Two-dimensional Gas Chromatography Research Articles

Comparison of Comprehensive Two-Dimensional Gas Chromatography with a Flame Ionization Detector and D2425 Methods in the Analysis of Different Hydrocarbon Types in Jet Fuel

Comparison of Comprehensive Two-Dimensional Gas Chromatography with a Flame Ionization Detector and D2425 Methods in the Analysis of Different Hydrocarbon Types in Jet Fuel

Optimized quantification of fatty acids in complex media using advanced analytical techniques.

Various medium formulations contain essential fatty acids at concentrations ranging from 10 to 100 mg/L. Accurate and precise lipid measurement in media is crucial for monitoring media quality and conducting studies on lipids in the context of cell culture. This study employed two-dimensional gas chromatography (GC × GC) analyses to offer enhanced resolution, sensitivity, and separation performance compared to GC. Quantification of fatty acid methyl esters (FAMEs) in a medium was conducted using GC × GC combined with a high-resolution mass spectrometer and flame ionization detector, considering potential interference from nonionic surfactant Tween 80, which was precipitated and removed by optimizing the concentration of cobalt thiocyanate (CTA) solution during pretreatment. This advanced analytical approach enabled identification of cis and trans isomers of identical molecular weights and determination of the location and number of double bonds in the same carbon number structure. Our analysis identified 36 FAMEs within the C6-C24 region, and a 5% CTA solution was optimal for efficient removal of Tween 80 during lipid extraction. Additionally, this advanced method minimized FAME contamination and loss during pretreatment, thereby significantly reducing the sample volume required to detect trace levels of FAMEs. This improvement led to a fatty acid recovery rate of 106% while maintaining the average relative standard deviation for the target FAMEs of about 3%. Our research paves the way for future investigation into medium quality control and the role of fatty acids in cell culture. This offers the possibility for economical and effective trace quantification of fatty acids in complex media.

Online sequential analysis of volatile and semivolatile organic compounds in water matrices by double robotic sample preparations and dual-channel mono and comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry system

The monitoring of organic compounds in aquatic matrices poses challenges due to its complexity and time-intensive nature. To address these challenges, we introduce a novel approach utilizing a dual-channel mono (1D) and comprehensive two-dimensional (2D) gas chromatography coupled with time-of-flight mass spectrometry (GC × GC–TOFMS) system, integrated with a robotic pretreatment platform, for online monitoring of both volatile organic compounds (VOCs) and semivolatile organic compounds (SVOCs) in water matrices. Employing the robotic platform, we establish a suite of online liquid–liquid extraction (LLE) pretreatment processes for water samples, marking the first instance of such procedures. Leveraging the automatic headspace (HS) module, dual robotic preparations of HS and LLE are sequentially executed to extract VOCs and SVOCs from water matrices. The GC × GC–TOFMS system is distinguished by its dual-channel analytical column configuration, facilitating sequential analysis of VOCs in GC–TOFMS mode and SVOCs in GC × GC–TOFMS mode. Quantitative detection of 55 target VOCs and 104 SVOCs is achieved in a water sample using the instrument system. Our method demonstrates excellent correlation coefficients ranging from 0.990 to 1.000, method detection limits ranging from 0.08 to 4.78 μg L–1, relative standard deviations below 19.3 %, and recovery rates ranging from 50.0 % to 124.0 %. To validate the online monitoring capabilities of our system, we assess target SVOCs at three different concentration levels over a 3-day period. Most compounds exhibit recovery rates ranging from 70.0 % to 130.0 %. Furthermore, we apply our method to analyze a real water sample, successfully identifying over 100 target and nontarget VOCs/SVOCs, including alcohols, aldehydes, ketones, acids, esters, and phenols. These results highlight the efficacy of the proposed analysis system, capable of conducting two distinct analyses in automatic sequence, thereby enhancing the efficiency and accuracy of organic compound analysis in water matrices.

The influence of drying and storage conditions on the volatilome and cannabinoid content of Cannabis sativa L. inflorescences.

The increasing interest in hemp and cannabis poses new questions about the influence of drying and storage conditions on the overall aroma and cannabinoids profile of these products. Cannabis inflorescences are subjected to drying shortly after harvest and then to storage in different containers. These steps may cause a process of rapid deterioration with consequent changes in precious secondary metabolite content, negatively impacting on the product quality and potency. In this context, in this work, the investigation of the effects of freeze vs tray drying and three storage conditions on the preservation of cannabis compounds has been performed. A multi-trait approach, combining both solid-phase microextraction (SPME) two-dimensional gas chromatography coupled to mass spectrometry (SPME-GC × GC-MS) and high-performance liquid chromatography (HPLC), is presented for the first time. This approach has permitted to obtain the detailed characterisation of the whole cannabis matrix in terms of volatile compounds and cannabinoids. Moreover, multivariate statistical analyses were performed on the obtained data, helping to show that freeze drying conditions is useful to preserve cannabinoid content, preventing decarboxylation of acid cannabinoids, but leads to a loss of volatile compounds which are responsible for the cannabis aroma. Furthermore, among storage conditions, storage in glass bottle seems more beneficial for the retention of the initial VOC profile compared to open to air dry tray and closed high-density polyethylene box. However, the glass bottle storage condition causes formation of neutral cannabinoids at the expenses of the highly priced acid forms. This work will contribute to help define optimal storage conditions useful to produce highly valuable and high-quality products.

Parametric Study of Polyethylene Primary Decomposition Using a Micropyrolyzer Coupled with Two-Dimensional Gas Chromatography

Parametric Study of Polyethylene Primary Decomposition Using a Micropyrolyzer Coupled with Two-Dimensional Gas Chromatography

Retraction Note: A streak detection approach for comprehensive two-dimensional gas chromatography based on image analysis

Retraction Note: A streak detection approach for comprehensive two-dimensional gas chromatography based on image analysis

Comprehensive Two-Dimensional Gas Chromatography with a TOF MS Detector-An Effective Tool to Trace the Signature of Grape Varieties.

Varietal volatile compounds are characteristic of each variety of grapes and come from the skins of the grapes. This work focuses on the development of a methodology for the analysis of free compounds in grapes from Trincadeira, Cabernet Sauvignon, Syrah, Castelão and Tinta Barroca from the 2021 and 2022 harvests, using HS-SPME-GC × GC-TOFMS. To achieve this purpose, a previous optimization step of sample preparation was implemented, with the optimized conditions being 4 g of grapes, 2 g of NaCl, and 2 mL of H2O. The extraction conditions were also optimized, and it was observed that performing the extraction for 40 min at 60 °C was the best for identifying more varietal compounds. The fiber used was a triple fiber of carboxen/divinylbenzene/polydimethylsiloxane (CAR/DVB/PDMS). In addition to the sample preparation, the analytical conditions were also optimized, enabling the adequate separation of analytes. Using the optimized methodology, it was possible to identify fifty-two free volatile compounds, including seventeen monoterpenes, twenty-eight sesquiterpenes, and seven C13-norisoprenoids. It was observed that in 2021, more free varietal volatile compounds were identifiable compared to 2022. According to the results obtained through a linear discriminant analysis (LDA), the differences in volatile varietal signature are observed both among different grape varieties and across different years.

Conversion of Polypropylene into Light Hydrocarbons and Aromatics by Metal Exchanged Zeolite Catalysts.

Polyolefins can be converted into C2-C5 hydrocarbons and benzene-toluene-xylene (BTX) aromatics as high-demand petrochemical feedstocks via catalytic pyrolysis on acidic zeolites. Bro̷nsted and Lewis acid sites are responsible for cracking polyolefins into olefins and subsequent aromatic formation. In this study, we have subjected the parent HZSM-5 zeolite to postsynthetic partial metal exchange with Fe, Co, Ni, Cu, and Ce cations to perturb Bro̷nsted/Lewis acidity. We have investigated these metal-modified HZSM-5 on the catalytic pyrolysis of polypropylene (PP) in a micropyrolyzer connected to a two-dimensional gas chromatograph coupled to a time-of-flight mass spectrometer and flame ionization detector (Tandem Pyrolyzer-GC × GC-TOF-MS/FID setup). Whereas Fe-, Co-, Cu-, and Ce-exchanged zeolites (with 2.5, 2.3, 1.9, and 0.8 wt % metal, respectively) had comparable product yields with the parent zeolite, Ni-exchanged zeolites with Ni content of 0.5 to 2 wt % were associated with enhanced BTX formation (28-38 wt %) compared to that of the parent zeolite (22 wt %). Pyridine-FTIR indicated that the Bro̷nsted/Lewis acid ratio of the parent zeolite decreased upon metal ion exchange. According to Pyridine-TPD, the parent zeolite's medium-strength acid sites were redistributed into weak and strong acid sites in Ni-exchanged zeolites. The higher amount of carbon deposits on Ni-exchanged zeolites compared to the parent and other metal ion exchanged zeolites was attributed to the enhanced aromatization activity by the simultaneous decrease in the Bro̷nsted/Lewis acid ratio and emergence of strong acid sites.

Serum metabolic profiling in pregnant Holstein cows 3 weeks prior to parturition using two-dimensional gas chromatography time-of-flight mass spectrometry.

This preliminary study explored potential serum biomarkers for predicting the onset of milk fever (MF), a bovine parturient disease with hypocalcemia. We conducted two-dimensional gas chromatography mass spectrometry-based metabolomics in 8 and 17 pregnant Holstein cows that did and did not develop MF 3 weeks later, respectively. In principal component analysis (PCA) applied to a dataset containing 1498 metabolites, serum metabolites exhibited highly similar chemical profiles between cows with and without MF. PCA with a limited dataset of metabolites containing fatty acids, which had significantly different values between the groups and/or correlation coefficients of >0.5 for the serum calcium concentration, distinguished the two groups. These suggest the possibility of developing serum biomarkers for predicting bovine MF.

Characterization of odor-active compounds in Liuzhou River snail rice noodles soup by sensory-directed flavor analysis

Liuzhou River snails rice noodles, a special snack of Liuzhou City in the Guangxi Zhuang Autonomous Region, China, possess a unique flavor of spicy, refreshing, fresh, sour, and hot. The present study aimed to characterize the composition of volatile compounds and key odor-active compounds in river snails rice noodles soup (RSRNS) through aroma extract dilution analysis and odor activity value calculation using solid-phase microextraction (SPME) combined with comprehensive two-dimensional gas chromatography–olfactometry–mass spectrometry (GC×GC–O–MS) and gas chromatography–olfactometry–mass spectrometry (GC–O–MS). A total of 71 volatile compounds were identified by GC–O–MS, of which 49 were odor-active. Meanwhile, 125 volatile compounds were identified by GC×GC–O–MS, of which 68 were odor-active. These results indicated that 3-methylbutanal, linalool, 1,8-cineole, myrcene, 2-acetylpyrazine, 4-allylanisole, 2-acetylthiazole, 1-octen-3-ol, hexanal, and eugenol were the main odor-active compounds of RSRNS.

Elucidating the unexpected importance of intermediate-volatility organic compounds (IVOCs) from refueling procedure

Evaporative emissions release organic compounds comparable to gasoline exhaust in China. However, the measurement of intermediate volatility organic compounds (IVOCs) is lacking in studies focusing on gasoline evaporation. This study sampled organics from a real-world refueling procedure and analyzed the organic compounds using comprehensive two-dimensional gas chromatography coupled with a mass spectrometer (GC×GC-MS). The non-target analysis detected and quantified 279 organics containing 93 volatile organic compounds (VOCs, 64.9 ± 7.4 % in mass concentration), 182 IVOCs (34.9 ± 7.4 %), and 4 semivolatile organic compounds (SVOCs, 0.2 %). The refueling emission profile was distinct from that of gasoline exhaust. The b-alkanes in the B12 volatility bin are the most abundant IVOC species (1.9 ± 1.4 μg m−3) in refueling. A non-negligible contribution of 17.5 % to the ozone formation potential (OFP) from IVOCs was found. Although IVOCs are less in concentration, secondary organic aerosol potential (SOAP) from IVOCs (58.1 %) even exceeds SOAP from VOCs (41.6 %), mainly from b-alkane in the IVOC range. At the molecular level, the proportion of cyclic compounds in SOAP (12.1 %) indeed goes above its mass concentration (3.1 %), mainly contributed by cyclohexanes and cycloheptanes. As a result, the concentrations and SOAP of cyclic compounds (>50 %) could be overestimated in previous studies. Our study found an unexpected contribution of IVOCs from refueling procedures to both ozone and SOA formation, providing new insights into secondary pollution control policy.

Environmental temperature variations drive the changes of microbial communities to affect Baijiu flavor quality: Case study of Qingxiangxing Baijiu

Environmental temperature is a crucial factor that affects the fermentation quality of Baijiu. In this study, Illumina Miseq sequencingd, Two-dimensional gas chromatography coupled to mass spectrometry (GC × GC-MS), and physicochemical analyses were employed to investigate the microbial communities, flavor compounds, and physicochemical properties during fermentation at different ambient temperatures (10 ± 2 °C in the lower environmental temperature (LT) group and 22 ± 2 °C in the higher environmental temperature (HT) group). The findings demonstrated an augmentation in microbial diversity, ecological network complexity, and utilization of raw materials by microorganisms in HT group. Sensory analysis showed that sensory properties of Baijiu produced by the HT group had a better overall performance. The Baijiu in the HT group exhibited higher quality in terms of sweetness, fruity and floral, whereas the Baijiu in the LT group displayed a greater degree of unpleasant pungency and acidity. 24 flavor compounds were identified with the Variable Importance in Projection (VIP) > 1, and they were the main factors contributing to the differences in Baijiu flavors at two environmental temperatures. Correlation analysis showed that ambient temperature influenced microbial interactions and their correlation with metabolites. This difference showed the quality change of Baijiu driven by different temperatures. These results provide solid data support for optimizing the Baijiu fermentation process under different seasonal temperatures.

A novel headspace solid-phase microextraction arrow method employing comprehensive two-dimensional gas chromatography–mass spectrometry combined with chemometric tools for the investigation of wine aging

BackgroundOmics is used as an analytical tool to investigate wine authenticity issues. Aging authentication ensures that the wine has undergone the necessary maturation and developed its desired organoleptic characteristics. Considering that aged wines constitute valuable commodities, the development of advanced omics techniques that guarantee aging authenticity and prevent fraud is essential. ResultsΑ solid phase microextraction Arrow method combined with comprehensive two-dimensional gas chromatography-mass spectrometry was developed to identify volatiles in red wines and investigate how aging affects their volatile fingerprint. The method was optimized by examining the critical parameters that affect the solid phase microextraction Arrow extraction (stirring rate, extraction time) process. Under optimized conditions, extraction took place within 45 min under stirring at 1000 rpm. In all, 24 monovarietal red wine samples belonging to the Xinomavro variety from Naoussa (Imathia regional unit of Macedonia, Greece) produced during four different vintage years (1998, 2005, 2008 and 2015) were analyzed. Overall, 237 volatile compounds were tentatively identified and were treated with chemometric tools. Four major groups, one for each vintage year were revealed using the Hierarchical Clustering Analysis. The first two Principal Components of Principal Component Analysis explained 86.1% of the total variance, showing appropriate grouping of the wine samples produced in the same crop year. A two-way orthogonal partial least square – discriminant analysis model was developed and successfully classified all the samples to the proper class according to the vintage age, establishing 17 volatile markers as the most important features responsible for the classification, with an explained total variance of 88.5%. The developed prediction model was validated and the analyzed samples were classified with 100% accuracy according to the vintage age, based on their volatile fingerprint. SignificanceThe developed methodology in combination with chemometric techniques allows to trace back and confirm the vintage year, and is proposed as a novel authenticity tool which opens completely new and hitherto unexplored possibilities for wine authenticity testing and confirmation.

Monitoring Changes to Alkenone Biosynthesis in Commercial Tisochrysis lutea Microalgae.

Alkenones are unique lipids produced by certain species of microalgae, well-known for use in paleoclimatology, and more recently pursued to advance sustainability across multiple industries. Beginning in 2018, the biosynthesis of alkenones by commercially grown Tisochrysis lutea (T-Iso) microalgae from one of the world's most established producers, Necton S.A., changed dramatically from structures containing 37 and 38 carbons, to unusual shorter-chain C35 and C36 diunsaturated alkenones (C35:2 and C36:2 alkenones). While the exact reasons for this change remain unknown, analysis of alkenones isolated from T-Iso grown in 2021 and 2023 revealed that this change has persisted. The structure of these rare shorter-chain alkenones, including double bond position, produced by Necton T-Iso remained the same over the last five years, which was determined using a new and optimized cross-metathesis derivatization approach with analysis by comprehensive two-dimensional gas chromatography and NMR. However, noticeable differences in the alkenone profiles among the different batches were observed. Combined with fatty acid compositional analysis, the data suggest a connection between these lipid classes (e.g., increased DHA corresponds to lower amounts of shorter-chain alkenones) and the ability to manipulate their biosynthesis in T-Iso with changes to cultivation conditions.

Fingerprinting dissolved organic compounds: A potential tool for identifying the surface infiltration environments of meteoric groundwaters

Current methods for tracing decades-old groundwaters rely on isotope geochemistry, to determine groundwater age and altitude at the point of infiltration. Temporal and spatial variability in atmospheric conditions, and water-rock interactions, can make the interpretation of isotopes uncertain. Here, we propose a new method of groundwater tracing based on fingerprinting of natural dissolved organics. We present our initial findings from the Grimsel Test Site in Switzerland, located within a fractured granite. Using two-dimensional gas chromatography, we derive detailed organic fingerprints from surface soils at several locations and show that different soils produce distinctly different dissolved organic signatures. We then compare the soils with groundwater and lake water using a non-targeted approach using principal component analysis and hierarchical cluster analysis. Our analysis finds three statistically significant clusters. Most groundwaters are clustered with the lakewater samples, but two are clustered with soil from the highest altitude surface sampling location. We hypothesize that for samples to form a significant cluster, they must have derived from a common environment, with a unique combination of organic compounds. For groundwaters to cluster with soil samples or lakewater, we theorize there must be a hydraulic connection between the type of infiltration environment and the groundwater sampling locations within each cluster. Our research demonstrates that organic molecules derived from the surface environment can be used to discriminate near-surface environment(s) through which meteoric groundwater has infiltrated. Organic fingerprinting could prove a powerful tool for improved understanding of groundwater flow systems, particularly when combined with other complementary techniques. Thematic collection: This article is part of the Sustainable geological disposal and containment of radioactive waste collection available at: https://www.lyellcollection.org/topic/collections/radioactive Supplementary material: https://doi.org/10.6084/m9.figshare.c.712998

Characterization of key odorants in ‘Baimaocha’ black teas from different regions

‘Baimmaocha’ is a distinctive resource for production of high-quality black tea, and its processed black tea has unique aroma characteristics. 190 volatile compounds were identified by comprehensive two-dimensional gas chromatography–olfactometry-quadrupole-time-of-flight mass spectrometry(GC × GC-O-Q-TOMS), and among them 23 compounds were recognized as key odorants contributing to forming different aroma characteristics in ‘Baimaocha’ black teas of Rucheng, Renhua, and Lingyun (RCBT, RHBT, LYBT). The odor activity value coupled with GC-O showed that methyl salicylate (RCBT), geraniol (RHBT), trans-β-ionone and benzeneacetaldehyde (LYBT) might be the most definitive aroma compounds identified from their respective regions. Furthermore, PLS analysis revealed three odorants as significant contributors to floral characteristic, four odorants related to fruity attribute, four odorants linked to fresh attribute, and three odorants associated with roasted attribute. These results provide novel insights into sensory evaluation and chemical substances of ‘Baimaocha’ black tea and provide a theoretical basis for controlling and enhancement tea aroma quality.

Comparison of Trace Organic Chemical Removal Efficiencies between Aerobic and Anaerobic Membrane Bioreactors Treating Municipal Wastewater.

Evaluating persistent trace organic chemicals (TOrCs) and transformation products (TPs) in membrane bioreactors (MBRs) is essential, given that MBRs are now widely implemented for wastewater treatment and water reuse. This research applied comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC×GC/TOF-MS)-based nontargeted analysis to compare the effectiveness of parallel aerobic and anaerobic MBRs (AeMBRs and AnMBRs, respectively), treating the same municipal wastewater. The average total chromatographic feature peak area abundances were significantly reduced by 84% and 72% from influent to membrane permeate in both the AeMBR and AnMBR (p < 0.05), respectively. However, the reduction of the average number of chromatographic features was significant for only AeMBR treatment (p = 0.006). A similar number of TPs were generated during both AeMBR and AnMBR treatments (165 vs 171 compounds, respectively). The overall results suggest that the AeMBR was more effective for reducing the diversity of TOrCs than the AnMBR, but both aerobic and anaerobic processes had a similar reduction of TOrC abundance. Suspect screening analysis using GC×GC/TOF-MS, which resulted in the tentative identification of 351 TOrCs, proved to be a powerful approach for uncovering compounds previously unreported in wastewater, including many fragrances and personal care products.

An Exploratory Investigation of Organic Chemicals Detected in Baby Teeth: Differences in Children with and without Autism.

Autism spectrum disorder (ASD) is a behaviorally defined neurodevelopmental disorder characterized by deficits in language, communication, and social function with an estimated prevalence rate of between 1 in 30 and 44 U.S. births. Gene/environment (G × E) interactions are widely regarded as the most probable explanation for idiopathic ASD, especially because some genes are selectively targeted by various environmental xenobiotics. Because deciduous teeth are a likely biomarker of in utero exposure, the present study investigated if the quantity of chemicals found in deciduous teeth differs between children with and without ASD. Twenty-two deciduous teeth from children with ASD and 20 teeth from typically developed children were prepared and analyzed using THE Two-Dimensional Gas Chromatography Time-of-Flight Mass Spectrometer (GC × GC-TOF MS) with ChromaTOF version 23H2 software and Agilent 7890 gas chromatograph. The autism sample had significantly more chemicals in their teeth than the typical developing sample (99.4 vs. 80.7, respectively) (p < 0.0001). The majority of chemicals were identified as phthalates, plasticizers, pesticides, preservatives, or intermediary solvents used in the production of fragranced personal care or cleaning products or flavoring agents in foods. The known toxic analytes reported in this study are likely biomarkers of developmental exposure. Why there were greater concentrations of toxic chemicals in the teeth that came from children with ASD is unclear. A further understanding of the cavalcade of multiple biological system interactions (Interactome) could help with future efforts to reduce risks. Notwithstanding, the avoidance of pesticides, plastics, and scented personal care products may be warranted under the precautionary principle rule.

Nontarget screening analysis of organic compounds in river sediments: a case study in the Taipu River of the Yangtze River Delta Region in China.

Sediments are the vital fate of organic compounds, and the recognition of organic compounds in sediments is constructive in providing comprehensive and long-term information. In this study, a three-step nontarget screening (NTS) analysis workflow using comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GC × GC-TOFMS) revealed the extensive existence of organic compounds in the Taipu River sediment. Organic compounds (705) were detected and divided into four structure-related groups or eight use-related classes. In the Taipu River's mainstream, a significant difference was found in the composition profiles of the identified organic compounds among various sites, demonstrating the organic compounds were more abundant in the midstream and downstream than in the upstream. Meanwhile, the hydrodynamic force was recognized as a potential factor influencing organic compounds' occurrence. Based on multiple statistical analyses, the shipping and textile printing industries were considered the significant contributors to the identified organic compounds. Considering the principles of the priority substances and the current status of the substances, two traditional pollutants and ten emerging organic compounds were recognized as the priority organic compounds for the Taipu River. Conclusively, this study established a workflow for NTS analysis of sediment samples and demonstrated the necessity of NTS analysis to evaluate the impact of terrestrial emissions of organic compounds on the aquatic environment.

Metabolite profiling of Piper longum L. fruit volatiles by two-dimensional gas chromatography and time-of-flight mass spectrometry: Insights into the chemical complexity.

Piper longum L. (long pepper) is an economically and industrially important medicinal plant. However, the characterization of its volatiles has only been analyzed by gas chromatography-mass spectrometry (GC-MS). In the present study, precise characterization of P. longum fruit volatiles has been performed for the first time through advanced two-dimensional gas chromatography-time-of-flight spectrometry (GC×GC-TOFMS). A total of 146 constituents accounting for 93.79% were identified, of which 30 were reported for the first time. All these constituents were classified into alcohols (4.5%), alkanes (8.9%), alkenes (6.71%), esters (6.15%), ketones (0.58%), monoterpene hydrocarbons (1.64%), oxygenated monoterpenes (2.24%), sesquiterpene hydrocarbons (49.61%), oxygenated sesquiterpenes (13.03%), phenylpropanoid (0.23%), and diterpenes (0.2%). Among all the classes, sesquiterpene hydrocarbons were abundant, with germacrene-D (2.87% ± 0.01%) as the major one, followed by 8-heptadecene (2.69% ± 0.03%), β-caryophyllene (2.43% ± 0.03%), n-heptadecane (2.4% ± 0.04%), n-pentadecane (2.11% ± 0.05%), and so forth. Further, 20 constituents were observed to be coeluted and separated precisely in the two-dimensional column. The investigation provides an extensive metabolite profiling of P. longum fruit volatiles, which could be helpful to improve its therapeutic potential.