Solid-phase Microextraction Gas Chromatography Research Articles

Sensory and chemical characterization of chestnuts processed in different methods using instrumental analyses and the Check-all-that-apply method

Chestnuts are known for their unique sensory characteristics and nutritional value. However, the changes in their sensory attributes after processing remain unclear. This study used instrumental analysis and sensory evaluation combined with multivariate statistical analysis to investigate the effect of packaging and thermal sterilization procedures on the sensory characteristics of chestnuts. The results showed that the significant variations (p < 0.05) between the different processing methods for chestnuts were revealed via the texture analysis, headspace solid-phase microextraction gas chromatography × gas chromatography-time of flight-mass spectrometry (HS-SPME-GC×GC-TOF-MS), and check-all-that-apply (CATA) sensory evaluation. The packaging had a more significant influence on the sensory quality of the chestnuts than thermal sterilization procedures. The HS-SPME-GC×GC-TOF-MS identified 116 volatile compounds, and the partial least squares-discriminant analysis (PLS-DA) identified the 28 volatile compounds responsible for the similarities and differences among different processing methods of chestnuts. Principal component analysis (PCA) combined with texture analysis and the fingerprint of HS-SPME-GC×GC-TOF-MS, as well as the correspondence analysis (CA) analysis of CATA, could discriminate samples from different packaging of chestnuts. This study provides chestnuts processing recommendations for satisfying consumer preferences and predicting possible related quality changes.

Screening and tentatively identifying of volatile hazards of desiccant and deoxidizer in food package

Food desiccant and deoxidizer are becoming more prevalent in food preservation, where they keep food in good quality for longer periods of time by absorbing moisture and oxygen. In such a way that they are in direct contact with the food inside the food package. However, their safety is still unclear and they must be fully screened and identified. In this study, the volatiles in five representative desiccants and two deoxidizers in the market were screened and tentatively identified by headspace solid-phase microextraction gas chromatography coupled with mass spectrometry (HS-SPME-GC-MS), compared with NIST spectral libraries, and combined with manual analysis. Specific migration limits are provided in accordance with EU NO 10/2011. Risk classes are predicted for substances lacking toxicological data through toxtree software. More than half of the substances were initially screened with toxicological data, seven with specific migration limits, three Cramer III substances, the remainder being Cramer I substances and substances with no risk level. The high-risk substances were further analyzed and traced back to their potential sources. However, there are a few substances for which the potential sources are still unclear and require further research. Despite this, this study has established the safety of desiccant and deoxidizer for use in food to a large extent, providing a solid basis for the future development of the industry.

Correlation between physicochemical properties, flavor characteristics and microbial community structure in Dushan shrimp sour paste

Dushan shrimp sour paste (DSSP), a traditional Guizhou condiment, and its unique flavor is determined by the fermentation microbiota. However, the relationship between the microbiota structure and its flavor remains unclear. This study identified 116 volatile flavor compounds using electronic nose and headspace solid-phase microextraction-gas chromatography mass spectrometry (HS-SPME-GC–MS) techniques, of which 19 were considered as key flavor compounds, mainly consisting of 13 esters and 1 alcohol. High-throughput sequencing technique, the bacterial community structure of nine groups of DSSPs was determined. Further analysis revealed Vagococcus, Lactococcus, and Tepidimicrobium as key bacteria involved in flavor formation. This study contributes to our understanding of the relationship between bacterial communities and the flavor formation, and provides guidance for screening starter culture that enhance the flavor of DSSP in industrial production.

Yeasts volatile organic compounds (VOCs) as potential growth enhancers and molds biocontrol agents of mushrooms mycelia

Volatile organic compounds (VOCs) produced by yeasts can positively affect crops, acting as antifungals or biostimulants. In this study, Aureobasidium pullulans and Metschnikowia pulcherrima were evaluated as potential antagonists of Trichoderma spp., common fungal pathogen in mushroom cultivation. To assess the biocontrol ability and biostimulant properties of the selected yeast species, in vitro co-culture and VOCs exposure assays were conducted. In both assays, VOCs produced by Aureobasidium spp. showed the stronger antifungal activity with a growth inhibition up to 30 %. This result was further confirmed by the higher volatilome alcohol content revealed by solid phase microextraction-gas chromatography mass spectrometry (SPME/GC–MS). Overall, Aureobasidium strains can be potentially used as biocontrol agent in Pleorotus ostreatus and Cyclocybe cylindracea mycelial growth, without affecting their development as demonstrated by VOCs exposure assay and Fourier-transform infrared spectroscopy (FT-IR). Conversely, M. pulcherrima was characterized by a lower or absent antifungal properties and by a volatilome composition rich in isobutyl acetate, an ester often recognized as plant growth promoter. As confirmed by FT-IR, Lentinula mycelia exposed to M. pulcherrima VOCs showed a higher content of proteins and lipids, suggesting an improvement of some biochemical properties. Our study emphasizes that VOCs produced by specific yeast strains are potentially powerful alternative to synthetic fungicide in the vegetative growth of mushroom-forming fungi and also able to modify their biochemical composition.

Comprehensive analysis of the dynamic changes of volatile and non-volatile metabolites in boletus edulis during processing by HS-SPME-GC–MS and UPLC-MS/MS analysis

In order to investigate the dynamic changes of flavor compounds, Ultra Performance Liquid Chromatography Tandem Mass Spectrometry (UPLC-MS/MS) combined with Headspace Solid Phase Microextraction Gas Chromatography Mass Spectrometry (HS-SPME-GC–MS) was used to detect the metabolites in different drying processes. A total of 80 volatile compounds and 1319 non-volatile compounds were identified. The trend in the changes of C-8 compounds and sulfur-containing compounds were generally consistent with the trend of key enzyme activities. 479 differential metabolites were identified and revealed that metabolic profiles of compounds in Boletus edulis were altered with increased organic acids and derivatives and lipids and lipid-like molecules. Fatty acids and amino acids were transformed into volatile compounds under the action of enzymes, which played a significant role in the formation of the distinctive flavor of Boletus edulis. Our study provided a theoretical support for fully comprehending the formation mechanism of flavor from Boletus edulis during drying processes.

Identifying potential breath biomarkers for early diagnosis of papillary thyroid cancer based on solid-phase microextraction gas chromatography-high resolution mass spectrometry with metabolomics.

Thyroid cancer incidence rate has increased substantially worldwide in recent years. Fine needle aspiration biopsy (FNAB) is currently the golden standard of thyroid cancer diagnosis, which however, is invasive and costly. In contrast, breath analysis is a non-invasive, safe and simple sampling method combined with a promising metabolomics approach, which is suitable for early cancer diagnosis in high volume population. This study aims to achieve a more comprehensive and definitive exhaled breath metabolism profile in papillary thyroid cancer patients (PTCs). We studied both end-tidal and mixed expiratory breath, solid-phase microextraction gas chromatography coupled with high resolution mass spectrometry (SPME-GC-HRMS) was used to analyze the breath samples. Multivariate combined univariate analysis was applied to identify potential breath biomarkers. The biomarkers identified in end-tidal and mixed expiratory breath mainly included alkanes, olefins, enols, enones, esters, aromatic compounds, and fluorine and chlorine containing organic compounds. The area under the curve (AUC) values of combined biomarkers were 0.974 (sensitivity: 96.1%, specificity: 90.2%) and 0.909 (sensitivity: 98.0%, specificity: 74.5%), respectively, for the end-tidal and mixed expiratory breath, indicating of reliability of the sampling and analysis method CONCLUSION: This work not only successfully established a standard metabolomic approach for early diagnosis of PTC, but also revealed the necessity of using both the two breath types for comprehensive analysis of the biomarkers.

Volatile flavor behavior characterization of Hericium erinaceus during postharvest storage using E-nose, HS-GC-IMS, and HS-SPME-GC–MS after treated with electron-beam generated X-ray irradiation

Flavor alteration is a crucial factor affecting the quality of mushrooms during preservation. The dynamic variations of volatile profiles of fresh Hericium erinaceus with electron-beam generated X-ray irradiation were investigated by combining E-nose, headspace-gas chromatography-ion mobility spectrometry (HS-GC-IMS), and headspace solid-phase microextraction gas chromatography–mass spectrometry (HS-SPME-GC–MS). E-nose analysis achieved rapid discrimination in all treatments over storage time. 65 and 73 volatile organic compounds (VOCs) were identified by HS-GC-IMS and HS-SPME-GC–MS, respectively. Thereinto, 1-octen-3-ol, 1-octen-3-one, and 2-octanone were screened out as the characteristic VOCs, which contents declined during storage. While the contents of (E)-2-octenal, (E)-2-nonenal, and 1-octanol increased. The flavor profile changes from distinct mushroom and floral odor to an intense alcohol and fatty odor. Notably, one-kGy irradiation remained more volatiles and denser mushroom odor after storage. Multivariate analysis further confirmed that 1.0 kGy irradiation contributed to the overall aroma retention during postharvest storage of H. erinaceus.

Influence of germination and roasting on the characteristic volatile organic compounds of quinoa using sensory evaluation, E-nose, HS-GC-IMS, and HS-SPME-GC-MS

This study aimed to investigate the effects of germination and roasting on the flavor of quinoa. Firstly, the aroma of quinoa and germinated quinoa roasted under different conditions was analyzed using sensory evaluation and electronic nose (E-nose). Results showed that the best favorable aroma of quinoa and germinated quinoa was obtained when roasted at 160 °C for 15 min. Then, a total of 34 and 80 volatile organic compounds (VOCs) of quinoa and germinated quinoa roasted at 160 °C for 15 min were determined using headspace-gas chromatography-ion mobility spectrometry (HS-GC-IMS) and headspace solid-phase microextraction gas chromatography–mass spectrometry (HS-SPME-GC–MS), respectively. Germination and roasting effectively reduced the contents of VOCs that produced undesirable flavor. Moreover, germination improved the floral aromas, while roasting mainly produced caramel, cocoa, and roasted nut aromas of quinoa. This study indicated that germination and roasting treatments might serve as promising processing methods to improve the flavor of quinoa.

Geographical identification of Chinese wine based on chemometrics combined with mineral elements, volatile components and untargeted metabonomics

Identifying the geographic origin of a wine is of great importance, as origin fakery is commonplace in the wine industry. This study analyzed the mineral elements, volatile components, and metabolites in wine using inductively coupled plasma-mass spectrometry, headspace solid phase microextraction gas chromatography–mass spectrometry, and ultra-high-performance liquid chromatography-quadrupole-exactive orbitrap mass spectrometry. The most critical variables (5 mineral elements, 13 volatile components, and 51 metabolites) for wine origin classification were selected via principal component analysis and orthogonal partial least squares discriminant analysis. Subsequently, three algorithms—K-nearest neighbors, support vector machine, and random forest —were used to model single and fused datasets for origin identification. These results indicated that fused datasets, based on feature variables (mineral elements, volatile components, and metabolites), achieved the best performance, with predictive rates of 100% for all three algorithms. This study demonstrates the effectiveness of a multi-source data fusion strategy for authenticity identification of Chinese wine.

Characterization of Key Aroma Compounds and Main Contributing Amino Acids in Hot-Pressed Oil Prepared from Various Peanut Varieties.

The production of peanut oil in the industrial sector necessitates the utilization of diverse raw materials to generate consistent batches with stable flavor profiles, thereby leading to an increased focus on understanding the correlation between raw materials and flavor characteristics. In this study, sensory evaluations, headspace solid-phase micro-extraction gas chromatography mass spectrometry (HS-SPME-GC-MS), odor activity value (OAV) calculations, and correlation analysis were employed to investigate the flavors and main contributing amino acids of hot-pressed oils derived from different peanut varieties. The results confirmed that the levels of alcohols, aldehydes, and heterocyclic compounds in peanut oil varied among nine different peanut varieties under identical processing conditions. The OAVs of 25 key aroma compounds, such as methylthiol, 3-ethyl-2,5-dimethylpyrazine, and 2,3-glutarone, exceeded a value of 1. The sensory evaluations and flavor content analysis demonstrated that pyrazines significantly influenced the flavor profile of the peanut oil. The concentrations of 11 amino acids showed a strong correlation with the levels of pyrazines. Notably, phenylalanine, lysine, glutamic acid, arginine, and isoleucine demonstrated significant associations with both pyrazine and nut flavors. These findings will provide valuable insights for enhancing the sensory attributes of peanut oil and selecting optimal raw peanuts for its production.

Biomarker Aroma Compounds of Monofloral Honey From Kazakhstan by Gas Chromatography–Mass Spectrometry (GC–MS) and Chemometric Analysis*

The aroma compounds of honey provide useful information to determine the geographical origin. This work focuses on the study of aroma compounds of 16 honey samples using headspace (HS)-solid-phase microextraction (SPME) gas chromatography–mass spectrometry (GC-MS) to reaffirm the geographical features of 4 monofloral honey. 7 sunflower, 3 buckwheat, 2 agrimonia, and 4 tamarix monofloral honey samples were obtained from four regions of Kazakhstan. Moreover, the GC-MS data were applied to chemometric analysis for the common aroma compounds to discriminate the monofloral honeys. In total, 76 aroma compounds were detected and 72 were identified. α-Pinene, benzaldehyde, octanal, hotrienol, limonene, cosmene, nonanol, linalool oxide, dehydro-p-cymene, β-linalool, 2-nonen-1-ol, carvacrol, lilac aldehyde A, β-citral, 2-decen-1-al, and β-damascenone were identified as common aroma compounds for all honey types. According to principal component analysis (PCA), the aroma compounds of sunflower, buckwheat, agrimonia, and tamarix honey were distinguished. Dehydro-p-cymene, β-linalool, 2-nonen-1-ol, and linalool oxide were determined as dominant compounds for agrimonia honey, while nonanol, benzaldehyde, octanol, dehydro-p-cymene and β-linalool for buckwheat, β-citral, lilac aldehyde A, 2-decen-1-al, D-limonene, β-damascenone, linalool oxide for tamarix honey, and hotrienol, cosmene, α-pinene, and carvacrol for the sunflower product. PCA revealed that the dominant compounds for each honey could be used as biomarker compounds to detect the origin of the honey and possible adulteration, such as blending and inverted sugar addition.

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.

Analysis of Three Dimethyl Sulfides in Freshwater Lakes Using Headspace Solid-Phase Microextraction-Gas Chromatography with Flame Photometric Detection

Dimethyl sulfides are ubiquitous odorous substances in eutrophic freshwater bodies. In this study, a simple headspace solid-phase microextraction-gas chromatography-flame photometric detection method was developed to detect three representative algal-derived dimethyl sulfides in freshwater lake water samples: dimethyl monosulfide (DMS), dimethyl disulfide (DMDS), and dimethyl trisulfide (DMTS). The effects of extraction fiber, temperature, pH, ionic strength, and sample volume were investigated orthogonally, and the optimized method was applied to analyze surface water samples from Lake Ulansuhai in Inner Mongolia, China. Optimal extraction was obtained with a 50/30 µm DVB/CAR/PDMS extraction fiber, 20% ion concentration, 87 min extraction time, and 50 °C extraction temperature. The correlation coefficients of the standardized working curves for DMS, DMDS, and DMTS were 0.9967, 0.9907, and 0.9994, respectively, indicating good linear relationships. Limits of detection were in the nanogram range, and the recoveries of the spiked standards for DMS, DMDS, and DMTS were 97.22~99.07%, 93.39~99.34%, and 91.17~99.25%, with relative standard deviations of 5.18~5.94%, 3.08~6.25%, and 2.56~5.47%, respectively. This method is stable and reliable, and can be used for the determination of volatile sulfides in freshwater lake water.

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.

Aromatic Characterization of Graševina Wines from Slavonia and Podunavlje Sub-Regions

This study investigated the chemical aromatic profiles of 60 volatile organic compounds (VOCs), including 21 terpenes, 6 norisoprenoids, 6 volatile phenols, 4 C-6 alcohols, and 23 esters, in Graševina wines originating from Slavonia and Podunavlje sub-regions (Croatia). Headspace solid-phase microextraction gas chromatography coupled with mass spectrometric detection (HS-SPME-GCMS) was used to assess 60 VOCs, and a novel HS-SPME-GCMS method for the determination of terpenes and norisoprenoids was developed and validated. Statistical analysis found no significant differences between VOCs present in Graševina wines and others wines (Chardonnay and Pinot gris); nonetheless, comparison of VOC fingerprints between different wines from the same producer showed that four terpenes (α-terpinene, γ-terpinene, 1,4-cineol, and 4-terpineol) were present in higher amounts in Graševina wines when compared to other wines. By exclusively examining VOCs within Graševina wines through the utilization of a heatmap and hierarchical clustering, a distinct visualization of samples and VOCs emerged, highlighting the vintage effect. Simultaneously, a partial least squares discriminant analysis model was developed with a confidence interval of 95%, demonstrating a noticeable distinction between samples originating from the western and eastern regions. Furthermore, by employing the heatmap using only VOCs from the terpene and norisoprenoidic groups, a clear separation of samples into two groups was observed based on geographical origin; namely, higher concentrations of norisoprenoids and terpenes were observed in the Slavonia sub-region. These results suggest that terpenes and norisoprenoids to a lower extent may be valuable aromatic markers for the regional typicality of Graševina wines.

Black Truffle Aroma Evaluation: SPME-GC-MS vs. Sensory Experts.

Nowadays, the truffle aroma attribute is not included as a quality parameter in the current recommendation that explains the truffle quality (UNECE standard 53 FFV3) and establishes the truffle commercial categories. However, the aroma is the main reason why truffles are worldwide appreciated. Indeed, more than 30 aromatic molecules compose it, and this is the reason why the human evaluation and identification of these odorants, without previous training, is quite subjective. Analytical techniques such as gas chromatography techniques, however, can establish an aromatic profile and detect potential aromatic markers. In this study, 16 tasting experts were trained to make more objective the truffle aroma evaluation and odorants identification. For this, a comparison between solid-phase microextraction gas chromatography coupled with mass spectrometry (SPME-GC-MS) and sensory expert evaluation was carried out in six sessions during different harvesting times in the black truffle season (December, January, and February). Both techniques were able to separate truffles depending on the harvesting time. Also, a list of volatile organic compounds related to the aromatic attributes was reported. This information will help to provide a more objective T. melanosporum truffle sensory evaluation.

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.

Insight into the Relationship between the Causes of Off-Odour and Microorganism Communities in Xuanwei Ham.

To expound on the correlation between the microorganism communities and the formation of off-odour in Xuanwei ham, the microorganism communities and volatile compounds were investigated in the biceps femoris (BF) and semimembranosus (SM) of Xuanwei ham with different quality grades (normal ham and spoiled ham). The single molecule real-time sequencing showed that differential bacteria and fungi were more varied in normal hams than in spoiled hams. Headspace solid-phase microextraction-gas chromatography (HS-SPME-GC-MS) results indicated that aldehydes and alcohols were significantly higher in spoiled hams than those in normal hams (p < 0.05). The off-odour of spoiled hams was dominated by ichthyic, malodourous, sweaty, putrid, sour, and unpleasant odours produced by compounds such as trimethylamine (SM: 13.05 μg/kg), hexanal (BF: 206.46 μg/kg), octanal (BF: 59.52 μg/kg), methanethiol (SM: 12.85 μg/kg), and valeric acid (BF: 15.08 μg/kg), which are positively correlated with Bacillus cereus, Bacillus subtilis, Bacillus licheniformis, Pseudomonas sp., Aspergillus ruber, and Moraxella osloensis. Furthermore, the physicochemical property and quality characteristics results showed that high moisture (BF: 56.32 g/100 g), pH (BF: 6.63), thiobarbituric acid reactive substances (TBARS) (SM: 1.98 MDA/kg), and low NaCl content (SM: 6.31%) were also responsible for the spoilage of hams with off-odour. This study provided a deep insight into the off-odour of Xuanwei ham from the perspective of microorganism communities and a theoretical basis for improving the flavour and overall quality of Xuanwei hams.

Volatile Organic Compounds (VOCs) Produced by Levilactobacillus brevis WLP672 Fermentation in Defined Media Supplemented with Different Amino Acids.

Fermentation by lactic acid bacteria (LAB) is a promising approach to meet the increasing demand for meat or dairy plant-based analogues with realistic flavours. However, a detailed understanding of the impact of the substrate, fermentation conditions, and bacterial strains on the volatile organic compounds (VOCs) produced during fermentation is lacking. As a first step, the current study used a defined medium (DM) supplemented with the amino acids L-leucine (Leu), L-isoleucine (Ile), L-phenylalanine (Phe), L-threonine (Thr), L-methionine (Met), or L-glutamic acid (Glu) separately or combined to determine their impact on the VOCs produced by Levilactobacillus brevis WLP672 (LB672). VOCs were measured using headspace solid-phase microextraction (HS-SPME) gas chromatography-mass spectrometry (GC-MS). VOCs associated with the specific amino acids added included: benzaldehyde, phenylethyl alcohol, and benzyl alcohol with added Phe; methanethiol, methional, and dimethyl disulphide with added Met; 3-methyl butanol with added Leu; and 2-methyl butanol with added Ile. This research demonstrated that fermentation by LB672 of a DM supplemented with different amino acids separately or combined resulted in the formation of a range of dairy- and meat-related VOCs and provides information on how plant-based fermentations could be manipulated to generate desirable flavours.

Use of NMR, FTIR and GC–MS to monitor the oxidation products of phospholipids in bighead carp head during cooking process

Bighead carp head soup is a traditional Chinese cuisine with a pleasant aroma, but the effect of fish head phospholipids (FPLs) on the odorants is not fully understood. In this study, nuclear magnetic resonance (NMR), attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR) and headspace solid-phase microextraction gas chromatography–mass spectrometry (HS-SPME–GC–MS) were used to monitor the oxidation products of phospholipids in fish head soup during the cooking process, and the fish head triglycerides (FTGs) were used as controls. In 1H NMR spectra, the signals of unsaturated acyl groups and the oxidation compounds in FPLs were significantly higher than those in FTGs. The results of FTIR showed that the changes of functional group absorptions of the oxidation compounds in FPLs were greater than FTGs. GC–MS demonstrated that FPLs samples produced more lipid-derived volatile compounds than FTGs samples. These results showed that FPLs were more prone to oxidation and could produce more lipid-derived odorants. Therefore, FPLs rather than FTGs, were the main precursor substance of lipid-derived odorants in bighead carp head soup.