Extraction-gas Chromatography-mass Spectrometry Research Articles

Comparative analysis of feature annotation methods for SESI-HRMS in exhaled breath analysis

Secondary electrospray ionization coupled to high-resolution mass spectrometry (SESI-HRMS) is a powerful method for the analysis of exhaled breath in real time. However, feature annotation is challenging due to the flow-injection nature of the technique. To evaluate alternative methods for enhancing feature annotation, a study was conducted where the exhaled breath of sixteen subjects was condensed and analyzed using dynamic headspace vacuum in-trap extraction gas chromatography-mass spectrometry (DHS-V-ITEX-GC–MS) and liquid chromatography coupled to mass spectrometry (LC-MS) using polar and reverse-phase conditions along with a data-independent MS2-acquisition method based on multiple injections. The annotation results obtained from these methods were compared to those from SESI-HRMS. The use of these techniques on breath condensate is unprecedented. The GC–MS method primarily detected compounds of exogenous origin, particularly additives in oral hygiene products like menthol. On the other hand, LC-MS detected a vast number of features, especially with the utilized data-independent acquisition method. Chemical classes to these features were assigned in-silico. In positive ion mode, mostly amino acids and amines were detected, while the largest group in negative ion mode consisted of carboxylic acids. Approximately 25% and 5% of SESI features had a corresponding match with LC-MS and GC–MS. While both GC–MS and LC-MS methods partially overlapped with the SESI features, there was limited overlap of both in the mass-to-charge range from 150 to 200. In conclusion, both GC–MS and LC-MS analysis of breath condensate can serve as supplementary tools for annotating features obtained from SESI-MS. However, to increase confidence in the annotation results, combining these methods with additional on-line fragmentation techniques is recommended.

Postharvest dehydration of red grapes: impact of temperature and water-loss conditions on free and glycosylated volatile metabolites of exocarp and epicarp of Nebbiolo and Aleatico varieties.

Postharvest dehydration affects the metabolism of grapes, impacting odorous secondary metabolites and therefore the features of the corresponding passito wines - high-quality products with winemaking practices linked to specific territories and related autochthonous grape varieties. Water loss and temperature conditions are the main variables of the dehydration process. This study assessed how they impacted the patterns of free and glycosylated volatile organic compounds (VOCs) of the exocarp (pulp) and epicarp (skin) in Nebbiolo and Aleatico, a neutral and semi-aromatic red grape variety, respectively. Dehydration parameters were set in tunnel conditions, and VOCs were quantitatively analyzed by solid phase extraction-gas chromatography-mass spectrometry. For Nebbiolo grapes, weight loss had a greater impact on free volatiles than dehydration temperature, with a 20% weight loss increasing total VOCs in both exocarp and epicarp. Low temperature (10 °C) significantly increased (P < 0.05) the glycosylated VOCs' terpene content. In Aleatico grapes, weight loss was key in modulating free volatiles, with 30% weight loss and 15 °C leading to significant increases in VOCs, especially exocarp terpenes, acids and benzenoids. More stressful dehydration (30% weight loss at 25 °C) resulted in higher aroma precursor concentrations. These findings can assist passito wine production in preserving varietal aromas of original grapes trough optimized dehydration conditions, preventing sensory homologation occurring because of strong uncontrolled dehydration. They can also promote optimization of energy consumption, thus fostering financial and environmental sustainability. © 2024 The Author(s). Journal of the Science of Food and Agriculture published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry.

Volatile profiles of Murcott and Ponkan mandarins obtained by stir bar sorptive extraction technique and their contributions to the fruit aroma.

Citrus species have undergone immense diversification ever since their ancestral origin. Ponkan and Murcott are two mandarin varieties widely consumed in Brazil and their aroma producing active compounds have not yet been extensively investigated. The present study analyzed the volatile constituents of the Ponkan and Murcott varieties employing the stir bar sorptive extraction (SBSE) technique and gas chromatography-mass spectrometry (GC-MS) analysis for the first time. Extraction was performed using the two phases of Twister bar, polydimethyl siloxane (PDMS), and ethylene glycol (EG) silicone in immersion and headspace modes. Among the detected 62 compounds comprising alcohols, aldehydes, esters, terpenes, and others identified, 55 and 37 compounds in the Ponkan and Murcott variety were determined, respectively, from both immersion and headspace modes using the two phases of Twister bar. From the odor active values, the Ponkan was characterized with the domination of compounds such as hexanal, decanal, nonanal, (E)-2-hexanal, ethyl hexanoate, d-limonene, linalool, and geraniol. Similarly, the Murcott variety was characterized with predominant compounds, namely, nonanal, octanal, hexanal, (E)-2-hexanal, ethyl hexanoate, d-limonene, and linalool. The profile of volatile compounds was found to be unique in both the varieties studied, and SBSE technique with GC-MS analysis favored the characterization of their respective profile due to the high amount of phase in the Twister bars, when compared to similar techniques, like solid phase microextraction. The PDMS Twister bar showed better capacity of adsorption of volatile compounds, since it is a relatively low-polarity polymer, which discriminates less analytes with different structures and polarities sampled from complex matrices, such as fruits juice.

Optimization of volatile organic compounds sampling from dairy cow exhaled breath using polymer-based solid-phase extraction cartridges for gas chromatographic analysis

We explored appropriate technical setups for the detection of volatile organic compounds (VOCs) from exhaled cow breath by comparing six different polymer-based solid-phase extraction (SPE) cartridges currently on the market for gas chromatography/mass spectrometry (GC-MS) screening. Exhaled breath was sampled at a single timepoint from five lactating dairy cows using six different SPE cartridges (Bond Elut ENV (ENV); Chromabond HRX (HRX); Chromabond HRP (HRP); Chromabond HLB (HLB); Chromabond HR-XCW (XCW) and Chromabond HR-XAW (XAW)). The trapped VOCs were analyzed by dynamic headspace vacuum in-tube extraction GC-MS (DHS-V-ITEX-GC-MS). Depending on the SPE cartridge, we detected 1174–1312 VOCs per cartridge. Most VOCs were alkenes, alkanes, esters, ketones, alcohols, aldehydes, amines, nitriles, ethers, amides, carboxylic acids, alkynes, azoles, terpenes, pyridines, or sulfur-containing compounds. The six SPE cartridges differed in their specificity for the chemical compounds, with the XAW cartridge showing the best specificity for ketones. The greatest differences between the tested SPE cartridges appeared in the detection of specific VOCs. In total, 176 different VOCs were detected with a match factor >80%. The greatest number of specific VOCs was captured by XAW (149), followed by ENV (118), HLB (117), HRP (115), HRX (114), and XCW (114). We conclude that the tested SPE cartridges are suitable for VOC sampling from exhaled cow breath, but the SPE cartridge choice enormously affects the detected chemical groups and the number of detected VOCs. Therefore, an appropriate SPE adsorbent cartridge should be selected according to our proposed inclusion criteria. For targeted metabolomics approaches, the SPE cartridge choice depends on the VOCs or chemical compound groups of interest based on our provided VOC list. For untargeted approaches without information on the animals’ metabolic condition, we suggest using multi-sorbent SPE cartridges or multiple cartridges per animal.

Noninvasive Assessment of Chicken Egg Fertility during Incubation Using HSSE-GC-MS VOC Profiling.

Volatile organic compounds (VOCs) carry crucial information about chicken egg fertility. Assessing the fertility before incubation holds immense potential for poultry industry efficiency. Our study used headspace sorptive extraction-gas chromatography-mass spectrometry to analyze egg VOCs before and during the initial 12 incubation days. A total of 162 VOCs were identified. Hexanal was significantly higher in unfertilized eggs, whereas compounds such as propan-2-ol, propan-2-one, and carboxylic acids were higher in fertilized eggs. Furthermore, the obtained multiple logistic regression model outperformed the partial least-squares-discriminant analysis (PLS-DA) model, demonstrating lower complexity and superior performance. Fertile eggs were accurately identified in the validation set in 68-75% of the cases during the initial 4 days, to 85 and 100% on days 6 and 8. Finally, hierarchical cluster analysis in fertilized eggs revealed the clustering of VOCs of the same chemical class, indicative of their shared biochemical origin. This suggests a promising direction for future research aimed at understanding the biological information embedded in VOCs and their relationship to biochemical processes during embryo development.

Comprehensive analysis of the effect of etiolated tea cultivars and harvest seasons on volatile compounds and in vitro antioxidant capacity in steamed green teas

To explore the effects of harvest seasons and etiolated cultivars on the volatile compounds of steamed green teas, this study analyzed comprehensively the volatile compounds of steamed green teas using simultaneous distillation extraction-gas chromatography–mass spectrometry (SDE-GC–MS) and chemometrics analytical techniques in combination with odor activity value (OAV). Additionally, the in vitro antioxidant capacity of the steamed green teas was evaluated. The results showed that 95 volatile compounds were identified, among which aldehydes, ketones, alcohols, and acids were the main types in steamed green teas made from etiolated tea cultivars. Furthermore, the relative content of volatile compounds in steamed green tea was significantly negatively correlated with season (P < 0.05). In steamed green teas harvested in different seasons, spring tea contained a higher abundance of volatile compounds such as (+)-δ-cadinene, farnesyl acetone, carvenone, trans-β-ionone, and nerolidol. The differences of total volatile compounds among the three etiolated tea cultivars were not remarkable (P > 0.05). Combined with the OAV, 20 and 19 key aroma compounds in steamed green teas from different harvest seasons and cultivars were identified, respectively, which could bring unique aromas to different steamed green tea samples. By comparison, summer tea had the strongest antioxidant capacity, while there was no obvious difference in the antioxidant capacity among cultivars. This study provided a scientific basis for the aroma quality of steamed green teas made from etiolated tea cultivars in different harvest seasons.

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.

Determination of nine aromatic amines in water by cloud point extraction-gas chromatography-mass spectrometry

Aromatic amines are a class of compounds bearing amino groups on their benzene rings; these compounds are important raw materials for the industrial production of rubber chemicals, pesticides, dyes, pharmaceuticals, photosensitive chemicals, and agricultural chemicals. Research has revealed that some aromatic amines teratogenetic, carcinogenic, and mutagenic properties. Given the high toxicity and potential harm caused by aromatic amines, monitoring their levels in water sources is critical. Aromatic amines are among the 14 strategic environmental pollutants blacklisted in China, and assessing their exposure levels is essential for protecting human health and the environment. At present, the standard method for detecting aromatic amines in water is liquid-liquid extraction-gas chromatography-mass spectrometry (LLE-GC-MS). However, this method has the disadvantages of large sample size requirement, complex operation, long analysis time, and high reagent consumption. In this study, instead of traditional LLE technology, cloud point extraction (CPE) technology was used in combination with GC-MS to establish an efficient, sensitive, and environment-friendly method for the detection of nine aromatic amines, namely, 2-chloramine, 3-chloramine, 4-chloramine, 2-nitroaniline, 3-nitroaniline, 4-nitroaniline, 1-naphthylamine, 2-naphthylamine, and 4-aminobenzene, in water. Triton X-114 was used as the extraction agent. The main experimental parameters were optimized using a single-factor optimization method. The aromatic amines in various water samples were quantitatively analyzed using GC-MS. The nine aromatic amines were separated on a DB-35 MS capillary column (30 m×0.25 mm×0.25 μm). The mass spectrometer was operated in selected ion monitoring (SIM) mode, and quantitative analysis was performed using the internal standard method. The results demonstrated that all nine aromatic amines could be completely separated within 16 min and had good linearities within accurate mass concentration ranges, with correlation coefficients (R2) greater than 0.998. The limits of detection (LODs) and quantification (LOQs) of these aromatic amines in water were 0.12-0.48 and 0.40-1.60 μg/L, respectively. The accuracy and precision of the method were assessed via the determination of aromatic amines in surface water of drinking water sources, offshore seawater, wastewater of the typical printing and dyeing industry at levels of 2.0 and 10.0 μg/L. The recoveries of the aromatic amines in surface water of drinking water sources were 81.1%-109.8%, with intra-day and inter-day relative standard deviations (RSDs) of 0.7%-5.2% (n=6) and 1.6%-6.2% (n=3), respectively. The recoveries of the aromatic amines in offshore seawater were 83.0%-115.8%, with intra-day RSDs (n=6) of 1.5%-8.6% and inter-day RSDs (n=3) of 2.4%-12.2%. The recoveries of the nine aromatic amines in wastewater of the typical printing and dyeing industry were 91.0%-120.0%, with intra-day RSDs (n=6) of 2.9%-12.9% and inter-day RSDs (n=3) of 2.5%-13.1%. The established method was used to detect nine aromatic amines in actual water samples. No aromatic amines were detected in the surface water of drinking water sources or offshore seawater samples. However, 2-chloramine, 4-chloramine, and 4-aminobenzene, which are frequently used in the printing and dyeing industry, were detected in the wastewater of the typical printing and dyeing industry samples. The proposed method offers the advantages of simple operation, high sensitivity, low cost, low organic reagent requirement, and good repeatability. Thus, this method provides reliable technical support for studying the residual status and environmental behavior of aromatic amines in water.

Distribution and Sensory Impact of (2E,4E,6Z)-nonatrienal and Trans-4,5-epoxy-(E)-2-decenal in Wines and Spirits.

This study reports the distribution of (2E,4E,6Z)-nonatrienal (1) and trans-4,5-epoxy-(E)-2-decenal (2) in wines and spirits. We validated a quantification method using solid-phase extraction (SPE) and negative chemical ionization (NCI, NH3) gas chromatography-mass spectrometry (GC-MS) analysis. Both were identified for the first time in wines and spirits from different grape varieties and raw materials. Their olfactory detection thresholds (ODTs) were 16 and 60 ng/L, respectively. Analysis of 66 wines showed that the highest levels of (1) (441.3 ng/L) and (2) (386.5 ng/L) were found in red and white wines, respectively. At these levels, they modify the balance of the fruity expression of red (fresh to cooked fruits) and white (vegetal/green hazelnut nuance) wines. Similar quantitative and sensory analyses were conducted in spirits. With ODT estimated at 500 and 400 ng/L and concentrations ranging from trace amounts to 1.1 and 2.4 μg/L respectively, (1) and (2) can contribute directly to the aroma of spirits.

Combined volatile compounds and non-targeted metabolomics analysis reveals variation in flavour characteristics, metabolic profiles and bioactivity of mulberry leaves after Monascus purpureus fermentation.

Mulberry leaves (MLs) are widely used in food because of their nutritional and functional characteristics. However, plant cell walls and natural bitterness influence nutrient release and the flavor properties of MLs. Liquid-state fermentation using Monascus purpureus (LFMP) is a common processing method used to improve food properties. The present study used headspace solid-phase micro extraction gas chromatography-mass spectrometry (HS-SPME-GC-MS) and non-targeted metabolomics to examine changes in volatile and non-volatile metabolites in MLs. The transformation mechanism of LFMP was investigated by microscopic observation and dynamic analysis of enzyme activity, and changes in the biological activity of MLs were analyzed. LFMP significantly increased total phenolics, total flavonoids, free amino acids and soluble sugars in MLs, at the same time as decreasing phytic acid levels. In total, 92 volatile organic compounds (VOCs) were identified and quantified. VOCs such as (2R,3R)-(-)-2,3-butanediol, terpineol and eugenol showed some improvement in the flavour characteristics of MLs. By using non-targeted metabolomics, 124 unique metabolites in total were examined. LFMP altered the metabolic profile of MLs, mainly in plant secondary metabolism, lipid metabolism and amino acid metabolism. Microscopic observation and dynamic analysis of enzyme activity indicated that LFMP promoted cell wall degradation and biotransformation of MLs. In addition, LFMP significantly increased the angiotensin I-converting enzyme and α-glucosidase inhibitory activity of MLs. LFMP altered the flavour characteristics, metabolite profile and biological activity of MLs. These findings will provide ideas for the processing of MLs into functional foods. In addition, they also provide useful information for biochemical studies of fermented MLs. © 2023 Society of Chemical Industry.

In-silico Study of Methyl Beta D-xylopyranoside: A Spectroscopically Screened Small Molecule from Aganosma dichotoma

Background: To develop scientific evidence of unexplored traditional plants. Methods: Standardization of leaf powder was done as per World Health Organization (WHO) guidelines, followed by fourier-transform infrared spectroscopy (FTIR) analysis to identify basic phytoconstituents. Preliminary phytochemical analysis and spectroscopic analysis was done to validate the identified phytoconstituents. Molecular docking was done to identify a small molecule, methy beta D-xylopyranoside. Results: The air-dried leaves and barks were powdered and subjected to extraction based on the polarity of solvents through soxhlation, namely, methanol, ethanol, and chloroform, to obtain four different extracts. Further, preliminary phytochemical tests and qualitative determination of the different biologically active compounds from leave powder Aganosma dichotoma using FTIR revealed the presence of different phytoconstituents. And gas chromatography-mass spectrometry of crude extracts revealed different chemical entities with varying quantities and followed by in-silico molecular docking studies of hub genes against the photochemical small molecule. Thus, the identification of different biologically active compounds in the extracts of leaves A. dichotoma warrants further biological and pharmacological studies. Conclusion: Small molecules identified from A. dichotoma have robust activity against myocardial infarction, but need to be validated through in-vitro and in-vivo studies.

Determination of Volatile Organic Compounds and Endogenous Extracts and Study of Expression Patterns of TPS and BSMT in the Flowers of Seven Lilium Cultivars.

Lily is one of the most important cut flowers in the world, with a rich floral fragrance. To further explore the fragrance emission mechanisms of lily cultivars, headspace solid-phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) and organic solvent extraction-gas chromatography-mass spectrometry (OSE-GC-MS) were used to unveil the volatile organic compounds (VOCs) and endogenous extracts of seven lily cultivars. Furthermore, real-time quantitative PCR (qRT-PCR) was used to determine the expression levels of two key genes (TPS and BSMT) related to the biosynthesis of monoterpenoids and methyl benzoate. The results show that forty-five VOCs were detected in the petals of seven lily cultivars, and the main compounds were monoterpenoids and phenylpropanoids/benzenoids. Dichloromethane was the best solvent for extracting the endogenous extracts of Lilium 'Viviana' petals and eighteen endogenous extracts were detected using dichloromethane to extract the petals of seven lily cultivars. Each compound's emission ratio (natural logarithm of the ratio of VOC content to endogenous extract content) was calculated, and linear regression analyses between emission ratios and boiling points were conducted. Significant linear negative correlations existed between the emission ratios and boiling points of compounds, and the regression equations' coefficients of determination (R2) were all greater than 0.7. TPS was expressed highly in 'Viviana', 'Pink News', and 'Palazzo', and BSMT was expressed highly in 'Pink News' and 'Palazzo'. Correlation analyses between the gene expression levels and the monoterpenoids and methyl benzoate contents found that the TPS expression levels have strong positive correlations with monoterpenoids content, while no correlations were found between the expression levels of BSMT and the contents of methyl benzoate. This study lays the foundation for research on the release patterns of VOCs in the flowers of Lilium, and the breeding of lilies for their floral fragrance.

Non-destructive egg breed separation using advanced VOC analytical techniques HSSE-GC-MS, PTR-TOF-MS, and SIFT-MS: Assessment of performance and systems’ complementarity

Over the past decade, advanced analytical techniques have been utilized to examine volatile organic compounds (VOCs) in eggs. These VOCs offer valuable insights into factors such as freshness, fertility, the presence of cracks, embryo sex, and breed. In our study, we assessed three mass spectrometry-based systems (headspace sorptive extraction gas chromatography-mass spectrometry; HSSE-GC-MS, proton transfer reaction time-of-flight-mass spectrometry; PTR-TOF-MS; and selected ion flow tube mass spectrometry; SIFT-MS) to analyze and identify VOCs present in intact hatching eggs from three distinct breeds (Dekalb white layer, Shaver brown layer, and Ross 308 broiler). The eggs were sampled on incubation days 2 and 8, to identify VOCs that distinguish breeds irrespective of incubation day. VOC measurements were conducted on 15 eggs per breed by placing them together with PDMS-coated stir bars inside inert Teflon® air sampling bags. After an accumulation period of 2 h, the headspace was analyzed using PTR-TOF-MS and SIFT-MS, while the VOCs adsorbed onto the stir bars were analyzed using GC-MS for additional compound identification. Partial least squares discriminant analysis (PLS-DA) models were constructed for breed differentiation, and variable selection was performed. As a result, 111 VOCs were identified using HSSE-GC-MS, with alcohols and esters being the most abundant. The PLS-DA models demonstrated the efficacy of breed discrimination, with the HSSE-GC-MS and the PTR-TOF-MS exhibiting the highest balanced accuracy of 95.5 % using a reduced set of 11 VOCs and 5 product ions, respectively. The SIFT-MS model had a balanced accuracy of 92.8 % with a reduced set of 11 product ions. Furthermore, complementarity was observed between HSSE-GC-MS, which primarily selected higher molecular weight VOCs, and PTR-TOF-MS and SIFT-MS. A higher correlation was found for compound abundances between the HSSE-GC-MS and the PTR-TOF-MS relative to the SIFT-MS, indicating that the PTR-TOF-MS was better suited to quantify specific compounds identified by the HSSE-GC-MS. Finally, the findings support the presence of VOCs originating from both synthetic and natural sources, highlighting the ability of the VOC analysis systems to non-destructively perform quality control and reveal differences in management practices or biological information encoded in eggs.

Quality control of psychoactive substances in human breastmilk samples from a human milk bank by disposable pipette extraction-gas chromatography-mass spectrometry.

The lack of data regarding infant exposure to drugs of abuse consumed by lactating mothers has become a major health concern. Investigating psychoactive substances and their metabolites in breastmilk is an analytical approach to estimate the rate at which drugs of abuse are excreted and how much infants are exposed to them. In this study, we have developed and validated a GC-MS method using disposable pipette tips for simultaneously extracting ten analytes from breastmilk samples obtained from a milk bank in the city of Ribeirão Preto, Brazil. All the 67 analyzed samples tested negative for all the analytes. This is the first study that has applied disposable pipette extraction to analyze drugs of abuse in breastmilk samples.

Factors in Modulating the Potential Aromas of Oak Whisky Barrels: Origin, Toasting, and Charring.

In this study, the effects of origin (Chinese, France, and America), intensity of toasting, and degree of charring on the volatiles of oak whisky barrels were comprehensively investigated via liquid-liquid extraction-gas chromatography-mass spectrometry (LLE-GC-MS) combined with multivariate statistical analysis. Results of principal component analysis (PCA) showed that the main oak-derived volatiles in oak were more influenced by origin and toasting than by charring. French oak had a higher content of volatile compounds than the other two origins, and this difference decreased with toasting and charring. The process of toasting and charring was important for the release of volatile compounds from oak. The content of most oak-derived volatiles increased with deeper toasting intensity, and the degree of charring promoted or inhibited the release of oak-derived volatiles. The volatile components in oak blocks were affected by the two-factor interaction of toasting and charring. Continuing the process of the charring of oak at a certain level of toasting may have an enhancing or diminishing effect on the content of different volatile compounds, depending on the circumstances.

How volatile composition facilitates olfactory discrimination of fat content in beef and pork

Foods differing in fat content can be distinguished through olfaction alone. The mechanisms underlying the ability of humans to discriminate between foods differing in fat content through olfaction are underexplored. In this study, beef and pork samples were prepared (raw and roasted) with low (muscle tissue; raw: 2–5%; roasted: 5%), medium (muscle tissue with lard; raw: 25–30%; roasted: 36–44%), and high (lard; raw: 40–42%; roasted: 69–70%) fat content. Olfactory triangle discrimination tests and ranking tests were performed to explore whether humans can discriminate and rank fat content of the samples through orthonasal olfaction. Headspace-Solid Phase Micro Extraction-Gas Chromatography-Mass Spectrometry (SPME-GC–MS) was used to characterize the volatile compound composition of the headspace of samples differing in fat content. Partial least-squares regression and partial least squares-discriminant analysis were performed to determine the volatile compounds that were responsible for olfactory fat content discrimination. We found that fat content in both raw and roasted samples can be distinguished through orthonasal olfaction. Perceived odor differences did not always contribute to olfactory identification of fat content. Roasted beef and pork meats with higher fat content had more abundant fatty acids, aldehydes, and ketones. Phthalic acid, isobutyl 2-ropylpentyl ester, and carbon disulfide facilitated the olfactory discrimination of fat content in raw pork and beef samples. 2-Methyl-propanal, benzaldehyde, 1-hydroxy-2-propanone, 2,3-pentanedione, 2,5-octanedione, and 2-butanone contributed to odor differences of roasted beef samples differing in fat content. We conclude that beef and pork samples differing in fat content differ in volatile compound composition of the headspace, and that these differences facilitate discrimination between samples differing in fat content based on olfaction alone.

Iberian dry-cured ham sliced: Influence of vacuum packaging on volatile profile during chill-storage

Packed sliced ham has become one of the most relevant new sales format, but its influence on the volatile profile of Iberian ham has not been widely studied. Hence, in this work, the influence of storage time of Iberian dry-cured ham vacuum packaging on the volatile profile and therefore, on its quality, was evaluated. For that, 12 samples of three white label Iberian dry-cured ham pieces from three supermarkets were analysed by headspace sorptive extraction-gas chromatography-mass spectrometry, using 2 polydimethylsiloxano Twisters®. The results showed differences between the volatile profile of vacuum packed samples with different packaging times and those which were not, mainly in alcohols and ketones. Furthermore, important changes were observed after only one week of packaging. The most of the volatile compounds affected during the storage time in vacuum packaging were related to negative sensory notes, being able to influence the quality of this product.

Identification of volatile compounds in several meat and bone broth using Solid Phase Micro Extraction-Gas Chromatography Mass Spectrometry (SPME-GCMS) for initial detection of Halal and Non-Halal Food

The development of techniques for detecting halal and non-halal animal meat is of great importance as a useful tool for monitoring and assuring food quality for Muslim. Flavor or aroma is one of the sensory attributes for consumers to distinguish broth cattle. The differences aroma of broth cattle is contributed by the content of volatile compounds. This study was aimed to determine the composition of volatile compounds in meat and bone broth from five different animals, i.e., cow (beef), pig (pork), goat, lamb, and chicken for initial identification of halal and non halal food. A preliminary test for samples of meat and bone broth was done by identifying their physical properties including pH, viscosity, and density. The volatile compounds in meat and broth samples were extracted using a solid phase-micro extraction (SPME) at room temperature and analyzed by gas chromatography-mass spectrometry (GCMS). The results revealed the physical properties of meat and bone broth, i.e., pH, viscosity, and density, cannot be used to distinguish the type of broth produced from beef, pork, goat, lamb, and chicken. Successful results for the identification were achieved through chromatogram profile of volatile compounds from meat and bone broth which show characteristics to each type of animal, and therefore it can be used to distinguish pork from beef, goat, lamb, and chicken as initial detection for halal and non halal food. The research also identified 7 predominant volatile compounds as a marker for meat pork and other 8 specific compounds marker for pork bone.

Synthesis of a novel isotopically labelled standard for quantification of γ-nonalactone in New Zealand Pinot noir via SIDA-SPE-GC–MS

γ-Nonalactone is a linear aliphatic lactone ubiquitous in wine, associated with coconut, sweet, and stone fruit aroma descriptors. Little research has been conducted looking at the importance of this compound to New Zealand (NZ) wine aroma. 2H213C2-γ-Nonalactone, a novel isotopologue of γ-nonalactone, was synthesised in this work for use in a stable isotope dilution assay (SIDA) for quantification of γ-nonalactone in NZ Pinot noir wines for the first time. Synthesis was carried out using heptaldehyde as the starting material, and 13C atoms and 2H atoms were introduced via Wittig olefination and deuterogenation steps, respectively. The suitability of this compound as an internal standard was demonstrated by spiking model wine at normal and elevated conditions during sample preparation, with subsequent analysis via mass spectrometry showing stability of 2H213C2-γ-nonalactone. A model wine calibration, with concentrations of γ-nonalactone from 0 to 100 µg L−1, was shown to have excellent linearity (R2 > 0.99), reproducibility (0.72%), and repeatability (0.38%). Twelve NZ Pinot noir wines, representative of a range of NZ Pinot noir–producing regions, prices, and vintages, were analysed by solid-phase extraction–gas chromatography–mass spectrometry (SPE-GC–MS). The concentrations of γ-nonalactone ranged from 8.3 to 22.5 µg L−1, the latter of which was close to the odour detection threshold of this compound. These findings provide a basis for further research into γ-nonalactone and its impact on NZ Pinot noir aroma and provide a robust method for the quantification of this compound in Pinot noir.Graphical abstract

Formation mechanism of glandular trichomes involved in the synthesis and storage of terpenoids in lavender

BackgroundLavender (genus Lavandula, family Lamiaceae) is an aromatic plant widely grown as an ornamental plant. The chemical composition of lavender is characterized by monoterpenoids, sesquiterpenoids, and other compounds, which are primarily synthesized and stored in epidermal secretory structures called glandular trichomes (GTs). Volatile organic compounds (VOCs) are responsible for the aroma characteristics of plant oil that drive consumer preference. Aroma is usually regarded as a characteristic trait for the classification of aromatic plants. Interestingly, VOCs are synthesized and stored in GTs. Lamiaceae species such as purple perilla, peppermint, basil, thyme, and oregano usually possess two types of GTs: peltate glandular trichomes (PGTs) and capitate glandular trichomes (CGTs). But the development process of PGTs in lavender has been reported in only a few studies to date.ResultsIn this study, we identified and quantified the VOCs in four lavender cultivars by headspace-solid phase micro extraction-gas chromatography mass spectrometry (HS–SPME–GC–MS). A total of 66 VOCs were identified in these four cultivars, the most prominent of which were linalyl acetate and linalool, and flowers were the main site of accumulation of these VOCs. Here, we examined the developmental process of PGTs, including the formation of their base, body, and apex. The apex cells contained secretory cavities, which produced VOCs. Based on the reference genome sequence of the lavender cultivar ‘Jingxun 2’, several R2R3-MYB subfamily genes related to GT formation were identified. These results will guide the engineering of GTs and molecular breeding of lavender for improving the VOC content.ConclusionsIn this study, we identified the VOCs in four lavender cultivars. We analyzed the formation of GTs, and compared the number and diameter size of PGTs among four lavender cultivars. Additionally, we identified four candidate genes belonging to the R2R3-MYB family.