given species. T. delbrueckii and L. thermotolerans increased the total acidity of wines. The latter and Metschnikowia spp. strains produced lactic acid, which decreased the wine pH in the case of L. thermotolerans. According to their oenological traits the best rated strains of each species were Lt93, Td315, Mf278 and Sb474. In addition, the data obtained in pure fermentations were correlated to those chemical and aromatic compounds obtained with these non-Saccharomyces strains in sequential fermentations. CONCLUSIONS: Autochthonous strains of non-Saccharomyces yeast species contribute distinctive chemical characteristics to the wines. The correlations observed between wines fermented with the different non-Saccharomyces indigenous strains in pure and sequential fermentations suggest that their contribution to wine properties remains stable regardless of must composition or winemaking techniques.

Occurrence and risk assessment of 3-monochloropropanediols esters (3-MCPDE), 2-monochloropropanediol esters (2-MCPDE), and glycidyl esters (GE) in commercial infant formula samples from Malaysia.

The presence of 3-monochloropropanediol esters (3-MCPDE), 2-monochloropropanediol esters (2-MCPDE) and glycidyl esters (GE) in infant formula products has raised serious concerns. They incorporate vegetable oils, particularly palm-based oils, which are well-known to contain large amounts of these process contaminants. An analysis was conducted on infant formula samples (n = 16) obtained from the Malaysian market to determine the levels of 3-MCPDE, 2-MCPDE and GE using gas chromatography-mass spectrometry (GC-MS). The method was validated, with a limit of quantification (LOQ) on instrument of 0.10 µg/g for all analytes. The median concentrations of 3-MCPDE, 2-MCPDE and GE in infant formula in this study were 0.008 µg/g, 0.003 µg/g and 0.002 µg/g respectively. The estimated dietary intakes calculated from consumption of infant formula show higher exposures to infants within the age group of 0 to 5 months, highest for GE (1.61 µg/kg bw/day), followed by 3-MCPDE (0.68 µg/kg bw/day) and 2-MCPDE (0.41 µg/kg bw/day) compared to the age group of 6 to 12 months. Only one sample, relating to GE exposure is a potential risk for both age groups with MOE value below 25,000.

Positional and compositional analysis of saturated, monounsaturated, and polyunsaturated fatty acids in human adipose tissue triglyceride by 13 C nuclear magnetic resonance.

The synthesis and turnover of triglyceride in adipose tissue involves enzymes with preferences for specific fatty acid classes and/or regioselectivity regarding the fatty acid position within the glycerol moiety. The focus of the current study was to characterize both the composition of fatty acids and their positional distribution in triglycerides of biopsied human subcutaneous adipose tissue, from subjects with wide ranges of body mass index (BMI) and insulin sensitivity, using 13 C nuclear magnetic resonance (NMR) spectroscopy. The triglyceride sn2 position was significantly more enriched with monounsaturated fatty acids compared with that of sn1,3, while the abundance of saturated fatty acids was significantly lower in the sn2 position compared with that of sn1,3. Furthermore, the analysis revealed significant positive correlations between the total fraction of palmitoleic acid with both BMI and insulin sensitivity scores (homeostatic model assessment of insulin resistance index). Additionally, we established that 13 C NMR chemical shifts for ω-3 signals, centered at 31.9 ppm, provided superior resolution of the most abundant fatty acid species, including palmitoleate, compared with the ω-2 signals that were used previously. 13 C NMR spectroscopy reveals for the first time a highly nonhomogenous distribution of fatty acids in the glycerol sites of human adipose tissue triglyceride, and that these distributions are correlated with different phenotypes, such as BMI and insulin sensitivity.

Effect of Crude Glycerin in the Feed of Lactating Goats on Concentrations of Essential and Toxic Metals in Serum, Urine, Milk, and Artisanal "Coalho" Cheese.

Goat farming is concentrated in semi-arid and tropical regions in Brazil. From 2006 to 2017, the number of goats sold in the country increased by 65.7%. The dairy products from these animals present higher digestibility, high vitamin A and B content, hypoallergenicity, and less lactose compared to dairy products from cows, in addition to having a higher sales value. Since corn and soybean meal generate an expense for feed management, crude glycerin, originating from the manufacture of biodiesel, has been studied as an energy substitute. However, this product contains heavy metals, posing risks to animal and human health. Few data are available on trace elements in biological samples and products derived from goats' milk with the dietary introduction of glycerin. The objective was to quantify aluminum (Al), cadmium (Cd), cobalt (Co), chromium (Cr), copper (Cu), iron (Fe), manganese (Mn), molybdenum (Mo), nickel (Ni), lead (Pb), and zinc (Zn) in the serum, urine, milk, and artisanal "coalho" cheese of dairy goats fed different levels of crude glycerin in feed management. In total, 16 Saanen goats were selected, lactating females, that were distributed in four Latin squares and randomly treated with different levels of crude glycerin (0, 5, 10, and 15%). After the end of each experiment cycle, serum, urine, milk, and artisanal "coalho" cheese samples were collected at the four moments. The samples were submitted to digestion assisted by microwave radiation. The multi-element analysis was carried out using inductively coupled plasma optical emission spectrometry (ICP OES). There was no influence of crude glycerin levels replacing corn in serum, milk, urine, and artisanal "coalho" cheese. The serum concentration of the metals Cu, Fe, Zn, and Mn; urine concentrations of Cu, Zn, Mn, Mo, and Cr; and milk and artisanal "coalho" cheese concentrations of Cu, Zn, and Mn remained within the standards found in the literature. The inclusion of 5 to 15% of crude glycerin, derived from cotton oil, in the diets of dairy goats in partial replacement of corn, does not alter the concentration of essential and toxic metals in serum, urine, milk, and artisanal "coalho" cheese and does not, therefore, present a risk factor for intoxication.

Influence of ultrasonic-microwave power on the structure and in vitro digestibility of lotus seed starch-glycerin monostearin complexes after retrogradation.

The digestibility of starches with high amylose content can be modulated by the complexation with lipids, which is largely influenced by physical modification methods. In the current work, the impact of ultrasound-microwavre synergistic treatment on the structure and in vitro digestibility of lotus seed starch-glycerin monostearin complexes (LS-GMSc) after retrogradation were investigated. Results showed that 400 W of ultrasound treatment combined with microwave was more conducive to the formation of LS-GMSc, which increased the microcrystalline region and ordering degree of starch. However, excessively high ultrasound intensity weakened V-type diffraction and promoted amylose recrystallization. Investigation of the micromorphology and thermal properties revealed that the existence of V-complexes retarded starch retrogradation, and this effect was significantly enhanced after appropriate ultrasound (400 W) treatment. The digestion showed that 400 W of ultrasound treatment improved the digestive resistance of starch complexes and increased the content of resistant starch. These results are significant to the theoretical foundation and functional application of V-type complexes on anti-gelling and anti-digestion.

Qualitative and Quantitative Analysis of Five Indoles or Indazole Amide Synthetic Cannabinoids in Suspected E-Cigarette Oil by GC-MS / 法医学杂志

OBJECTIVES@#To establish the GC-MS qualitative and quantitative analysis methods for the synthetic cannabinoids, its main matrix and additives in suspicious electronic cigarette (e-cigarette) oil samples.@*METHODS@#The e-cigarette oil samples were analyzed by GC-MS after diluted with methanol. Synthetic cannabinoids, its main matrix and additives in e-cigarette oil samples were qualitatively analyzed by the characteristic fragment ions and retention time. The synthetic cannabinoids were quantitatively analyzed by using the selective ion monitoring mode.@*RESULTS@#The linear range of each compound in GC-MS quantitative method was 0.025-1 mg/mL, the matrix recovery rate was 94%-103%, the intra-day precision relative standard deviations (RSD) was less than 2.5%, and inter-day precision RSD was less than 4.0%. Five indoles or indazole amide synthetic cannabinoids were detected in 25 e-cigarette samples. The main matrixes of e-cigarette samples were propylene glycol and glycerol. Additives such as N,2,3-trimethyl-2-isopropyl butanamide (WS-23), glycerol triacetate and nicotine were detected in some samples. The content range of synthetic cannabinoids in 25 e-cigarette samples was 0.05%-2.74%.@*CONCLUSIONS@#The GC-MS method for synthesizing cannabinoid, matrix and additive in e-cigarette oil samples has good selectivity, high resolution, low detection limit, and can be used for simultaneous qualitative and quantitative analysis of multiple components; The explored fragment ion fragmentation mechanism of the electron bombardment ion source of indole or indoxamide compounds helps to identify such substances or other compounds with similar structures in cases.

Mechanism of the Initial Tubulin Nucleation Phase.

Tubulin nucleation is a highly frequent event in microtubule (MT) dynamics but is poorly understood. In this work, we characterized the structural changes during the initial nucleation phase of dynamic tubulin. Using size-exclusion chromatography-eluted tubulin dimers in an assembly buffer solution free of glycerol and tubulin aggregates enabled us to start from a well-defined initial thermodynamic ensemble of isolated dynamic tubulin dimers and short oligomers. Following a temperature increase, time-resolved X-ray scattering and cryo-transmission electron microscopy during the initial nucleation phase revealed an isodesmic assembly mechanism of one-dimensional (1D) tubulin oligomers (where dimers were added and/or removed one at a time), leading to sufficiently stable two-dimensional (2D) dynamic nanostructures, required for MT assembly. A substantial amount of tubulin octamers accumulated before two-dimensional lattices appeared. Under subcritical assembly conditions, we observed a slower isodesmic assembly mechanism, but the concentration of 1D oligomers was insufficient to form the multistranded 2D nucleus required for MT formation.

Computational modeling method to estimate secondhand exposure potential from exhalations during e-vapor product use under various real-world scenarios.

Potential secondhand exposure of exhaled constituents from e-vapor product (EVP) use is a public health concern. We present a computational modeling method to predict air levels of exhaled constituents from EVP use. We measured select constituent levels in exhaled breath from adult e-vapor product users, then used a validated computational model to predict constituent levels under three scenarios (car, office, and restaurant) to estimate likely secondhand exposure to non-users. The model was based on physical/thermodynamic interactions between air, vapor, and particulate phase of the aerosol. Input variables included space setting, ventilation rate, total aerosol amount exhaled, and aerosol composition. Exhaled breath samples were analyzed after the use of four different e-liquids in a cartridge-based EVP. Nicotine, propylene glycol, glycerin, menthol, formaldehyde, acetaldehyde, and acrolein levels were measured and reported based on a linear mixed model for analysis of covariance. The ranges of nicotine, propylene glycol, glycerin, and formaldehyde in exhaled breath were 89.44-195.70 µg, 1199.7-3354.5 µg, 5366.8-6484.7 µg, and 0.25-0.34 µg, respectively. Acetaldehyde and acrolein were below detectable limits; thus, no estimated exposure to non-EVP users is reported. The model predicted that nicotine and formaldehyde exposure to non-users was substantially lower during EVPs use compared to cigarettes. The model also predicted that exposure to propylene glycol, glycerin, nicotine and formaldehyde among non-users was below permissible exposure limits.

Effect of a chitosan coating incorporating epigallocatechin gallate on the quality and shelf life of bighead carp (Aristichthys nobilis) fillets during chilled storage.

The objective of this study was to investigate the potential application of chitosan coatings incorporating epigallocatechin gallate (EGCG) for preserving fillets of bighead carp during chilled storage. The fillets were coated with acetic acid and glycerol, chitosan, and chitosan-EGCG, respectively, and the changes in their physicochemical, microbiological, and sensory characteristics during storage at 4 °C were determined. Notably, total volatile basic nitrogen, thiobarbituric-acid-reactive substances, and K value of chitosan-EGCG coated fillets sampled on day 15 were 48.04 %, 60.19 %, and 32.91 % lower than untreated fillets, respectively. Microbial enumeration suggested that the inclusion of EGCG significantly improved the inhibitory effect of pure chitosan coating on the proliferation of microorganisms. Furthermore, the chitosan-EGCG coated fillets also performed the best in terms of color, texture, and sensory analysis, and extended the shelf-life of the fillets for at least 6 days. A principal component analysis further confirmed the preserving effect of the chitosan-EGCG coating. Mantel test results suggested that the fillets' organoleptic characteristics strongly correlated with physicochemical and microbiological indicators. Overall, this work provides an effective protocol for food quality control and the extension of shelf life during chilled storage, and it clarifies the relationships between organoleptic characteristics and physicochemical and microbiological indexes.

Valorization of Amaranth (Amaranthus cruentus) Grain Extracts for the Development of Alginate-Based Active Films.

This research work investigates the development of alginate-based films incorporating phenolic compounds extracted from Amaranthus cruentus grain using different solvents. Alginate, glycerol, and amaranth grain phenolic compounds at various concentrations were used to produce the films. An experimental Central Composite Rotatable Design (CCRD) was used to evaluate the effect of these variables on different film's properties, i.e., water vapor permeability, hydrophobicity, moisture content, solubility, thermal, mechanical, and optical properties. This study demonstrated that high phenolic compound content and antioxidant capacity were obtained from amaranth grain using ethanol as the extraction solvent. Alginate films incorporating amaranth phenolic compounds were successfully manufactured, and this study can be used to tailor the formulation of alginate films containing amaranth phenolic compounds, depending on their final food application. For example, less flexible but more resistant and water-soluble films can be produced by increasing the alginate concentration, which was confirmed by a Principal Component Analysis (PCA) and Partial Least Squares (PLS) analysis. This study showed that active alginate films with amaranth phenolic compounds can be tailored to be used as food packaging material with potential antioxidant activity.

Analysis of Polar Lipids in Hemp (Cannabis sativa L.) By-Products by Ultra-High Performance Liquid Chromatography and High-Resolution Mass Spectrometry.

Polar lipids were extracted from residual biomass of hemp (Cannabis sativa L.) by-products with EtOH and partitioned into aqueous and chloroform fractions. The chloroform fractions were studied for their lipid composition using solid-phase extraction (SPE) followed by UHPLC/HRMS and NMR analyses. The 1H NMR and gravimetric yield of SPE indicated triacylglycerols covered ≥ 51.3% of the chloroform fraction of hemp seed hulls and hemp cake. UHPLC/HRMS analyses of remaining polar lipids led to the identification of nine diacylglycerols (DAGs), six lysophosphatidylcholines (LPCs), five lysophosphatidylethanolamines (LPEs), eight phosphatidylethanolamines (PEs), and thirteen phosphatidylcholines (PCs) for the first time from hemp seed hulls. The regiospecificity of fatty acyl substitutes in glycerol backbone of individual phospholipids were assigned by analyzing the diagnostic fragment ions and their intensities. The heat-map analysis suggested that DAG 18:2/18:2, 1-LPC 18:2, 1-LPE 18:2, PE 18:2/18:2, and PC 18:2/18:2 were the predominant molecules within their classes, supported by the fact that linoleic acid was the major fatty acid covering > 41.1% of the total fatty acids determined by GC-FID analysis. The 31P NMR analysis confirmed the identification of phospholipids and suggested PC covers ≥ 37.9% of the total phospholipid present in hemp by-products. HPLC purification led to the isolation of 1,2-dilinoleoylphosphatidylcholine and 1-palmitoyl-2-linoleoylphosphatidylcholine. These two major PCs further confirmed the UHPLC/HRMS finding.

Occurrence of 2- and 3-monochloropropanediol esters (MCPDE) in infant formula products on the Canadian market between 2015 and 2019.

2- and 3-monochloropropanediol esters (MCPDEs) are most commonly formed as process-induced contaminants during the refinement of vegetable oils used for food production. 'In vivo' hydrolysis of 3-MCPDEs releases the potential carcinogen 3-monochloropropanediol (3-MCPD). Levels of MCPDEs in infant formula are of particular concern, as refined oils are commonly used as main fat ingredients. For this study, infant formula samples (powders, liquid concentrates and ready-to-feed infant formula samples) from the Canadian market were purchased and analysed in 2015 (35 samples) and 2019 (33 samples). MCPDE concentrations (expressed as free MCPD equivalents) were examined through an indirect analytical approach, applying acid-catalysed ester cleavage and using cyclohexanone as derivatising agent. Labelled diesters were used as internal standards. 2015 Survey data were analysed by gas chromatography-mass spectrometry (GC-MS) in selected ion monitoring mode (SIM). 2019 Survey data were analysed with an updated method using GC-MS/MS in multiple reaction monitoring modes (MRM). In 2015, levels in reconstituted formula ranging from 3.7 ng/g to 111 ng/g for 3-MCPD and 2.2 ng/g to 56.2 ng/g for 2-MCPD were found. In 2019, levels ranging from 3.9 ng/g to 74.8 ng/g for 3-MCPD and 1.0 ng/g to 33.9 ng/g for 2-MCPD were found. A significantly reduced mean of combined MCPDEs was observed between 2015 and 2019 data (64.5 ng/g, standard deviation (SD) 8.6 ng/g in 2015 to 31.8 ng/g, SD 5.6 ng/g in 2019, p-value = 0.024). For the majority of manufacturers, the data comparison among brand products over time shows decreased levels of MCPDEs. Occurrence data of MCPDEs, including data from previously published surveys (2012/2013), were also compared and a temporal trend was established.