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The role of comprehensive two-dimensional gas chromatography in mineral oil determination
Mineral oil hydrocarbons (MOH) contain a wide structural diversity of molecules, for which the reference method of analysis is the online coupled liquid chromatography-gas chromatography with flame ionization detection (LC-GC-FID). These compounds are very heterogeneous from a toxicological viewpoint, and an accurate risk assessment when dealing with a MOH contamination can only be performed if sufficient information is available on the types of structures present (i.e., number of carbons, degree of alkylation, number of aromatic rings). Unfortunately, the separation performances of the current LC-GC-FID method are insufficient for such characterization, not even mentioning the possible coelution of interfering compounds which additionally hinder MOH determination. Comprehensive two-dimensional gas chromatography (GC × GC), while mostly used for confirmation purposes in the past, starts to prove its relevance for overcoming the weaknesses of the LC-GC method and reaching even better the analytical requirements defined in the latest EFSA opinion. The present paper therefore aims at highlighting how GC × GC has contributed to the understanding of the MOH topic, how it has developed to meet the requirements of MOH determination, and how it could play a role in the field for overcoming many of the current analytical and toxicological challenges related to the topic.
Journal Article
Comparison on aroma compounds in Chinese soy sauce and strong aroma type liquors by gas chromatography–olfactometry, chemical quantitative and odor activity values analysis
In order to elucidate the differences on aroma compounds in Chinese liquors with different aroma styles and the reasons, aroma compounds of Xijiu in soy sauce aroma and strong aroma type were investigated in the research. By gas chromatography–olfactometry (GC–O), aroma compounds in Chinese liquor were chosen for quantitative and odor activity value (OAV) analysis. Ethyl hexanoate, butanoic acid, 3-methylbutanoic acid, hexanoic acid and dimethyl trisulfide were considered to be the most powerful odorants in both liquor samples (aroma intensity ≥3.5) by GC–O. As important aroma compounds (OAV ≥10) in the liquors, ethyl propanoate, ethyl 2-methylpropanoate and 1-propanol were considered with much higher OAVs in soy sauce aroma type liquor, while OAVs of ethyl pentanoate, ethyl hexanoate, ethyl heptanoate, ethyl octanoate, ethyl lactate, hexyl acetate, butyl hexanoate, hexyl hexanoate and hexanoic acid were far lower in strong aroma type liquor. The OAV of ethyl hexanoate in strong aroma type liquor exceeded 50,000, which explained the reason why strong aroma liquor was considered with prominent fruity aroma. The odor differences between the liquors were mainly caused by the manufacturing practices.
Journal Article
Identification of terpenes and essential oils by means of static headspace gas chromatography-ion mobility spectrometry
Static headspace gas chromatography-ion mobility spectrometry (SHS GC-IMS) is a relatively new analytical technique that has considerable potential for analysis of volatile organic compounds (VOCs). In this study, SHS GC-IMS was used for the identification of the major terpene components of various essential oils (EOs). Based on the data obtained from 25 terpene standards and 50 EOs, a database for fingerprint identification of characteristic terpenes and EOs was generated utilizing SHS GC-IMS for authenticity testing of fragrances in foods, cosmetics, and personal care products. This database contains specific normalized IMS drift times and GC retention indices for 50 terpene components of EOs. Initially, the SHS GC-IMS parameters, e.g., drift gas and carrier gas flow rates, drift tube, and column temperatures, were evaluated to determine suitable operating conditions for terpene separation and identification. Gas chromatography-mass spectrometry (GC-MS) was used as a reference method for the identification of terpenes in EOs. The fingerprint pattern based on the normalized IMS drift times and retention indices of 50 terpenes is presented for 50 EOs. The applicability of the method was proven on examples of ten commercially available food, cosmetic, and personal care product samples. The results confirm the suitability of SHS GC-IMS as a powerful analytical technique for direct identification of terpene components in solid and liquid samples without any pretreatment.
Graphical abstract
Fingerprint pattern identification of terpenes and essential oils using static headspace gas chromatography-ion mobility spectrometry.
Journal Article
Mass spectrometry-based metabolomics: a guide for annotation, quantification and best reporting practices
Mass spectrometry-based metabolomics approaches can enable detection and quantification of many thousands of metabolite features simultaneously. However, compound identification and reliable quantification are greatly complicated owing to the chemical complexity and dynamic range of the metabolome. Simultaneous quantification of many metabolites within complex mixtures can additionally be complicated by ion suppression, fragmentation and the presence of isomers. Here we present guidelines covering sample preparation, replication and randomization, quantification, recovery and recombination, ion suppression and peak misidentification, as a means to enable high-quality reporting of liquid chromatography– and gas chromatography–mass spectrometry-based metabolomics-derived data.This Perspective, from a large group of metabolomics experts, provides best practices and simplified reporting guidelines for practitioners of liquid chromatography– and gas chromatography–mass spectrometry-based metabolomics.
Journal Article
Bioaccumulation of microplastics in decedent human brains
Rising global concentrations of environmental microplastics and nanoplastics (MNPs) drive concerns for human exposure and health outcomes. Complementary methods for the robust detection of tissue MNPs, including pyrolysis gas chromatography–mass spectrometry, attenuated total reflectance–Fourier transform infrared spectroscopy and electron microscopy with energy-dispersive spectroscopy, confirm the presence of MNPs in human kidney, liver and brain. MNPs in these organs primarily consist of polyethylene, with lesser but significant concentrations of other polymers. Brain tissues harbor higher proportions of polyethylene compared to the composition of the plastics in liver or kidney, and electron microscopy verified the nature of the isolated brain MNPs, which present largely as nanoscale shard-like fragments. Plastic concentrations in these decedent tissues were not influenced by age, sex, race/ethnicity or cause of death; the time of death (2016 versus 2024) was a significant factor, with increasing MNP concentrations over time in both liver and brain samples (
P
= 0.01). Finally, even greater accumulation of MNPs was observed in a cohort of decedent brains with documented dementia diagnosis, with notable deposition in cerebrovascular walls and immune cells. These results highlight a critical need to better understand the routes of exposure, uptake and clearance pathways and potential health consequences of plastics in human tissues, particularly in the brain.
Pyrolysis gas chromatography–mass spectrometry reveals the presence of microplastics and nanoplastics in human kidney, liver and brain tissue samples from 2016 and 2024, with higher proportions found in the brain.
Journal Article
Comparison of pyrolysis gas chromatography/mass spectrometry and hyperspectral FTIR imaging spectroscopy for the analysis of microplastics
Analysis of microplastics (MP) in environmental samples is an emerging field, which is performed with various methods and instruments based either on spectroscopy or thermoanalytical methods. In general, both approaches result in two different types of data sets that are either mass or particle number related. Depending on detection limits of the respective method and instrumentation the derived polymer composition trends may vary. In this study, we compare the results of hyperspectral Fourier-transform infrared (FTIR) imaging analysis and pyrolysis gas chromatography-mass spectrometry (Py-GC/MS) analysis performed on a set of environmental samples that differ in complexity and degree of microplastic contamination. The measurements were conducted consecutively, and on exactly the same sample. First, the samples were investigated with FTIR using aluminum oxide filters; subsequently, these were crushed, transferred to glass fiber filters, in pyrolysis cups, and measured via Py-GC/MS. After a general data harmonization step, the trends in MP contamination were thoroughly investigated with regard to the respective sample set and the derived polymer compositions. While the overall trends in MP contamination were very similar, differences were observed in the polymer compositions. Furthermore, polymer masses were empirically calculated from FTIR data and compared with the Py-GC/MS results. Here, a most plausible shape-related overestimation of the calculated polymer masses was observed in samples with larger particles and increased particle numbers. Taking into account the different measurement principles of both methods, all results were examined and discussed, and future needs for harmonization of intermethodological results were identified and highlighted.
Journal Article
Physicochemical characterization and quantification of nanoplastics: applicability, limitations and complementarity of batch and fractionation methods
A comprehensive physicochemical characterization of heterogeneous nanoplastic (NPL) samples remains an analytical challenge requiring a combination of orthogonal measurement techniques to improve the accuracy and robustness of the results. Here, batch methods, including dynamic light scattering (DLS), nanoparticle tracking analysis (NTA), tunable resistive pulse sensing (TRPS), transmission electron microscopy (TEM), and scanning electron microscopy (SEM), as well as separation/fractionation methods such as centrifugal liquid sedimentation (CLS) and field-flow fractionation (FFF)–multi-angle light scattering (MALS) combined with pyrolysis gas chromatography mass spectrometry (pyGC–MS) or Raman microspectroscopy (RM) were evaluated for NPL size, shape, and chemical composition measurements and for quantification. A set of representative/test particles of different chemical natures, including (i) polydisperse polyethylene (PE), (ii) (doped) polystyrene (PS) NPLs, (iii) titanium dioxide, and (iv) iron oxide nanoparticles (spherical and elongated), was used to assess the applicability and limitations of the selected methodologies. Particle sizes and number-based concentrations obtained by orthogonal batch methods (DLS, NTA, TRPS) were comparable for monodisperse spherical samples, while higher deviations were observed for polydisperse, agglomerated samples and for non-spherical particles, especially for light scattering methods. CLS and TRPS offer further insight with increased size resolution, while detailed morphological information can be derived by electron microscopy (EM)–based approaches. Combined techniques such as FFF coupled to MALS and RM can provide complementary information on physical and chemical properties by online measurements, while pyGC–MS analysis of FFF fractions can be used for the identification of polymer particles (vs. inorganic particles) and for their offline (semi)quantification. However, NPL analysis in complex samples will continue to present a serious challenge for the evaluated techniques without significant improvements in sample preparation.
Journal Article
Methods and recent advances in speciation analysis of mercury chemical species in environmental samples: a review
Mercury (Hg) and its compounds are much concerned for their high toxicity and wide presence in the environment. Since the toxicity of Hg is species dependent, various methods have been developed for the speciation analysis of Hg. This review focus on the determination and speciation analysis of Hg chemical species in water, sediment, and soil samples. Recent developments on sample pre-treatment and extraction/pre-concentration, separation, and quantification of Hg chemical species, and associated analytical challenges have been reviewed and briefly discussed based on recent reports.
Journal Article
Quantification of microplastics in environmental samples via pressurized liquid extraction and pyrolysis-gas chromatography
The quantification of microplastics (MP) in environmental samples is currently a challenging task. To enable low quantification limits, an analytical method has been developed combining pressurized liquid extraction (PLE) and pyrolysis GC-MS. The automated extraction includes a pre-extraction step via methanol followed by a subsequent PLE using tetrahydrofuran. For the most frequently used synthetic polymers polyethylene (PE), polypropylene (PP), and polystyrene (PS), limits of quantification were achieved down to 0.007 mg/g. Recoveries above 80% were attained for solid matrices such as soil and sediments. The developed method was applied for MP quantification in environmental samples such as sediment, suspended matter, soil, and sewage sludge. In all these matrices, PE and PP were detected with concentrations ranging from 0.03 to 3.3 mg/g. In sewage sludge samples, all three polymers were present with concentration levels ranging between 0.08 ± 0.02 mg/g (PP) and 3.3 ± 0.3 mg/g (PE). However, especially for solid samples, the analysis of triplicates revealed elevated statistical uncertainties due to the inhomogeneous distribution of MP particles. Thus, care has to be taken when milling and homogenizing the samples due to the formation of agglomerates.
Journal Article