Solid-phase Microextraction-gas Chromatography-mass Spectrometry Research Articles

Tracking dry gin volatile organic compounds over distillation: a time course study

Why was the work done: The influence of distillation time on the volatile composition of gin has not been examined in detail at a commercial distillery. How was the work done: Headspace Solid-Phase Micro-Extraction Gas Chromatography-Mass Spectrometry (HS-SPME-GC-MS) was used to tentatively identify 74 aroma compounds, with their concentration tracked in distillate samples over the course of three gin distillations. What are the main findings: Four unique fractions were identified using Agglomerative Hierarchical Clustering: ‘heads’, ‘early hearts’, ‘late hearts, and ‘tails’. The hearts fraction (n=24 samples) was examined further, fitting statistically appropriate models to 54 aroma volatiles. Three sub-groups of volatiles were identified, (i) highly volatile monoterpenes with rapidly decreasing concentration over the early hearts fraction, (ii) volatiles whose concentration increased gradually over the hearts fraction and (iii) less volatile sesquiterpenes, sesquiterpenoids, and monoterpenoids which increased rapidly in concentration in the later distillate. Complex cubic models fit 34 volatiles with very high significance (p>0.0001) over the hearts fraction (72%). Informal aroma sensory bench testing identified distinct aroma categories with, for example, ‘Spicy’ being commonly detected in the later distillate. Why is the work important: This investigation characterises the kinetics of flavour extraction over the course of a commercial gin distillation process. These findings highlight the potential for the expression of specific flavour characteristics by modifying the cut points of the distillation process

Detection of Volatile Compounds and Their Contribution to the Nutritional Quality of Chinese and Japanese Welsh Onions (Allium fistulosum L.)

Allium vegetables attract attention for their flavor and aroma in Asia, especially in China and Japan. The aim of this experiment was to uncover the differences in the unique flavor compounds of two Welsh onions that are typical cultivars in China and Japan (‘Zhangqiu’ and ‘Tenko’). Chemical methods and solid-phase microextraction–gas chromatography-mass spectrometry were performed to determine the nutritional quality and quantity of volatile compounds of various organs of Welsh onions. The results show that a total of 30, 37, and 28 compounds were detected in the roots, pseudostem, and leaves of ‘Zhangqiu’, respectively, while 21, 27, and 20 compounds were detected in the corresponding organs of ‘Tenko’. The distribution of sulfur compounds in the roots, pseudostem, and leaves of ‘Zhangqiu’ accounted for 72%, 83%, and 26% of the total content, while those of ‘Tenko’ accounted for 55%, 84%, and 57%, respectively. Aldehydes are the second largest class of volatiles in Welsh onions. The distribution of aldehydes in the leaves was notably different: 52% and 27% in ‘Zhangqiu’ and ‘Tenko’, respectively. The contribution of S to the volatile substances was outstanding, and through forward selection, it was found that P, Ca, and Mg contribute to the volatile substances of Welsh onions. The above results indicate that the different genotypes of Welsh onions have various flavors, and mineral elements contribute variously to these flavors. Calcium could be a new topic of interest for our subsequent research on elements and volatiles.

Impact of storage time on microbial communities and flavor profiles in highland barley grains

Microbial activity and the resulting flavor changes in stored highland barley grains may reduce the product quality and pose potential risks to food safety with economic losses. This study aims to elucidate the association between microbial load and flavor compounds during the preservation of highland barley. High-throughput sequencing (HTS) was used to investigate the microbial composition in stored highland barley. The volatile flavor components of the latter were identified via the headspace solid-phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS). Moreover, the study examined the correlation between the types of microorganisms and volatile flavor molecules. The results indicated that the dominant phyla in highland barley were Ascomycota and Basidiomycota, with the dominant genera being Cladosporium, Vishniacozyma, Filobasidium, Udeniomyces, Cystofilobasidium, Aspergillus, Alternaria, Monographella, Didymella, and Neoascochyta. Inside，Cystofilobasidium, Itersonilia, Sarocladium, Ustilago, Penicillium and Pyrenophora served as effective biomarkers to distinguish highland barley grains stored at different times. Further, the highland barley samples contained 192 volatile organic compounds (VOCs), such as alcohols, ketones, esters, alkanes, aldehydes, etc. The top 20 volatile flavor compounds with differences were selected based on the variable importance of projection (VIP) > 1. Based on the correlation analysis findings, it was found that the genera Cystofilobasidium, Aspergillus, and Cladosporium hold promise in contributing volatile flavor compounds to highland barley. This study examined a pattern of changes in safety and quality across varying storage durations, providing crucial insights to enhance the flavor profile and texture of highland barley products.

Detection and Analysis of VOCs in Cherry Tomato Based on GC-MS and GC×GC-TOF MS Techniques.

Volatile organic compounds (VOCs) play a significant role in influencing the flavor quality of cherry tomatoes (Solanum lycopersicum var. cerasiforme). The scarcity of systematic analysis of VOCs in cherry tomatoes can be attributed to the constraints imposed by detection technology and other contributing factors. In this study, the cherry tomato cultivar var. 'Zheyingfen1' was chosen due to its abundant fruit flavor. Two detection technology platforms, namely the commonly employed headspace solid-phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) and the most advanced headspace solid-phase microextraction-full two-dimensional gas chromatography-time-of-flight mass spectrometry (HS-SPME-GC×GC-TOFMS), were employed in the analysis. The VOCs of cherry tomato cultivar var. 'Zheyingfen1' fruits at red ripening stage were detected. A combined total of 1544 VOCs were detected using the two aforementioned techniques. Specifically, 663 VOCs were identified by through the HS-SPME-GC-MS method, 1026 VOCs were identified by through the HS-SPME-GC×GC-TOFMS, and 145 VOCs were identified by both techniques. The identification of β-ionone and (E)-2-nonenal as the principal VOCs was substantiated through the application of the relative odor activity value (rOAV) calculation and subsequent analysis. Based on the varying contribution rates of rOAV, the analysis of sensory flavor characteristics revealed that cherry tomato cultivar var. 'Zheyingfen1' predominantly exhibited green and fatty attributes, accompanied by elements of fresh and floral flavor characteristics. In conclusion, our study conducted a comprehensive comparison of the disparities between these two methodologies in detecting VOCs in cherry tomato fruits. Additionally, we systematically analyzed the VOC composition and sensory flavor attributes of the cherry tomato cultivar var. 'Zheyingfen1'. This research serves as a significant point of reference for investigating the regulatory mechanisms underlying the development of volatile flavor quality in cherry tomatoes.

Discrimination and screening of volatile metabolites in atractylodis rhizoma from different varieties using headspace solid-phase microextraction-gas chromatography-mass spectrometry and headspace gas chromatography-ion mobility spectrometry, and ultra-fast gas chromatography electronic nose

Atractylodis rhizoma is a common bulk medicinal material with multiple species. Although different varieties of atractylodis rhizoma exhibit variations in their chemical constituents and pharmacological activities, they have not been adequately distinguished due to their similar morphological features. Hence, the purpose of this research is to analyze and characterize the volatile organic compounds (VOCs) in samples of atractylodis rhizoma using multiple techniques and to identify the key differential VOCs among different varieties of atractylodis rhizoma for effective discrimination. The identification of VOCs was carried out using headspace solid-phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC–MS) and headspace gas chromatography-ion mobility spectrometry (HS-GC-IMS), resulting in the identification of 60 and 53 VOCs, respectively. The orthogonal partial least squares discriminant analysis (OPLS-DA) model was employed to screen potential biomarkers and based on the variable importance in projection (VIP ≥ 1.2), 24 VOCs were identified as critical differential compounds. Random forest (RF), K-nearest neighbor (KNN) and back propagation neural network based on genetic algorithm (GA-BPNN) models based on potential volatile markers realized the greater than 90 % discriminant accuracies, which indicates that the obtained key differential VOCs are reliable. At the same time, the aroma characteristics of atractylodis rhizoma were also analyzed by ultra-fast gas chromatography electronic nose (Ultra-fast GC E-nose). This study indicated that the integration of HS-SPME-GC–MS, HS-GC-IMS and ultra-fast GC E-nose with chemometrics can comprehensively reflect the differences of VOCs in atractylodis rhizoma samples from different varieties, which will be a prospective tool for variety discrimination of atractylodis rhizoma.

Volatile Compounds for Discrimination between Beef, Pork, and Their Admixture Using Solid-Phase-Microextraction-Gas Chromatography-Mass Spectrometry (SPME-GC-MS) and Chemometrics Analysis.

This study addresses the prevalent issue of meat species authentication and adulteration through a chemometrics-based approach, crucial for upholding public health and ensuring a fair marketplace. Volatile compounds were extracted and analyzed using headspace-solid-phase-microextraction-gas chromatography-mass spectrometry. Adulterated meat samples were effectively identified through principal component analysis (PCA) and partial least square-discriminant analysis (PLS-DA). Through variable importance in projection scores and a Random Forest test, 11 key compounds, including nonanal, octanal, hexadecanal, benzaldehyde, 1-octanol, hexanoic acid, heptanoic acid, octanoic acid, and 2-acetylpyrrole for beef, and hexanal and 1-octen-3-ol for pork, were robustly identified as biomarkers. These compounds exhibited a discernible trend in adulterated samples based on adulteration ratios, evident in a heatmap. Notably, lipid degradation compounds strongly influenced meat discrimination. PCA and PLS-DA yielded significant sample separation, with the first two components capturing 80% and 72.1% of total variance, respectively. This technique could be a reliable method for detecting meat adulteration in cooked meat.

Identification of key off-flavor compounds during storage of fried pepper (Zanthoxylum bungeanum Maxim.) oils by sensory-directed flavor analysis and partial least squares regression (PLSR)

Fried pepper oil (FPO) is a widely used flavoring oil in China, but it suffers from complex chemical reactions that give an unpleasant odor. The aim of this paper is to study the main causes of off-flavor in FPO, as well as identify key off-flavor compounds in FPO. Fifty-eight volatiles were identified using HS-SPME–GC–MS (headspace solid-phase microextraction–gas chromatography–mass spectrometry) during storage. Fifteen off-flavor compounds were initially targeted by odor activity values (OAVs) calculations and partial least squares regression (PLSR) analysis. Eventually, five key off-flavor compounds were identified by recombination experiments and omission test, which were hexanal, (E)-2-octenal, terpinyl acetate, α-terpineol, and hexanoic acid. The off-flavors could derive from the oxidative degradation of long-chain fatty acids and the acid-catalyzed rearrangement of terpenes. The results of the study provide a theoretical basis for the regulation of off-flavor in FPO and a practical guide for the industrial production of FPO.

Enhancing the Quality of Low-Alcohol Navel Orange Wine through Simultaneous Co-Fermentation Using Saccharomyces cerevisiae SC-125, Angel Yeast SY, and Lactiplantibacillus plantarum BC114.

To date, there has been limited research on the interactive effects of yeast and lactic acid bacteria (LAB) on the sensory qualities of navel orange wine. In this study, using Jintang navel orange juice as the raw material, multi-microbial fermentation was conducted with Saccharomyces cerevisiae SC-125 and Angel yeast SY, as well as Lactiplantibacillus plantarum BC114. Single yeast and co-fermentation with Lactiplantibacillus plantarum were used as the control groups. The research aimed to investigate the physicochemical parameters of navel orange wine during fermentation. Additionally, headspace solid-phase microextraction gas chromatography-mass spectrometry (HP-SPME-GC-MS) was employed to determine and analyze the types and levels of flavor compounds in the navel orange wines produced through the different fermentation methods. The co-fermentation using the three strains significantly enhanced both the quantity and variety of volatile compounds in the navel orange wine, concomitant with heightened total phenol and flavonoid levels. Furthermore, a notable improvement was observed in the free radical scavenging activity. A sensory evaluation was carried out to analyze the differences among the various navel orange wines, shedding light on the impact of different wine yeasts and co-fermentation with LAB on the quality of navel orange wines.

Evolution of volatile compounds of baked dried tofu during catalytic infrared baking process and their correlation with relevant physicochemical properties.

Energy-saving and low-carbon baking processes, as well as the need to determine the flavor-forming mechanisms of baked dried tofu, are becoming increasingly necessary. The application of emerging catalytic infrared radiation (CIR) technology in baking of dried tofu is considered of high interest due to the low energy consumption and high baking efficiency compared to traditional baking methods. Hence, this study aimed to investigate the evolution of aroma compounds in baked dried tofu during the CIR baking process and reveal relevant relationships between physical qualities, potential flavor precursors and key volatile compounds. The results showed that the surface color of dried tofu gradually turned an appetizing golden yellow color during the rapid heating process, caused by the uniform infrared radiation from the radiant emitters. Meanwhile, the moisture of dried tofu experienced minimal reduction and the hardness of dried tofu gradually increased with the formation of crust on the surface. In addition, 49 volatile compounds were identified by headspace solid-phase microextraction-gas chromatography-mass spectrometry and 13 substances - 1-hexanol, 1-octen-3-ol, 1-pentanol, heptanal, nonanal, hexanal, (E,E)-2,4-decadienal, (E,Z)-2,4-decadienal, octanal, (E)-2-octenal, (E)-2-nonenal, 2-heptanone and 2-pentylfuran - were confirmed as key aroma compounds. Moreover, the amino acids aspartic acid, glutamic acid, isoleucine, lysine and arginine, and the fatty acids butyric, caprylic, capric, tridecanoic, stearic, oleic and linolenic were responsible for the unique flavor of CIR-baked dried tofu. Consequently, the findings can provide a scientific basis for manufacturers to achieve precise quality control and large-scale production of CIR-baked dried tofu products. © 2024 Society of Chemical Industry.

Improvement mechanism of volatile flavor in fermented tilapia surimi by cooperative fermentation of Pediococcus acidilactici and Latilactobacillus sakei: Quantization of microbial contribution through influence of genus

Single starter can hardly improve the volatile flavor of fermented fish surimi. In this study, the changes of volatile compounds (VCs) and microbial composition during cooperative fermentation of Latilactobacillus sakei and Pediococcus acidilactici were studied by headspace solid-phase microextraction gas chromatography–mass spectrometry and 16S rRNA gene high-throughput sequencing. During cooperative fermentation, most VCs and the abundance of Latilactobacillus and Lactococcus significantly increased, while Pediococcus, Acinetobacter, and Macrococcus obviously decreased. After evaluation of correlation and abundance of each genus, Latilactobacillus and Lactococcus possessed the highest influence on the formation of volatile flavor during cooperative fermentation. Compared with the natural fermentation, cooperative fermentation with starters significantly enhanced most of pleasant core VCs (odor activity value≥1), but inhibited the production of trimethylamine and methanethiol, mainly resulting from the absolutely highest influence of Latilactobacillus. Cooperative fermentation of starters is an effective method to improve the volatile flavor in the fermented tilapia surimi.

The role of volatile organic compounds for assessing characteristics and severity of non-cystic fibrosis bronchiectasis: an observational study.

Hypoxic conditions and Pseudomonas aeruginosa (P. aeruginosa) infection are significant factors influencing the prognosis and treatment of patients with bronchiectasis. This study aimed to explore the potential for breath analysis to detect hypoxic conditions and P. aeruginosa infection in bronchiectasis patients by analyzing of volatile organic compounds (VOCs) in exhaled breath condensate (EBC). EBC samples were collected from stable bronchiectasis patients and analyzed using solid phase microextraction-gas chromatography-mass spectrometry (SPME-GCMS). The association of VOCs with bronchiectasis patients' phenotypes including hypoxic conditions and P. aeruginosa isolation was analyzed, which may relate to the severity of bronchiectasis disease. Levels of 10-heptadecenoic acid, heptadecanoic acid, longifolene, and decanol in the hypoxia group were higher compared to the normoxia group. Additionally, the levels of 13-octadecenoic acid, octadecenoic acid, phenol, pentadecanoic acid, and myristic acid were increased in P. aeruginosa (+) group compared to the P. aeruginosa (-) group. Subgroup analysis based on the bronchiectasis severity index (BSI)reveled that the levels of 10-heptadecenoic acid, heptadecanoic acid, decanol, 13-octadecenoic acid, myristic acid, and pentadecanoic acid were higher in the severe group compared to the moderate group. Multivariate linear regression showed that 10-heptadecenoic acid and age were independent prognostic factors for bronchiectasis patients with hypoxia. Furthermore, octadecenoic acid, phenol and gender were identified as independent prognostic factors for bronchiectasis patients with P. aeruginosa isolation. The study provides evidence that specific VOCs in EBC are correlated with the severity of bronchiectasis, and 10-heptadecenoic acid is shown to be a predictive marker for hypoxia condition in bronchiectasis patients.

Detection of Maize Mold Based on a Nanocomposite Colorimetric Sensor Array under Different Substrates.

This study developed a novel nanocomposite colorimetric sensor array (CSA) to distinguish between fresh and moldy maize. First, the headspace solid-phase microextraction gas chromatography-mass spectrometry (HS-SPME-GC/MS) method was used to analyze volatile organic compounds (VOCs) in fresh and moldy maize samples. Then, principal component analysis and orthogonal partial least-squares discriminant analysis (OPLS-DA) were used to identify 2-methylbutyric acid and undecane as key VOCs associated with moldy maize. Furthermore, colorimetric sensitive dyes modified with different nanoparticles were employed to enhance the dye properties used in the nanocomposite CSA analysis of key VOCs. This study focused on synthesizing four types of nanoparticles: polystyrene acrylic (PSA), porous silica nanospheres (PSNs), zeolitic imidazolate framework-8 (ZIF-8), and ZIF-8 after etching. Additionally, three types of substrates, qualitative filter paper, polyvinylidene fluoride film, and thin-layer chromatography silica gel, were comparatively used to fabricate nanocomposite CSA combining with linear discriminant analysis (LDA) and K-nearest neighbor (KNN) models for real sample detection. All moldy maize samples were correctly identified and prepared to characterize the properties of the CSA. Through initial testing and nanoenhancement of the chosen dyes, four nanocomposite colorimetric sensitive dyes were confirmed. The accuracy rates for LDA and KNN models in this study reached 100%. This work shows great potential for grain quality control using CSA methods.

Analysis and Comparison of Volatile Compounds in Stropharia Rugosoannulata and Tricholoma Lobayense by Headspace Solid-Phase Microextraction-Gas Chromatography-Mass Spectrometry

The volatile components of Stropharia rugosoannulata and Tricholoma lobayense were analyzed by mass spectrometry, and the relative contents of each component were determined by the internal standard method. In Stropharia rugosoannulata, 58 volatile components were identified, including 10 alcohols, 14 esters, 9 aldehydes, 5 ketones, 1 phenol, 3 alkanes, 4 amines, 5 acids, 1 furan, 1 pyrazine, 1 olefin, 1 oxime, 1 pyrazole, and 2 other components. Among them, the most abundant volatile component was hexanal (1655.40 ng/g), followed by pentanoic acid (1503.10 ng/g) and phenylethyl alcohol (1215.94 ng/g). In Tricholoma lobayense, 68 volatile components were identified, including 17 aldehydes, 11 ketones, 8 acids, 10 esters, 5 alcohols, 1 phenol, 2 furans, 4 alkanes, 1 alkene, 1 oxime, 1 pyrazole, 1 amine, and 6 other components. Among them, the most abundant volatile component was benzaldehyde (2190.67 ng/g), followed by hexanal (1708.81 ng/g) and furan, 2-pentyl- (838.45 ng/g). There were 21 common volatile components between the two different edible fungi, including 7 aldehydes, 5 esters, 3 ketones, 2 alcohols, 2 acids, 1 oxime, and 1 furan.

Impact of different smoke flavors on the quality of hermetically sealed green chili paste (Nam Prik Num)

This research examined how various smoke flavors such as powdered smoke, teak, and longan wood affected the quality of hermetically sealed green chili paste (Nam Prik Num). Teak and longan wood smoking produced a darker green color than the control and smoke powder samples. The smoky aroma had no impact on yield, pH, water release, or chemical composition. However, it did influence moisture content, lightness (L*), redness (a*), yellowness (b*), and water activity (aw) compared to control and smoke-flavored samples. The attenuated total reflection-Fourier transform infrared spectroscopy (ATR-FTIR) showed structural changes, control with C-H groups at 2924 cm−1, and smoking introduced –COOR at 1744 cm−1, signifying flavor-induced alterations. The heightened peak hinted at a distinctive smoke aroma, deepening our understanding of molecular transformations. Sample smoke flavor compounds studied using a solid-phase microextraction-gas chromatography-mass spectrometry (SPME-GC-MS), included hydrocarbons, alcohol, aldehydes, ketones, esters, acids, and sulfide compounds, with sulfide compounds, alcohol, hydrocarbon, and alcohol compounds as the predominant volatiles. Nam Prik Num with smoke powder scored higher in appearance, color, aroma, taste, and texture than the control. Flavoring with smoke powder is more effective than charcoal grilling for adding smoky taste to Nam Prik Num.

Volatile profile of bee bread

Bee bread is one of the least studied bee products. In this study, ten bee bread samples were characterized using palynology and HS–SPME–GC–MS (headspace solid-phase microextraction gas chromatography-mass spectrometry). In total, over one hundred different volatile components were identified, belonging to different chemical groups. Only ten common components were detected in all the samples. These volatiles were ethanol, methylene chloride, ethyl acetate, acetic acid, α-pinene, furfural, nonane, nonanal, n-hexane and isovaleric acid. Several other components were commonly shared among various bee bread samples. Over sixty detected compounds have not been previously reported in bee bread. The analysis required a mild extraction temperature of 40 °C, as higher temperatures resulted in the Maillard reaction, leading to the production of furfural. The profile of volatile compounds of the tested bee pollen samples was complex and varied. Some relationships have been shown between botanical origin and volatile organic compound profile.

Non-targeted metabolomic analysis reveals the mechanism of quality formation of citrus flower-green tea.

Citrus flower-green tea (CT) is a scented tea processed from green tea (GT) and fresh citrus flower, which is favored by consumers due to its potential health benefits and unique citrus flavor. This study evaluated the quality of CT and revealed the mechanism of its quality formation. The CT had a significant citrus flavor and a good antioxidant activity, and its sensory quality was superior to that of GT. Headspace solid-phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) analysis revealed that the scenting process resulted in a significant increase of alkenes such as β-pinene, trans-β-ocimene, α-farnesene, isoterpinolene, and γ-terpinene, as well as a significant decrease of alcohols such as α-terpineol, l-menthol, and linalool in CT in comparison with GT. Liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis revealed that the levels of flavonoids (such as neohesperidin, hesperidin, tangeritin, hesperetin 5-O-glucoside, and nobiletin) and alkaloids (such as trigonelline and theobromine) in CT increased significantly after scenting process, while the levels of amino acids (such as valine and l-phenylalanine) and organic acids (such as ascorbic acid) decreased significantly. These observations showed that the scenting process promoted the absorption of aroma from citrus flowers by GT and the changes in its non-volatile metabolites, leading to the formation of citrus flavor quality in CT. © 2024 Society of Chemical Industry.

Qualitative and quantitative analysis for monitoring the fishy odor of anchovy oil

Abstract The fishy odor of fish oil, a popular nutritional supplement, affects its quality as well as consumer acceptance and eating experience. An objective or scientific method for analyzing fish oil’s olfactory characteristics is still lacking. This study examined anchovy oil to develop qualitative and quantitative approaches for identifying fishy odor components. Multiple fish oil refining samples were analyzed using gas chromatography-ion mobility spectrometry (GC-IMS). Due to their significant alterations during fish oil refining, low threshold values, and distinct olfactory properties, the unsaturated aldehydes (E)-2-pentenal and (E,E)-2,4-heptadienal and the unsaturated ketone 1-penten-3-one may contribute to the fishy odor. Among the chemicals, (E,E)-2,4-heptadienal was chosen as the marker for developing a method to quantify fishy odor and analyze deodorization samples using headspace solid-phase micro-extraction gas chromatography-mass spectrometry (HS-SPME-GC-MS). The quantitative study of fishy odor in fish oil is a pioneering approach that can help improve quality assurance and refining process.

Quantifying exhaled acetone and isoprene through solid phase microextraction and gas chromatography-mass spectrometry

BackgroundAcetone, isoprene, and other volatile organic compounds (VOCs) in exhaled breath have been shown to be biomarkers for many medical conditions. Researchers use different techniques for VOC detection, including solid phase microextraction (SPME), to preconcentrate volatile analytes prior to instrumental analysis by gas chromatography-mass spectrometry (GC-MS). These techniques include a previously developed method to detect VOCs in breath directly using SPME, but it is uncommon for studies to quantify exhaled volatiles because it can be time consuming due to the need of many external/internal standards, and there is no standardized or widely accepted method. The objective of this study was to develop an accessible method to quantify acetone and isoprene in breath by SPME GC-MS. ResultsA system was developed to mimic human exhalation and expose VOCs to a SPME fiber in the gas phase at known concentrations. VOCs were bubbled/diluted with dry air at a fixed flow rate, duration, and volume that was comparable to a previously developed breath sampling method. Identification of acetone and isoprene through GC-MS was verified using standards and observing overlaps in chromatographic retention/mass spectral fragmentation. Calibration curves were developed for these two analytes, which showed a high degree of linear correlation. Acetone and isoprene displayed limits of detection/quantification equal to 12 ppb/37 ppb and 73 ppb/222 ppb respectively. Quantification results in healthy breath samples (n = 15) showed acetone concentrations spanned between 71 ppb and 294 ppb, and isoprene varied between 170 ppb and 990 ppb. Both concentration ranges for acetone and isoprene in this study overlap with those reported in existing literature. SignificanceResults indicate the development of a system to quantify acetone and isoprene in breath that can be adapted to diverse sampling methods and instrumental analyses beyond SPME GC-MS.

Evaluation of aroma characteristics of Penaeus vannamei with different drying methods using HS-SPME-GC-MS, MMSE-GC-MS, and sensory evaluation

The effects of microwave drying (MD), hot air drying (HAD), vacuum hot air drying (VD), and vacuum freeze drying (VFD) on the volatile profiles of Penaeus vannamei were investigated. A total of 89 and 94 volatile compounds were identified by headspace solid-phase microextraction-gas chromatography–mass spectrometry (HS-SPME-GC–MS) and monolithic material sorptive extraction gas chromatography–mass spectrometry (MMSE-GC–MS), respectively. Orthogonal partial least squares-discriminant analysis (OPLS-DA) and variable influence on projection (VIP) models were utilized to select characteristic volatiles and key marker compounds (e.g., octanal, 1-octen-3-ol, 2-methyl-butanal, 2-ethyl-furan, and trimethyl-pyrazine) to discriminate among four drying methods. Based on synthesis of odor descriptions and sensory evaluation, it was found that P. vannamei via MD, HAD, and VD greatly reduced the fishy and generated roasted, fatty, and smoked odors. This study systematically analyzed the aroma characteristics of four traditional dried P. vannamei products, which may provide theoretical guidance for industrial production.

Phytochemical profiling of red raspberry (Rubus idaeus L.) honey and investigation of compounds related to its pollen occurrence.

Red raspberry (Rubus idaeus L.) is an important nectar source for honey production in some specific habitats as well as an important crop, so the definition of the features of this kind of honey is noteworthy. However, due to its rarity on the market, red raspberry honey is poorly characterized. The aim of this work was the phytochemical characterization of honey containing red raspberry from different geographical origins, through melissopalynological analyses concurrently with untargeted metabolomics achieved with different chromatographic techniques coupled to mass spectrometry: solid-phase micro-extraction/gas chromatography/mass spectrometry (SPME-GC-MS) and high-performance liquid chromatography/Orbitrap mass spectrometry (HPLC-Orbitrap). Only 4 out of the 12 samples involved in the study contained raspberry pollen as dominant pollen, although these honeys did not group in the hierarchical cluster analysis nor in the classical multidimensional scaling analyses used for data evaluation. The first result was the detection of mislabelling in two samples, which contained raspberry pollen only as minor or important minor pollen. Of the 188 compounds identified by HPLC-Orbitrap and of the 260 identified by SPME-GC-MS, 87 and 31 compounds were present in all samples, respectively. The structurally related compounds nicotinaldehyde and nicotinamide, nicotinic acid and nicotinyl alcohol were present in 100% of the samples and correlated with R. idaeus pollen count (r > 0.60, Pearson's correlation analysis). This study reveals important aspects about the characterization of red raspberry honey and could give new insights on bee diet and preferences, since niacin compounds resulted interestingly to be related to the presence of red raspberry pollen. © 2024 Society of Chemical Industry.