Multidimensional Gas Chromatography Research Articles

Profiling of seized Cannabis sativa L. flowering tops by means of microwave-assisted hydro distillation and gas chromatography analyses

This research aimed to support police forces in their battle against illicit drug trafficking by means of a multi-technique approach, based on gas chromatography. In detail, this study was focused on the profiling of volatile substances in narcotic Cannabis sativa L. flowering tops. For this purpose, the Scientific Investigation Department, RIS Carabinieri of Messina, provided 25 seized samples of Cannabis sativa L. The content of Δ9-tetrahydrocannabinol (THC), useful to classify cannabis plant as hemp (≤ 0.2 %) or as marijuana (> 0.2 %), was investigated. Essential oils of illicit drug samples were extracted using a microwave-assisted hydro-distillation (MAHD) system; GC–MS and GC-FID analytical techniques were used for the characterization of the terpenes and terpenoids fingerprint. Furthermore, the enantiomeric and carbon isotopic ratios of selected chiral compounds were investigated using a heart-cutting multidimensional GC (MDGC) approach. The latter exploited a combination of an apolar column in the first dimension, and a chiral cyclodextrin-based column in the second one, prior to parallel isotope-ratio mass spectrometry (C-IRMS) and MS detection. Finally, all the data were gathered into a statistical model, to demonstrate the existence of useful parameters to be used for the classification of seized samples.

Enhancing Odor Analysis with Gas Chromatography-Olfactometry (GC-O): Recent Breakthroughs and Challenges.

Gas chromatography-olfactometry (GC-O) has made significant advancements in recent years, with breakthroughs in its applications and the identification of its limitations. This technology is widely used for analyzing complex odor patterns. The review begins by explaining the principles of GC-O, including sample preparation, separation methods, and olfactory evaluation techniques. It then explores the diverse range of applications where GC-O has found success, such as food and beverage industries, environmental monitoring, perfume and aroma development, and forensic analysis. One of the major breakthroughs in GC-O analysis is the improvement in separation power and resolution of odorants. Techniques like rapid GC, comprehensive two-dimensional GC, and multidimensional GC have enhanced the identification and quantification of odor-active chemicals. However, GC-O also has limitations. These include the challenges in detecting and quantifying trace odorants, dealing with matrix effects, and ensuring the repeatability and consistency of results across laboratories. The review examines these limitations closely and discusses potential solutions and future directions for improvement in GC-O analysis. Overall, this review presents a comprehensive overview of the recent advances in GC-O, covering breakthroughs, applications, and limitations. It aims to promote the wider usage of GC-O analysis in odor analysis and related industries. Researchers, practitioners, and anyone interested in leveraging the capabilities of GC-O in analyzing complex odor patterns will find this review a valuable resource. The article highlights the potential of GC-O and encourages further research and development in the field.

Changes in the fatty acid profiles and health indexes of bovine colostrum during the first days of lactation and their impact on human health

Our objective was to analyze the changes in fatty acid (FA) profiles of bovine colostrum and immature milk during the first four days of lactation and assess their potential impact on human health. Colostrum and immature milk samples were collected from Czech Fleckvieh cows during their first to third lactation and the FA profiles were analyzed using multidimensional gas chromatography with a vacuum ultraviolet detector (GC×GC-VUV). The colostrum of primiparous cows contained lower levels of medium-chain and saturated fatty acids, and higher levels of mono- and unsaturated fatty acids compared to that of multiparous cows. The atherogenic and thrombogenicity indexes, as well as the hypocholesterolemic-to-hypercholesterolemic fatty acid ratio, were more favourable in primiparous cows. This makes colostrum fat an attractive product for human nutrition. To obtain the maximum health benefits, we recommend collecting and processing the colostrum of primiparous cows and immature milk at the end of the milk transition separately.

Cross-Contamination of Ignitable Liquid Residues on Wildfire Debris—Effects of Packaging and Storage on Detection and Characterization

Producing defensible data for legal proceedings requires strict monitoring of sample integrity. In fire debris analysis, various approved packaging and storage solutions are designed to achieve this by preventing cross-contamination. This study examines the efficiency of current practices at preventing cross-contamination in the presence of a sample matrix (charred wood) via analysis by comprehensive multidimensional gas chromatography coupled with time-of-flight mass spectrometry (GC×GC-ToF MS). The transfer of ignitable liquid residue (ILR) was assessed by comparing percentages of the target ILR area relative to the total chromatogram area and applying chemometric tools developed to detect cross-contamination. All practices reduced cross-contamination in comparison to faulty packaging. Individual practices varied in their performance. Nylon-based packaging performed best, whereas commercial polyethylene-based packaging performed worst due to interfering compounds emitted from the material and sealing mechanism. Heat-sealing was the best sealing mechanism when applied correctly, followed by press-fit connections, and lastly, adhesive sealing. Refrigerated storage offered several advantages, with elevated impact for polyethylene-based packaging and adhesive sealing mechanisms. Triple-layer packaging practices did not show significant benefits over double-layers. The recommended packaging approach based on these findings is mixed-material packaging (metal quart can in a heat-sealed nylon bag), offering advanced prevention of cross-contamination and practical advantages with continued refrigeration during transport.

Vacuum-assisted and multi-cumulative trapping in headspace solid-phase microextraction combined with comprehensive multidimensional chromatography-mass spectrometry for profiling virgin olive oil aroma

In the present work vacuum (Vac) and multiple cumulative trapping (MCT) headspace solid phase microextraction (HS-SPME) were evaluated as alternative or combined techniques for the volatile profiling. A higher extraction performance for semi-volatiles was shown by all three techniques. Synergic combination of Vac and MCT showed up to 5-times extraction power for less volatile compounds. The hyphenation of said techniques with comprehensive two-dimensional gas chromatography (GC × GC) enabled a comprehensive analysis of the volatilome. Firstly, 18 targeted quality markers, previously defined by means of classical HS-SPME, were explored for their ability to classify commercial categories. The applicability of such markers proved to be limited with the alternative sampling techniques. An untargeted approach enables the selection of specific features for each technique showing a better classification capacity of the commercial categories. No misclassifications were observed, except for one extra virgin olive oil classified as virgin olive oil in 3 × 10 min Vac-MCT-HS-SPME.

Solid-phase microextraction coupled to comprehensive multidimensional gas chromatography for food analysis.

Solid-phase microextraction and comprehensive multidimensional gas chromatography represent two milestone innovations that occurred in the field of separation science in the 1990s. They have a common root in their introduction and have found a perfect coupling in their evolution and applications. This review will focus on food analysis, where the paradigm has changed significantly over time, moving from a targeted analysis, focusing on a limited number of analytes at the time, to a more holistic approach for assessing quality in a larger sense. Indeed, not only some major markers or contaminants are considered, but a large variety of compounds and their possible interaction, giving rise to the field of foodomics. In order to obtain such detailed information and to answer more sophisticated questions related to food quality and authenticity, the use of SPME-GC × GC-MS has become essential for the comprehensive analysis of volatile and semi-volatile analytes. This article provides a critical review of the various applications of SPME-GC × GC in food analysis, emphasizing the crucial role this coupling plays in this field. Additionally, this review dwells on the importance of appropriate data treatment to fully harness the results obtained to draw accurate and meaningful conclusions.

A two-run heart-cut multidimensional gas chromatography method using flame ionization and mass spectrometry for automated and robust determination of nearly complete wine aroma-volatile profiles

A quantitative analytical method capable of determining the concentrations of 81 aroma-relevant wine volatiles covering nine orders of magnitude was developed and validated in this study. The method is based on stir bar sorptive extraction (SBSE) of 200 μL of wine diluted with 1.8 mL NaCl brine with pH 3.5. Volatiles thermally desorbed from the stir bars were separated in two runs in a heart-cut multidimensional gas chromatographic system and quantified using either a flame ionization detector (FID) in the first dimension (27 aroma compounds) or a mass spectrometer in the second dimension (54 aroma compounds, transferred to 22 cuts). Typical limits of compound detection lay around 0.02 mg/L by FID or ranged from 0.001 to 0.30 μg/L by mass spectrometry detector, liying below the corresponding odor thresholds in all cases. Linearity, reproducibility, and recovery were considered satisfactory for most compounds, with typical R2 values of 0.989–0.999, relative standard deviation below 10 % for 37 compounds and between 10 and 20 % for 44 compounds, and recovery rates of approximately 100 % (85–109 %) for all but acetaldehyde. An analysis of 20 wine samples completed our validation of the method, showing that a single-sample preparation procedure combined with heart-cut multidimensional two-detector gas chromatography can determine wine volatile concentrations ranging from 350 mg/L of isoamyl alcohol to 3.8 ng/L of 3-isobutyl-2-methoxypyrazine.

Leveraging the use of ionic liquid capillary columns and GC×GC-MS for fatty acid profiling in human colostrum samples.

Lipids in human colostrum provide the majority of energy intake and essential fatty acids for developing infants. The fatty acid composition of human colostrum is highly variable and influenced by multiple factors. Human colostrum is a complex sample bringing challenges to fatty acid profiling. This work aimed to optimize the use of ionic liquid (IL) columns and flow-modulated comprehensive two-dimensional gas chromatography coupled to mass spectrometry (FM-GC×GC-MS) for fatty acid profiling in human colostrum. Derivatization strategies were optimized and the elution behavior of fatty acid methyl esters (FAME) on various 1D column phases (Solgel-WAX, SLB-IL60i, SLB-IL76i, and SLB-IL111i). Derivatization with sodium methoxide yielded a satisfactory recovery rate (90%) at milder conditions and reduced time. The use of IL60 as the 1D column provided superior separation, good peak shape, and better utilization of elution space. As a proof of concept, the developed method was applied to access the effects of the mode of neonatal delivery (vaginal vs. C-section) on the fatty acid profile of human colostrum samples. The integrated multidimensional gas chromatography strategy improved FAME detection and separation and can be a useful tool for accessing the effects of different factors on the fatty acid profiling of complex samples.

Optimizing the identification of thiols in red wines using new oak-wood accelerated reductive treatment

This study proposes a new method for identifying thiols in red wines by mimicking specific chemical mechanisms that occur during bottle-aging. It involves the reaction of oak-wood extracts with hydrogen sulfide and the reduction of disulfides with DIBAL. After optimization of the reaction conditions, the aroma of fresh oak wood turned into intense “meaty” nuances reminiscent of the aging bouquet of red wines. Samples were analyzed by gas chromatography coupled with olfactometry (GC-O) and coupled with a pulsed flame photometric detector. This resulted in the identification of six odorant zones with meaty descriptors associated with sulfur compounds. One of the odorant zones was identified as 2-methoxybenzenethiol by using heart-cutting multidimensional GC coupled with olfactometry and time of flight mass spectrometer. Its identification in aged red wines was confirmed by GC coupled with tandem mass spectrometry analyses. Five other thiols associated with oak-wood precursors were also identified in red wines.

Identification, Quantitation, and Sensory Evaluation of Thiols in Bordeaux Red Wine with Characteristic Aging Bouquet.

Great Bordeaux red wines are known for their distinctive aging bouquet. However, the nature of volatile chemicals underpinning this sensory expression is not fully understood. This work investigated the empyreumatic aging bouquet of a collection of premium Bordeaux red wines using silver-ion (Ag+) solid-phase extraction, cryogenic heart-cutting multidimensional gas chromatography mass spectrometry/olfactometry, and comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry. In doing so, a substantial number of "meaty" odors were revealed. Three detected "meaty" notes were tentatively or unequivocally attributed to furan thiols. Among them, 2-methyltetrahydrofuran-3-thiol (1) with a pleasant "meaty" aroma was reported in wine for the first time. Its trans isomer (trans-1a) was resolved from its racemate by chemical modification, which confirmed its presence in wine. The odor detection threshold of trans-1a in the model wine was determined at 55 ng/L. Moreover, an additive effect between 1 and literature-known 2-methyl-3-furanthiol was observed. By a new ultra high-performance liquid chromatography quadrupole Orbitrap high-resolution mass spectrometry method, the concentration of trans-1a, in addition to those of 2-methyl-3-furanthiol and 2-furfuryl thiol, was measured in the wines at ng/L levels.

Association between flavor composition and sensory profile in thermally processed mandarin juices by multidimensional gas chromatography and multivariate statistical analysis.

Thermal pasteurization decreases the sensory quality of mandarin juice. Flavor composition was determined in four fresh-squeezed and heat-processed mandarin juice varieties using molecular sensory science approaches. The relationships between odorants and sensory profiles were analyzed, and markers for flavor deterioration were screened by multivariate statistical analysis. Seventy-four volatiles were identified, among which 36 odorants with flavor dilution factors ranging from 2 to 128 were detected by multidimensional gas chromatography-mass spectrometry/olfactometry (MDGC-MS/O) coupled with aroma extract dilution analysis (AEDA). Higher intensities of cooked and off-flavor notes were observed in the heated mandarin juice, which was related to the concentration changes of the methional, methanethiol, dimethyl sulfide, and carbon disulfide by partial least squares (PLS) analysis. Ten potential markers (methional, methanethiol, dimethyl sulfide, hydrogen sulfide, β-damascenone, camphene, trans-β-ionone, decanal, d-limonene, and α-pinene) were responsible for the sensory discrimination of fresh-squeezed and heated mandarin juices.

Preparative three-dimensional GC and nuclear magnetic resonance for the isolation and identification of two sesquiterpene ethers from Dictyota Dichotoma.

Separation science plays a crucial role in the isolation of novel compounds contained in complex matrices. Yet their rationale employment needs preliminary structure elucidation, which usually requires sufficient aliquots of grade substances to characterize the molecule by nuclear magnetic resonance experiments. In this study, two peculiar oxa-tricycloundecane ethers were isolated by means of preparative multidimensional gas chromatography from the brown alga species Dictyota dichotoma (Huds.) Lam., aiming to assign their 3D structures. Density functional theory simulations were carried out to select the correct configurational species matching the experimental NMR data (in terms of enantiomeric couples). In this case, the theoretical approach was crucial as the protonic signal overlap and spectral overcrowding were preventing any other unambiguous structural information. Just after the identification through the density functional theory data matching of the correct relative configuration it was possible to verify an enhanced self-consistency with the experimental data, confirming the stereochemistry. The results obtained further pave the way toward structure elucidation of highly asymmetric molecules, whose configuration cannot be inferred by other means or strategies.

Tijuca forest contribution to the improvement of air quality and wellbeing of citizens in the city of Rio de Janeiro, Brazil

The Tijuca Forest, one of the largest urban forests in the world, is a protected area of the Brazilian Atlantic Forest, one of the world's biodiversity hotspots. The forest and the Metropolitan Region of Rio de Janeiro coexist and interact, but their mutual influence regarding air quality is still not well known and a more detailed study is needed. Here, air samples were collected inside the forest, in Tijuca National Park (TNP) and Grajaú State Park (GSP) and in two representative urban areas (Tijuca and Del Castilho Districts). Sampling was performed using stainless steel canisters, and ozone precursor hydrocarbons (HCs) were analyzed with the aid of heart-cutting multidimensional gas chromatography. The sampling points within the forest are currently visited by hundreds of people. Total HC concentrations within the green area were clearly lower than in the urbanized districts, in spite of the anthropogenic impact of visitors and the proximity of the urban area. Median values were 21.5, 35.5, 57.9 and 148.6 μg m−3 at TNP, GSP, Tijuca and Del Castilho, respectively. Total HC concentrations were Del Castilho > Tijuca > GSP > TNP. The kinetic reactivity and ozone-forming potential of individual HCs were evaluated, as well as the intrinsic reactivity of air masses. The air masses in the urbanized area showed a higher average reactivity in all scales. In fact, in spite of the forest's contribution to isoprene emissions, its net contribution to ozone formation was lower than that of urbanized air masses, owing to a reduction in HC concentration, particularly for alkenes and monoaromatic compounds. It is not clear if the forest plays a role in the adsorption of pollutants or if it acts as a physical natural barrier to air masses carrying pollutants. Nonetheless, improving air quality within Tijuca Forest is essential to the welfare of citizens.

Development and validation of a GC × GC-ToFMS method for the quantification of pesticides in environmental waters

Water is a fundamental resource for living things, which is why its control is necessary. The widespread use of pesticides for agricultural and non-agricultural purposes has resulted in the presence of their residues in surface water and groundwater resources. Their presence in water is regulated through different directives, such as the Groundwater Directive, the Drinking Water Directive, and the Water Framework Directive, modified later several times, setting a maximum concentration of 0.1 µg.L−1 for individual pesticides and their degradation products, and 0.5 µg.L−1 for total pesticide residues present in a sample. There are different kinds of pesticides (e.g., organophosphorus and organochlorine pesticides, triazines, chloroacetamides, triazoles, (thio)carbamates) that have diverse chemical structures. Their determination and monitoring in a single analytical procedure are possible through multiresidue methods. In this study, 53 pesticides belonging to different chemical classes and their metabolites were selected based on their local occurrence and investigated in surface water and groundwater from agricultural areas susceptible to pesticide contamination. The methodology consisted of a classical solid-phase extraction (SPE) for the purification and enrichment of the pesticides, with a subsequent analysis in multidimensional gas chromatography coupled to mass spectrometry (GC×GC-MS). The quantification method was validated according to the Eurachem Guide in terms of linearity, precision, accuracy, limit of detection, and limit of quantification. After validation, the method was applied to 34 real-world water samples, and the results were compared with those obtained by a GC-QMS routine method.

Comparison of olefin/paraffin separation by ionic liquid and polymeric ionic liquid stationary phases containing silver(I) ion using one-dimensional and multidimensional gas chromatography

Silver(I) ions have been used in various studies as components within polymer membranes or ionic liquids (ILs) to enable separation of olefins from paraffins. Polymeric ionic liquids (PILs) are a class of polymers synthesized from IL monomers and typically possess higher thermal and chemical stability than the ILs from which they are formed. Until now, very little is known about the difference in strength of silver(I) ion-olefin interactions when they take place in an IL compared to a PIL. In this work, the chromatographic separation of olefins by stationary phases composed of silver(I) bis[(trifluoromethyl)sulfonyl]imide ([Ag+][NTf2−]) incorporated into the 1-hexyl-3-methylimidazolium NTf2 ([HMIM+][NTf2−]) IL and poly(1-hexyl-3-vinylimidazolium NTf2) (poly([HVIM+][NTf2−])) PIL at varying concentrations was investigated. Olefins were more highly retained by silver(I) ions in PILs than in ILs as the silver(I) salt concentration in the stationary was increased. The potential separation power of silver(I)-containing IL and PIL stationary phases in comprehensive two-dimensional gas chromatography (GC×GC) was compared to the conventional one-dimensional system. The separation selectivity of alkenes and alkynes from paraffins was significantly increased, while dienes and aromatic compounds showed insignificant changes in retention. The chemical structural features of IL and PIL that enhance silver(I) ion stability and olefin separation were investigated by using silver(I) trifluoromethanesulfonate ([Ag+][OTf−]), 1-decyl-3-methylimidazolium NTf2 ([DMIM+][NTf2−]) IL, poly(1-decyl-3-vinylimidazolium NTf2 (poly([DVIM+][NTf2−])) PIL, [HMIM+][OTf−] IL and poly([HVIM+][OTf−]) PIL. Longer alkyl substituents appended to the IL (and PIL) cation increased the strength of silver(I) olefin interaction, and [OTf−] anions in the IL (and PIL) tended to preserve silver(I) ion from thermal reduction, while also retaining olefins less than the [NTf2−]-containing columns. In general, silver(I) ions in PILs possessing analogous chemical structures to ILs exhibited higher silver(I) ion-olefin interaction strength but were less thermally stable.

Comprehensive analysis of floral scent and fatty acids in nectar of Silene nutans through modern analytical gas chromatography techniques

The aim of this work was to show the potential of multidimensional gas chromatography combined with mass spectrometry and suitable chemometrics means based on untargeted and profiling data analysis to strengthen the information provided by floral scent and nectar fatty acids of four genetically differentiated lineages (E1, W1, W2, and W3) of the nocturnal moth-pollinated herb Silene nutans. Volatile organic compounds emitted by flowers were trapped for a total of 42 samples by in-vivo sampling dynamic head space for analysing floral scent by untargeted approach, while 37 samples of nectar were collected for analysing fatty acids through profiling analysis. The resulting data from floral scent analysis were aligned and compared using a tile-based methodology followed by data mining to access high-level information. Based on floral scent and nectar fatty acid results, it was possible to distinguish E1 from the W lineages, and W3 from W1 and W2. This work puts the bases for a larger study aiming to clarify the existence of prezygotic barriers involved in speciation among lineages of S. nutans, and thus the possible implication of different flower scents and nectar compositions in this phenomenon.

A multifunction flow channel switching module for multi-column capillary gas chromatography using silicon pneumatic microvalves

Decades ago, multi-column GC was developed for separating analytes which cannot be separated with a single column by switching the flow channels and introducing them into multiple columns. Formerly, a channel switching system consisted of stainless-tube-type packed columns and multi-port switching valves which were connected by stainless-steel pipes. These systems utilizing packed columns are still widely used today, mainly for gas analysis, especially for refinery gas analysis and natural gas analysis related to oil refining. However, there have been no new development updates in terms of hardware for decades. Since multi-port switching valves are used, there are problems such as the high frequency of valve replacements due to wear of seals, high running costs as well as long downtimes. In recent years, a heart-cutting multidimensional capillary GC using pressure switching devices such as the Deans switch has been put into practical use. Compared to the switching valves, the pressure switching devices have no wearing parts and are maintenance-free. Multi-dimensional capillary GC using the pressure-switching method cannot be applied to the analysis of low-boiling-point gasses because the retention capacity of the capillary column is low and the column inlet pressure is far from the optimum value for switching. Because of this another related factors, it has not been able to completely replace the traditional methods. In this study, an ON/OFF type silicon pneumatic microvalve was designed and fabricated by semiconductor manufacturing technology, and a flow channel switching module was developed by mounting microvalves on a metallic channel plate which is made by diffusion bonding. The flow channel switching module using silicon pneumatic microvalves has a heat resistance of up to 310 °C, can withstand pressures up to 1.5 MPA or more, and a durability that can withstand over 2 million opening and closing operations. In addition, the reproducibility of the gas sample analysis showed good reproducibility values of RSD 0.1% or less for peak areas and RSD 0.01 to 0.04% for retention time. Flow path switching without the use of pressure switching simplifies method development in several ways. For instance, by incorporating the use of valves that can be opened and closed independently, it was possible to integrate several methods such as heart cut, precut, column switching, and backflushing flow path layouts.

Multidimensional Gas Chromatography of Organosulfur Compounds in Coffee and Structure-Odor Analysis of 2-Methyltetrahydrothiophen-3-one.

Organosulfur compounds (OSCs) in coffee remain challenging to analyze by conventional gas chromatography (GC) due to their low concentrations amid coffee's complex matrix and susceptibility to chiral-odor influences. In this study, multidimensional GC (MDGC) methods were developed to profile OSCs in coffee. Conventional GC was compared to comprehensive GC (GC×GC) for untargeted OSC analysis in eight specialty coffees, and GC×GC was found to improve the fingerprinting of OSCs in coffee (50 vs 16 OSCs identified). Of the 50 OSCs, 2-methyltetrahydrothiophen-3-one (2-MTHT) was of high interest due to its chirality and known aroma contribution. Following that, a heart-cutting method for chiral GC (GC-GC) was developed, validated, and applied to the coffees. The mean enantiomer ratio of 2-MTHT was observed to be 1.56 (R/S) in brewed coffees. Overall, MDGC techniques allowed for more comprehensive analyses of coffee OSCs, from which (R)-2-MTHT was found to be the predominant enantiomer with the lower odor threshold.

Foods and Contaminants Analysis Using Multidimensional Gas Chromatography: An Update of Recent Studies, Technology, and Applications.

ADVERTISEMENT RETURN TO ISSUEPREVReviewNEXTFoods and Contaminants Analysis Using Multidimensional Gas Chromatography: An Update of Recent Studies, Technology, and ApplicationsYada NolvachaiYada NolvachaiAustralian Centre for Research on Separation Science, School of Chemistry, Monash University, Wellington Road, Clayton, Victoria 3800, AustraliaMore by Yada NolvachaiView Biographyhttps://orcid.org/0000-0002-8436-1836, Michelle S. S. AmaralMichelle S. S. AmaralAustralian Centre for Research on Separation Science, School of Chemistry, Monash University, Wellington Road, Clayton, Victoria 3800, AustraliaMore by Michelle S. S. AmaralView Biography, and Philip J. Marriott*Philip J. MarriottAustralian Centre for Research on Separation Science, School of Chemistry, Monash University, Wellington Road, Clayton, Victoria 3800, Australia*E-mail: [email protected]. Phone: +61-(3)-99059630. Fax: +61-(3)-99054597.More by Philip J. MarriottView Biographyhttps://orcid.org/0000-0001-5180-1041Cite this: Anal. Chem. 2023, 95, 1, 238–263Publication Date (Web):January 10, 2023Publication History Published online10 January 2023Published inissue 10 January 2023https://doi.org/10.1021/acs.analchem.2c04680Copyright © 2023 American Chemical SocietyRIGHTS & PERMISSIONSArticle Views304Altmetric-Citations-LEARN ABOUT THESE METRICSArticle Views are the COUNTER-compliant sum of full text article downloads since November 2008 (both PDF and HTML) across all institutions and individuals. These metrics are regularly updated to reflect usage leading up to the last few days.Citations are the number of other articles citing this article, calculated by Crossref and updated daily. Find more information about Crossref citation counts.The Altmetric Attention Score is a quantitative measure of the attention that a research article has received online. Clicking on the donut icon will load a page at altmetric.com with additional details about the score and the social media presence for the given article. Find more information on the Altmetric Attention Score and how the score is calculated. Share Add toView InAdd Full Text with ReferenceAdd Description ExportRISCitationCitation and abstractCitation and referencesMore Options Share onFacebookTwitterWechatLinked InReddit Read OnlinePDF (9 MB) Get e-AlertsSUBJECTS:Chromatography,Food,Food analysis,Modulators,Volatile organic compounds Get e-Alerts

Investigation of the effect of refining on the presence of targeted mineral oil aromatic hydrocarbons in coconut oil

The goal of this work was to investigate the impact of refining on coconut oil particularly on the most toxicologically relevant fraction of the mineral oil aromatic hydrocarbon (MOAH) contamination, namely the fraction composed by the three to seven aromatic rings. A fully integrated platform consisting of a liquid chromatography (LC), a comprehensive multidimensional gas chromatography (GC) (LC-GC × GC) and flame ionization detector (FID) was used to obtained a more detailed characterization of the MOAH sub-classes distribution. The revised EN pr 16995:2017-08 official method was used for preparing the samples, both with and without the auxiliary epoxidation step. Crude coconut oil was spiked with different MOAH standards, namely naphthalenes, alkylated naphthalenes, benzo(a)pyrene, and its alkylated homologues. Refining was modelled by deodorization at 230 °C, stripping with 10 kg/h of steam under 1 mbar vacuum for 3 h. Complete removal of the naphthalenes and reduction of more than 98.8% of the benzo(a)pyrenes was observed. Epoxidation had a significant impact on the MOAH fraction with more than three rings, but with a high dependency on the sample matrix, being significantly less evident in the refined samples than in the crude ones.