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Edible wild mushrooms are one of the popular ingredients due to their high quality and unique flavor and nutrients. To gain insight into the effect of drying temperature on its composition, 86 Boletus bainiugan were divided into 5 groups and dried at different temperatures. Headspace solid-phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) was used for the identification of volatile organic compounds (VOCs) of Boletus bainiugan. The 21 differential VOCs that distinguish different drying temperatures of Boletus bainiugan were identified. 65 °C retained more VOCs. There were differences in their types and content at different temperatures, proteins, polysaccharides, crude fibers, and fats. Fourier transform near-infrared (FT-NIR) spectroscopy, Fourier transform infrared (FTIR) spectroscopy, and two-dimensional correlation spectroscopy (2DCOS) images were successfully characterized for differences in the chemical composition of Boletus bainiugan. Partial least squares discriminant analysis (PLS-DA) verified the variability in the chemical composition of Boletus bainiugan with the coefficient of determination (R2) = 0.95 and predictive performance (Q2) = 0.75 with 92.31% accuracy. Next, infrared spectroscopy provides a fast and efficient assessment of the content of Boletus bainiugan nutrients (proteins, polysaccharides, crude fibers, and fats).
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A new method was evaluated and developed for the analysis of pesticides in sandy-loam soil by direct-immersion solid phase microextraction (DI-SPME) followed by gas chromatography tandem-mass spectrometry (GC-MS/MS) determination. Ten pesticides were selected based on a literature survey of the compounds reported to be present in EU soils. The extraction was performed using SPME LC-Tips, a new SPME configuration with the coated fibers attached to a disposable and easy-to-handle micropipette tip, which was immersed into a soil slurry made by the addition of an aqueous solution to the soil sample. Ten experimental parameters were evaluated with a Plackett-Burman design, after which the extraction time and percentage of organic solvent in the aqueous extraction were optimized separately. The two fiber chemistries available (PDMS/DVB and C18) were evaluated in parallel for the entire work. In the final method, slurry samples were made by adding an aqueous solution (6 % methanol v/v) to 2 g of soil. The fiber was conditioned and then inserted, for extraction, into the samples, stirred by a magnetic bar. Afterwards, the analytes were desorbed onto 100 µL of methanol. After the addition of analyte protectants (ethylglycerol, gulonolactone, and sorbitol) the extract was injected into the GC-MS/MS system. Isotopically labelled penconazole was used as internal standard. A calibration was performed by extracting spiked soil with analyte concentrations of 0.1-50 µg/kg. Coefficients of determination of the linear calibration were between 0.94-0.98 for the PDMS/DVB and 0.92-0.99 for the C18. Limits of detection range between 0.01-10 µg/kg for the PDMS/DVB and 0.1-10 µg/kg for the C18. Overall, the C18 analytically outperformed the PDMS/DVB but required a longer extraction time (120 min vs 75 min for the PDMS/DVB). This method allows automation and generates low residual toxic waste, having the potential to be introduced as a greener and simpler alternative to currently used sample preparation methodologies.
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Dark tea (DT) holds a rich cultural history in China and has gained sizeable consumers due to its unique flavor and potential health benefits. In this study, headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-mass spectrometry (GC-MS), relative odor activity value (ROAV), and chemometrics approaches were used to detect and analyze aroma compounds differences among five dark teas from different geographical regions. The results revealed that the five DTs from different geographical regions differed in types, quantities, and relative concentrations of volatile compounds. A total of 1372 volatile compounds of were identified in the 56 DT samples by HS-SPME-GC-MS. Using ROAV and chemometrics approaches, based on ROAV>1 and VIP>1. Eighteen key aroma compounds can be used as potential indicators for DT classification, including dihydroactinidiolide, linalool, 1,2,3-trimethoxybenzene, geranyl acetone, 1,2,4-trimethoxybenzene, cedrol, 3,7-dimethyl-1,5,7-octatrien-3-ol, ß-ionone, 4-ethyl-1,2-dimethoxybenzene, methyl salicylate, α-ionone, geraniol, linalool oxide I, linalool oxide II, 6-methyl-5-hepten-2-one, α-terpineol, 1,2,3-trimethoxy-5-methylbenzene, and 1,2-dimethoxybenzene. These compounds provide a certain theoretical basis for distinguishing the differences in five DTs from different geographical regions. This study provides a potential method for identifying the volatile substances in DTs and elucidating the differences in key aroma compounds. Abbreviations: DT, dark tea; FZT, Fuzhuan tea; LPT, Guangxi Liupao tea; QZT, Hubei Qingzhuan tea; TBT, Sichuan Tibetan tea; PET, Yunnan Pu-erh tea; ROAV, Relative odor activity value; OT, Odor threshold; HS-SPME, Headspace solid-phase microextraction; GC-MS, Gas chromatography-mass spectrometry; PCA, Principal components analysis; PLS-DA, Partial least squares-discriminant analysis; HCA, Hierarchical clustering analysis.
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Cromatografía de Gases y Espectrometría de Masas , Odorantes , Microextracción en Fase Sólida , Té , Compuestos Orgánicos Volátiles , Cromatografía de Gases y Espectrometría de Masas/métodos , Compuestos Orgánicos Volátiles/análisis , Odorantes/análisis , Té/química , Microextracción en Fase Sólida/métodos , China , Quimiometría , Camellia sinensis/químicaRESUMEN
Background: Sapota, Manilkara zapota L., are tasty, juicy, and nutrient-rich fruits, and likewise used for several medicinal uses. Methods: The current study represents an integrated metabolites profiling of sapota fruits pulp via GC/MS and UPLC/MS, alongside assessment of antioxidant capacity, pancreatic lipase (PL), and α-glucosidase enzymes inhibitory effects. Results: GC/MS analysis of silylated primary polar metabolites led to the identification of 68 compounds belonging to sugars (74%), sugar acids (18.27%), and sugar alcohols (7%) mediating the fruit sweetness. Headspace SPME-GC/MS analysis led to the detection of 17 volatile compounds belonging to nitrogenous compounds (72%), ethers (7.8%), terpenes (7.6%), and aldehydes (5.8%). Non-polar metabolites profiling by HR-UPLC/MS/MS-based Global Natural Products Social (GNPS) molecular networking led to the assignment of 31 peaks, with several novel sphingolipids and fatty acyl amides reported for the first time. Total phenolic content was estimated at 6.79 ± 0.12 mg gallic acid equivalent/gram extract (GAE/g extract), but no flavonoids were detected. The antioxidant capacities of fruit were at 1.62 ± 0.2, 1.49 ± 0.11, and 3.58 ± 0.14 mg Trolox equivalent/gram extract (TE/g extract) via DPPH, ABTS, and FRAP assays, respectively. In vitro enzyme inhibition assays revealed a considerable pancreatic lipase inhibition effect (IC50 = 2.2 ± 0.25 mg/mL), whereas no inhibitory effect towards α-glucosidase enzyme was detected. This study provides better insight into sapota fruit's flavor, nutritional, and secondary metabolites composition mediating for its sensory and health attributes.
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Antioxidantes , Frutas , Lipasa , Lipasa/antagonistas & inhibidores , Lipasa/metabolismo , Frutas/química , Frutas/metabolismo , Antioxidantes/metabolismo , Cromatografía de Gases y Espectrometría de Masas/métodos , Extractos Vegetales/química , Extractos Vegetales/farmacología , Inhibidores de Glicósido Hidrolasas/farmacología , Cromatografía Líquida de Alta Presión/métodos , Inhibidores Enzimáticos/farmacología , Inhibidores Enzimáticos/química , alfa-Glucosidasas/metabolismo , Espectrometría de Masas en Tándem/métodosRESUMEN
Volatile sulfur compounds (VSCs) are not only important for their therapeutic potential but also significantly influence the flavor profiles of agricultural products. VSCs exhibit various chemical structures due to their stability and volatility, and they may form or be altered as a result of enzymatic and chemical reactions during storage and cooking. This study has focused on profiles of VSCs in 58 different vegetable samples by using HS-SPME-GC/MS technique and chemometric analyses. The validation was carried out using cabbage juice as a vegetable matrix for VSCs analysis, showing satisfactory repeatability (RSD 8.07% ~ 9.45%), reproducibility (RSD 4.22% ~ 7.71%), accuracy and specificity. The established method was utilized on various vegetables, revealing that 21 VSCs such as sulfides, disulfides, trisulfides, isothiocyanates, sulfhydryls, and thiophenes were successfully identified and quantified. These compounds were found in a range of vegetables including Allium species, Cruciferae, Capsicum species, green leafy vegetables, and mushrooms. In particular, isocyanate and allyl groups were abundant in Cruciferae and Allium vegetables, respectively. Cooking conditions were shown to reduce the levels of certain sulfur compounds such as dimethyl sulfide and dimethyl trisulfide in vegetables like broccoli and cabbage, suggesting that heat treatment can lead to the volatilization and reduction of these compounds. The present study provides reliable insights into the compositions of VSCs in various vegetables and examines the changes induced by different cooking methods.
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This work used headspace solid-phase microextraction with gas chromatography-mass spectrometry (HS-SPME-GC-MS) to analyze the volatile components of hydrosols of Citrus × aurantium 'Daidai' and Citrus × aurantium L. dried buds (CAVAs and CADBs) by immersion and ultrasound-microwave synergistic-assisted steam distillation. The results show that a total of 106 volatiles were detected in hydrosols, mainly alcohols, alkenes, and esters, and the high content components of hydrosols were linalool, α-terpineol, and trans-geraniol. In terms of variety, the total and unique components of CAVA hydrosols were much higher than those of CADB hydrosols; the relative contents of 13 components of CAVA hydrosols were greater than those of CADB hydrosols, with geranyl acetate up to 15-fold; all hydrosols had a citrus, floral, and woody aroma. From the pretreatment, more volatile components were retained in the immersion; the relative contents of linalool and α-terpineol were increased by the ultrasound-microwave procedure; and the ultrasound-microwave procedure was favorable for the stimulation of the aroma of CAVA hydrosols, but it diminished the aroma of the CADB hydrosols. This study provides theoretical support for in-depth exploration based on the medicine food homology properties of CAVA and for improving the utilization rate of waste resources.
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Monoterpenos Acíclicos , Citrus , Monoterpenos Ciclohexánicos , Cromatografía de Gases y Espectrometría de Masas , Microextracción en Fase Sólida , Compuestos Orgánicos Volátiles , Cromatografía de Gases y Espectrometría de Masas/métodos , Citrus/química , Microextracción en Fase Sólida/métodos , Compuestos Orgánicos Volátiles/análisis , Compuestos Orgánicos Volátiles/química , Compuestos Orgánicos Volátiles/aislamiento & purificación , Monoterpenos Acíclicos/análisis , Monoterpenos Ciclohexánicos/análisis , Terpenos/análisis , Terpenos/química , Monoterpenos/análisis , Monoterpenos/aislamiento & purificación , Odorantes/análisis , Destilación/métodos , AcetatosRESUMEN
Chardonnay is one of the most popular white grape wine varieties in the world, but this wine lacks typical aroma, considered a sensory defect. Our research group identified a Chardonnay bud sport with typical muscat characteristics. The goal of this work was to discover the key candidate genes related to muscat characteristics in this Chardonnay bud sport to reveal the mechanism of muscat formation and guide molecular design breeding. To this end, HS-SPME-GC-MS and RNA-Seq were used to analyze volatile organic compounds and the differentially expressed genes in Chardonnay and its aromatic bud sport. Forty-nine volatiles were identified as potential biomarkers, which included mainly aldehydes and terpenes. Geraniol, linalool, and phenylacetaldehyde were identified as the main aroma components of the mutant. The GO, KEGG, GSEA, and correlation analysis revealed HMGR, TPS1, TPS2, TPS5, novel.939, and CYP450 as key genes for terpene synthesis. MAO1 and MAO2 were significantly downregulated, but there was an increased content of phenylacetaldehyde. These key candidate genes provide a reference for the development of functional markers for muscat varieties and also provide insight into the formation mechanism of muscat aroma.
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Metaboloma , Odorantes , Transcriptoma , Compuestos Orgánicos Volátiles , Odorantes/análisis , Compuestos Orgánicos Volátiles/metabolismo , Compuestos Orgánicos Volátiles/análisis , Vitis/genética , Vitis/química , Vitis/metabolismo , Vino/análisis , Terpenos/metabolismo , Perfilación de la Expresión Génica , Monoterpenos Acíclicos/metabolismo , Regulación de la Expresión Génica de las Plantas , Cromatografía de Gases y Espectrometría de Masas , Acetaldehído/análogos & derivados , Acetaldehído/metabolismo , Monoaminooxidasa/genética , Monoaminooxidasa/metabolismoRESUMEN
Fifty-six samples of differently produced commercial Italian ciders were analysed for semi-volatile organic compounds (SVOCs) profiling, using comprehensive two-dimensional gas chromatography coupled to mass spectrometry (GC×GC-TOF-MS) technique for the very first time. To properly support the compositional investigation of this emerging beverage, a chemometric approach through Principal Component Analysis (PCA) was employed. This revealed a sample distribution in agreement with results of the sensory tasting panel performed on such ciders, highlighting an excellent correlation between variables and perceived odorants. In particular, the positions of peculiar and anomalous objects in the Principal Components (PCs) space are explicitly evaluated, exploring the associated loadings (i.e., the importance of the identified chemical compounds), paying attention to their biochemical origin along the cider-making process and their impact on the sample olfactory analysis. Besides this, the t-distributed Stochastic Neighbor Embedding (t-SNE) method was shown to be an efficient tool for gathering pear ciders from the other samples (apple ciders), better than PCA. This study stands for the first survey on Italian commercial craft cider, and its results are aimed to be a milestone for its characterization and to start and promote cider culture in this country.
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The authenticity of salted goose products is concerning for consumers. This study describes an integrated deep-learning framework based on a generative adversarial network and combines it with data from headspace solid phase microextraction/gas chromatography-mass spectrometry, headspace gas chromatography-ion mobility spectrometry, E-nose, E-tongue, quantitative descriptive analysis, and free amino acid and 5'-nucleotide analyses to achieve reliable discrimination of four salted goose breeds. Volatile and non-volatile compounds and sensory characteristics and intelligent sensory characteristics were analyzed. A preliminary composite dataset was generated in InfoGAN and provided to several base classifiers for training. The prediction results were fused via dynamic weighting to produce an integrated model prediction. An ablation study demonstrated that ensemble learning was indispensable to improving the generalization capability of the model. The framework has an accuracy of 95%, a root mean square error (RMSE) of 0.080, a precision of 0.9450, a recall of 0.9470, and an F1-score of 0.9460.
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This study aimed to investigate the effect of vacuum freeze drying combined with catalytic infrared drying (FD-CIRD) process on aromas, free amino acids, reducing sugars and free fatty acids in chive leaves and stems. Gas chromatography-mass spectrometry combined with multivariate data analysis revealed that dipropyl disulfide was the key aroma that distinguished the differences between chive leaves and stems. The key aromas benzeneacetaldehyde, decanal and 1-octen-3-ol enhanced FD-CIRD chive leaves and stems aromas. The free amino acid content was highest at FD-CIRD stage in all samples except for the control (FD), while the reducing sugar content was lowest. The content of unsaturated fatty acids gradually decreased at FD stage and increased at FD-CIRD stage. Additionally, correlation analysis revealed that phenylalanine was a potential precursor of benzacetenealdehyde, oleic and linolenic acids were potential precursors of decanal and 1-octen-3-ol. Therefore, FD-CIRD technique helps to improve the sensory profile of dried chives.
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Xijiao Huojiu (Xijiao), an ancient Chinese rice wine (ACRW), is produced using traditional methods, which involve biological-ageing-like process and result in distinctive sensory profiles. However, its aroma composition is still unclear. In this study, the aroma characteristics of three samples with varying ageing times were examined. Xijiao_SCT, with a short cellar time, exhibited a strong fruity and floral aroma and a less grain-like aroma. Conversely, Xijiao_LCT, which had a long cellar time, had a deep cocoa- and caramel-like aroma. A total of 27 key odorants that greatly influenced the aroma characteristics of Xijiao were identified. Comparative studies were used to identify 12 key odorants that distinguish Xijiao from modern Chinese rice wine (MCRW) and grape wines (GW). Additionally, 13 dominant latent ageing markers differentiated Xijiao_SCT from Xijiao_LCT. Our results suggested that ACRW and MCRW have overlapping but distinct volatile metabolomic profiles, highlighting the characteristics of ACRW during ageing process.
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Two firewood species (beech and olive) were used for grilling three meat types (lamb, pork, and veal) to assess their influence on the sensorial properties of meat. A multimethod approach was adopted, including sensory evaluation with consumers and two analytical techniques to characterize the volatile fraction (Solid-Phase Micro-Extraction Gas Chromatography-Mass Spectrometry [SPME-GC/MS] and electronic nose [e-nose]). The sensory session included three pairwise preference tests (one for each type of meat), an overall liking test, a Rate-All-That-Apply test, and a questionnaire on the interest and perceived value of using sustainably certified firewood in food preparation. The firewood species significantly affected the perception of a few crucial attributes. In particular, olive wood increased the roasted meat flavor perception in lamb and veal, while beech wood increased the perceived intensity of a vegetable/herbaceous flavor in veal. No effect of firewood was observed on preference within each pair of meat samples. Lamb was the significantly most liked meat by consumers, followed by pork; veal was the least liked meat type. Positive and negative drivers of preference were discussed. 36 volatile organic compounds were identified from SPME-GC/MS in meats. Congruently with sensory data, the two veal samples showed a greater distance in terms of volatile composition. Relative distances among samples on maps obtained from SPME-GC/MS and the e-nose were similar. This multi-method approach innovatively showed the potential of using firewood as a 'gastronomic' tool to sensorially characterize and valorize cooked meat.
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Comportamiento del Consumidor , Culinaria , Cromatografía de Gases y Espectrometría de Masas , Gusto , Compuestos Orgánicos Volátiles , Madera , Animales , Humanos , Culinaria/métodos , Compuestos Orgánicos Volátiles/análisis , Adulto , Masculino , Madera/química , Femenino , Adulto Joven , Porcinos , Ovinos , Persona de Mediana Edad , Microextracción en Fase Sólida/métodos , Carne de Cerdo/análisis , Nariz Electrónica , Carne/análisis , Carne Roja/análisis , Olea/química , Odorantes/análisis , Preferencias AlimentariasRESUMEN
Coffee, one of the most widely consumed commodities globally, embodies a sensory experience deeply rooted in social, cultural, and hedonic contexts. The cold brew (CB) method, characterized by cold extraction, is a refreshing and unique alternative to traditional coffee. Despite its growing popularity, CB lacks defined preparation parameters and comprehensive analysis of its aromatic composition. In this study, we aimed to obtain a representative extract of the volatile matrix of CB and characterize the aroma of sensory-active compounds using advanced techniques such as headspace-solid-phase Microextraction (HS-SPME) and headspace-solid-phase extraction (HS-SPE) for volatile compound extraction, followed by gas chromatography-olfactometry-mass Spectrometry (GC-O-MS) for compound identification. Optimization of the HS-SPME parameters resulted in the identification of 36 compounds, whereas HS-SPE identified 28 compounds, which included both complementary and similar compounds. In HS-SPME, 15 compounds exhibited sensory activity with descriptors such as floral, caramel, sweet, and almond, whereas seven exhibited sensory activity with descriptors such as chocolate, floral, coffee, and caramel. This comprehensive approach to HS-SPME and HS-SPE aroma extraction with GC-O-MS offers an efficient methodology for characterizing the aroma profile of CB, paving the way for future research and quality standards for this innovative coffee beverage.
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Lower urinary tract inflammation is a very common problem which occurs particularly in women. That is why the idea of a biotextronics system for preventive and supportive treatment came to be. The system is a kind of a therapeutic clothing in the form of underwear integrated with a four-layer pantiliner with biological active compounds (from chamomile essential oil) immobilized on the insert with a cellulose agar or microcrystalline cellulose agar film. In this research, the outer part of the insert was investigated for its ability to release compounds with antibacterial and anti-inflammatory activity under the temperature of the treatment (40 °C). The research was conducted on the day of the insert preparation (day 0) and also after 7, 14, 28, and 56 days to test the ability of the insert to be stored without changing its properties. The results showed that even after 56 days of storage, there are compounds released that are known to have antibacterial activity, such as α-bisabolol. The system requires further tests involving bacteria; however, chamomile essential oil seems to be good substrate for biotextronics systems for preventive and supportive treatment of lower urinary tract inflammations.
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Steamed bread is a traditional staple food in China, and it has gradually become loved by people all over the world because of its healthy production methods. With the improvement in people's living standards, the light flavor of steamed bread fermented by single yeast cannot meet people's needs. Multi-strain co-fermentation is a feasible way to improve the flavor of steamed bread. Here, the dynamic change profiles of volatile substances in steamed bread co-fermented by Saccharomyces cerevisiae SQJ20 and Wickerhamomyces anomalus GZJ2 were analyzed using the electronic nose (E-nose) and headspace solid-phase microextraction combined with gas chromatography-mass spectrometry (HS-SPME-GC-MS). The five detectors of the E-nose rapidly detected the changes in volatile substances in different dough or steamed bread with the highest response value in co-fermented dough. A total of 236 volatile substances were detected in all the samples using HS-SPME-GC-MS, and alcohols were the most variable component, especially Phenylethyl alcohol. Significantly, more alcohols and esters were upregulated in co-fermented dough, and the addition of W. anomalus GZJ2 improved the key volatile aroma compounds of steamed bread using the relative odor activity value method (ROAV), especially the aldehydes and alcohols. Moreover, these key volatile aroma compounds can be quickly distinguished using the W2S detector of the E-nose, which can be used for the rapid detection of aroma components in steamed bread.
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The olive oil from the Royal cultivar has not been studied in depth, especially its relationship between analytical and sensory parameters. Currently, it is a minority cultivar, but due to its excellent organoleptic properties, it is constantly growing. The research objective is to obtain excellent-quality olive oil from the Royal cultivar at an industrial extraction plant and characterize the oil sensory and analytically. For this purpose, three important factors were set: very early olives; very low-time olive paste malaxation; and environmental temperature. The analytical parameters studied were volatile and phenolic compounds, fatty acids, photosynthetic pigments, and other quality parameters. Fourteen phenolic compounds were identified and found in significantly higher concentrations in Royal olive oil, including the oleacein compound. Moreover, volatile compounds from the LOX pathway, such as hexenal, (E)-2-hexenal, and (Z)-3-hexen-1-ol, had significantly higher concentrations, which were related to organoleptic characteristics: very fruity, not very spicy, and very low bitterness. The highest values obtained were 74.98% extraction efficiency at 30 min; 71.31 mg/kg chlorophyll content at 30 min; 156.38 mg/kg phenolic compound at 30 min; 18.98 mg/kg volatile compounds at 15 min; and better organoleptic characteristics at 15 min. The oil extraction efficiency was lower than that of other olive cultivars; nevertheless, the content of volatile compounds is higher.
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Wheat starch fermentation slurry is the main substrate for producing Ganmianpi, a traditional Chinese fermented wheat starch-based noodle. In the present work, the microbial population dynamics and metabolite changes in wheat starch fermentation slurry at different fermentation times (0, 1, 2, 3, and 4 days) were measured by using high-throughput sequencing analysis and headspace solid-phase microextraction gas chromatography-mass spectrometry (HS-SPME/GC-MS) methods. The texture and sensory properties of Ganmianpi made from fermented starch slurry are also evaluated. The results showed that Latilactobacillus curvatus and Leuconostoc citreum were the dominant bacteria in wheat starch fermentation slurry, while Saccharomyces cerevisiae and Kazachstania wufongensis were identified as the main species of fungi. With the extension of fermentation time, the reducing sugar content first increased and then decreased, when the titratable acidity content showed an increasing trend, and the nonvolatile acid was significantly higher than the volatile acid. A total of 62 volatile flavor compounds were identified, and the highest content is alcohols, followed by acids. Fermentation significantly reduced the hardness and chewiness of Ganmianpi, and increased its resilience and cohesiveness. Ganmianpi made from fermented starch slurry for two and three days showed a higher sensory score than other samples. The present study is expected to provide a theoretical basis for exploiting the strains with potential for commercial application as starter cultures and quality improvement of Ganmianpi.
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Phthalate esters (PAEs) are used as additives to enhance the pliability and malleability of plastics. These substances frequently migrate from packaging materials to vegetable oils because of the absence of covalent bonds. Over time, this migration could result in the accumulation of PAEs in the human body through ingestion, contributing to various diseases. Therefore, accurate qualitative and quantitative analyses of PAEs in vegetable oils are imperative to assess the origins of contamination and investigate their toxicity, degradation, migration, and transformation patterns. However, the concentration of PAEs in most samples is low, and the composition of vegetable oils is complex. Thus, PAEs must be enriched and purified using appropriate sample pretreatment procedures before analysis. Common methods for pretreating PAEs in oil include solid-phase extraction (SPE), dispersive SPE, and magnetic SPE. These techniques require time-consuming and labor-intensive procedures such as oil dissolution, solvent extraction, and degreasing. These approaches also require numerous solvents and containers, increasing the risk of sample cross-contamination. Solid-phase microextraction (SPME) integrates sampling, extraction, purification, concentration, and injection into a single process, significantly accelerating analytical testing and reducing the potential for sample cross-contamination. In headspace (HS) mode, the analytes achieve equilibrium on the coating and are extracted in the gas phase. The fibers are shielded from nonvolatile and high-relative molecular mass substances in the sample matrix. Thus, SPME is an ideal method for extracting volatile compounds in vegetable oils. When HS-SPME coupled with gas chromatography-mass spectrometry (GC-MS), it can achieve the rapid screening of PAEs in vegetable oil. In this study, an SPME with cyclodextrin-based hypercrosslinked polymers (BnCD-HCP) coated on stainless steel fibers was employed to extract PAEs from vegetable oil. The structure and morphology of the polymers were characterized using Fourier-transform infrared spectroscopy, nuclear magnetic spectroscopy, and scanning electron microscopy. BnCD-HCP exhibited high stability and diverse interactions, including π-π, hydrophobic, and host-guest interactions. The oil samples were incubated with methanol, and the PAEs were extracted from the headspace using the probe. The optimal extraction parameters included an extraction time of 20 min, extraction temperature of 50 â, desorption time of 4 min, and desorption temperature of 275 â. The BnCD-HCP/HS-SPME method was evaluated under optimized experimental conditions. The limits of detection (LODs) and quantification (LOQs) were determined by applying signal-to-noise ratios (S/N) of 3 and 10, respectively. Method accuracy was evaluated using relative standard deviations (RSDs). Single-needle precision was evaluated by conducting three consecutive analyses at 3 h intervals within a day. Inter-needle precision was assessed by conducting the same analyses (three replicates) with differently coated fibers. The 12 PAE compounds exhibited good linearity with correlation coefficients (R2) of at least 0.99. The LODs and LOQs ranged from 0.21 to 3.74 µg/kg and from 0.69 to 12.34 µg/kg, respectively. The RSDs were in the range of 1.8%-11.4% and 5.1%-13.9% for the single-needle and needle-to-needle methods, respectively. The proposed method was applied to soybean, peanut, and sunflower oils, and two PAEs were found in all three oils. Moreover, the method demonstrated good precision (RSD=1.17%-11.73%) and recoveries (72.49%-124.43%). Compared with other methods, the developed method was able to extract many target analytes and had a low or comparable LOD and high recovery. More importantly, this method does not require tedious operations such as solvent extraction and purification. Consequently, the developed method can be used to extract not only PAEs in oils but also other substances with a high lipid content.
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Ésteres , Cromatografía de Gases y Espectrometría de Masas , Ácidos Ftálicos , Aceites de Plantas , Microextracción en Fase Sólida , Aceites de Plantas/química , Ácidos Ftálicos/análisis , Ésteres/análisis , Ésteres/química , Microextracción en Fase Sólida/métodos , Polímeros/química , Contaminación de Alimentos/análisisRESUMEN
Volatile organic compounds (VOCs) are continuously emitted into the atmosphere from natural and anthropogenic sources and rapidly spread from the atmosphere to different environments. A large group of VOCs has been included in the class of air pollutants; therefore, their determination and monitoring using reliable and sensitive analytical methods represents a key aspect of health risk assessment. In this work, an untargeted approach is proposed for the evaluation of the exposure to volatile organic compounds of workers in an engine manufacturing plant by GC-MS measurements, coupled with solid-phase microextraction (SPME). The analytical procedure was optimized in terms of SPME fiber, adsorption time, desorption time, and temperature gradient of the chromatographic run. For the microextraction of VOCs, the SPME fibers were exposed to the air in two different zones of the manufacturing factory, i.e., in the mixing painting chamber and the engine painting area. Moreover, the sampling was carried out with the painting system active and running (system on) and with the painting system switched off (system off). Overall, 212 compounds were identified, but only 17 were always present in both zones (mixing painting chamber and engine painting area), regardless of system conditions (on or off). Finally, a semi-quantitative evaluation was performed considering the peak area value of the potentially most toxic compounds by multivariate data analyses.
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Contaminación del Aire Interior , Monitoreo del Ambiente , Cromatografía de Gases y Espectrometría de Masas , Microextracción en Fase Sólida , Compuestos Orgánicos Volátiles , Compuestos Orgánicos Volátiles/análisis , Contaminación del Aire Interior/análisis , Monitoreo del Ambiente/métodos , Contaminantes Atmosféricos/análisis , Humanos , Lugar de Trabajo , Condiciones de TrabajoRESUMEN
This investigation explores the impact of various fermentation techniques and the inoculation of Bacillus subtilis spores on the physicochemical properties and principal flavor profiles of Huangjiu. Employing sensory analysis, headspace solid-phase microextraction, gas chromatography-tandem mass spectrometry (HS-SPME-GC-MS), and orthogonal partial least squares discriminant analysis (OPLS-DA), we observed that these variables significantly alter the physicochemical attributes of Huangjiu. Our analysis, integrating volatile organic compounds (VOCs) with odor activity values (OAV), revealed that while B. subtilis inoculation modifies the concentrations of key flavor compounds, it does not affect their types. Notably, the inoculation enhances the concentrations of 13 primary flavor compounds, thereby enriching floral and fruity notes while reducing higher alcohol levels. These findings contribute valuable insights into the flavor formation mechanisms of Huangjiu and guide the optimization of fermentation processes.