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Selenium (Se) is considered to be an essential trace element needed for all living organisms. The importance, deficiency, and toxic effects of Se mainly depend on its quantity and chemical nature. It has been observed that the inorganic versions of Se are more hazardous than the organic versions. This review is mainly focused on the application of different extraction methods used for Se extraction and determination such as microextraction, solid-phase extraction (SPE), and their modified modes in the last 12 years. The use of different dispersive medium (magnetic field, ultrasonic radiation, and vortex agitator) to enhance Se separation is also part of this review. The usage of environmentally friendly solvents such as supramolecular solvents, hydrophobic deep eutectic solvents (DESs), and ionic liquids (ILs) are also the focus of attention in this review. This review is also emphasized the application of advanced microextraction methods, particularly liquid-phase microextraction (LPME). The most recent advances in LPME extraction techniques for Se in various environmental samples, as well as their prospects, are reviewed. Additionally, a summary of cheap, simple, and accurate techniques that have not yet been used to determine small amounts of Se has been provided. [ABSTRACT FROM AUTHOR]

Methyltrimethoxysilane (MTMS) modified tin dioxide microspheres (MTMS/SnO2) were prepared by a facile hydrothermal method and heated reflux reaction strategy. The characterization results indicate that the modification of MTMS induced the formation of a hydrophobic network within the composites, while maintaining abundant adsorbed oxygen species. Subsequently, the MTMS/SnO2 microspheres were used as a solid-phase microextraction (SPME) coating for the efficient extraction and sensitive determination of trace polychlorinated biphenyls (PCBs) in aqueous solutions coupled to gas chromatography-mass spectrometry. MTMS/SnO2 coating exhibited superior extraction performances for PCBs compared with commercial SPME and pure SnO2 microspheres coatings, owing to the hydrophobic crosslinking and adsorbed oxygen-enhanced hydrogen bonding. The proposed analytical method presented respectable linearity in the concentration range 0.25–1000 ng L−1, with low limits of detection varying from 0.036 to 0.14 ng L−1 for seven PCBs and excellent precision, with relative standard deviations of 5.7–9.8% for a single fiber and 8.2–13.1% for five fibers. Finally, the proposed method was successfully used for determination of PCBs in real water with recoveries ranging from 75.8 to 115.6%. This study proposed a new type SPME coating of MTMS/SnO2 microspheres, which extended the potential of SnO2 in capturing and determining organic pollutants. [ABSTRACT FROM AUTHOR]

Sample preparation is one of the viable procedures to be used before analysis to enhance sensitivity and reduce the matrix effect. The current review is mainly emphasized the latest outcome and applications of microextraction techniques based on the miniaturization of the classical conventional methods based on liquid-phase and solid-phase extraction for the quantitative elemental analysis in different real samples. The limitation of the conventional sample preparation methods (liquid and solid phase extraction) has been overcome by developing a new way of reducing size as compared with the conventional system through the miniaturization approach. Miniaturization of the sample preparation techniques has received extensive attention due to its extraction at microlevels, speedy, economical, eco-friendly, and high extraction capability. The growing demand for speedy, economically feasible, and environmentally sound analytical approaches is the main intention to upgrade the conventional procedures apply for sample preparation in environmental investigation. A growing trend of research has been perceived to quantify the trace for elemental analysis in different natures of real samples. This review also recapitulates the current futuristic scenarios for the green and economically viable procedure with special overemphasis and concentrates on eco-friendly miniaturized sample-preparation techniques such as liquid-phase microextraction (LPME) and solid-phase microextraction (SPME). This review also emphasizes the latest progress and applications of the LPME and SPME approach and their future perspective. [ABSTRACT FROM AUTHOR]

This manuscript proposes a new extraction method for analyzing natural compounds in herbal supplements for weight loss and determining adulterants by a comprehensive two-dimensional gas chromatography system coupled to a quadrupole time-of-flight mass spectrometer (GCxGC/Q-TOFMS). In this new approach, a hydrophilic microporous cartridge (HMCart) was developed to enclose the samples, protecting the SPME (solid-phase microextraction) fibers. The cartridge is loaded with herbal supplement samples during direct immersion of SPME fiber in the aqueous phase to allow the analytes to be trapped. The new sample preparation method using chromatographic analyses enabled the detection of 650 compounds, including natural compounds, such as terpenes, aldehydes, ketones, and fatty acids. Adulterants found in other studies in the literature, such as sibutramine and ephedrine. The fluoxetine and caffeine were detected and quantified. The new method has achieved the goal of simple, effective, solvent-free, and versatile sample preparation that can be applied in future studies, including determining other compound classes in various matrix samples. [ABSTRACT FROM AUTHOR]

The ubiquitous presence and persistence of per‐ and polyfluoroalkyl substances (PFAS) in the environment have raised concerns in the scientific community. Current research efforts are prioritizing effective PFAS remediation through novel sorbents with orthogonal interaction mechanisms. Recognized sorption mechanisms between PFAS and sorbents include hydrophobic, electrostatic, and fluorine‐fluorine interaction. The interplay of these mechanisms contributes significantly to improved sorption capacity and selectivity in PFAS separations. In this study, a primary/secondary amine‐functionalized polystyrene‐divinylbenzene (Sepra‐WAX) polymer was modified to create a fluorinated WAX resin (Sepra‐WAX‐KelF‐PEI). The synthesis intermediate (Sepra‐WAX‐KelF) was also tested to assess the improvement of the final product (Sepra‐WAX‐KelF‐PEI). The adsorption capacity of Sepra‐WAX, Sepra‐WAX‐KelF, and Sepra‐WAX‐KelF‐PEI, and their interactions with PFAS were evaluated. The effect of pH, ionic strength, and organic solvents on PFAS sorption in aqueous solution was also investigated. The sorbents showed varied adsorption capacities for perfluorooctanoic acid, perfluoropentanoic acid, perfluoro‐n‐decanoic acid, and hexafluoropropylene oxide dimer acid, with the average extraction capacity of the four analytes being Sepra‐WAX‐KelF‐PEI (523 mg/g) > Sepra‐WAX (353 mg/g) > Sepra‐WAX‐KelF (220 mg/g). Sepra‐WAX‐KelF‐PEI provided the highest adsorption capacity for all analytes tested, proving that the combination of electrostatic and hydrophobic/fluorophilic interactions is crucial for the effective preconcentration of PFAS and its future applications for PFAS remediation from aqueous solutions. [ABSTRACT FROM AUTHOR]

Solid-phase microextraction (SPME) has been widely proposed for the extraction, clean-up, and preconcentration of analytes of environmental concern. Enrichment capabilities, preconcentration efficiency, sample throughput, and selectivity in extracting target compounds greatly depend on the materials used as SPME coatings. Supramolecular materials have emerged as promising porous coatings to be used for the extraction of target compounds due to their unique selectivity, three-dimensional framework, flexible design, and possibility to promote the interaction between the analytes and the coating by means of multiple oriented functional groups. The present review will cover the state of the art of the last 5 years related to SPME coatings based on metal organic frameworks (MOFs), covalent organic frameworks (COFs), and supramolecular macrocycles used for environmental applications. [ABSTRACT FROM AUTHOR]

Capillary zone electrophoresis-mass spectrometry (CZE-MS) has been recognized as a valuable technique for the proteomics of mass-limited biological samples (i.e., single cells). However, its broad adoption for single cell proteomics (SCP) of human cells has been impeded by the low sample loading capacity of CZE, only allowing us to use less than 5% of the available peptide material for each measurement. Here we present a reversed-phase-based solid-phase microextraction (RP-SPME)-CZE-MS platform to solve the issue, paving the way for SCP of human cells using CZE-MS. The RP-SPME-CZE system was constructed in one fused silica capillary with zero dead volume for connection via in situ synthesis of a frit, followed by packing C8 beads into the capillary to form a roughly 2 mm long SPME section. Peptides captured by SPME were eluted with a buffer containing 30% (v/v) acetonitrile and 50 mM ammonium acetate (pH 6.5), followed by dynamic pH junction-based CZE-MS. The SPME-CZE-MS enabled the injection of nearly 40% of the available peptide sample for each measurement. The system identified 257 ± 24 proteins and 523 ± 69 peptides (N = 2) using a Q-Exactive HF mass spectrometer when only 0.25 ng of a commercial HeLa cell digest was available in the sample vial and 0.1 ng of the sample was injected. The amount of available peptide is equivalent to the protein mass of one HeLa cell. The data indicate that SPME-CZE-MS is ready for SCP of human cells. [ABSTRACT FROM AUTHOR]

The study examines the unique production process of Aceto Balsamico Tradizionale di Modena PDO (ABTM), emphasizing its complex phases and the impact of raw materials and artisanal skill on its flavor characteristics. Analytical tests focused on the volatile composition of vinegars from different wood barrels at different aging stages, using solid-phase micro-extraction (SPME) coupled with gas chromatography, either with mass spectrometry (GC/MS) or flame ionization detector (FID). Multivariate analysis, including principal component analysis (PCA), was employed to investigate the presence of peculiarities among the volatile profiles of samples of different barrel origin. The research focuses on characterizing the volatile composition of vinegars sourced from individual wood barrels, such as Cherry, Chestnut, Mulberry, Juniper, and Oak. Although it was not possible to identify molecules directly connected to the woody essence, some similarities emerged between vinegar samples from mulberry and cherry barrels and between those of juniper and oak. The former group is characterized by analytes with high molecular weights, such as furfural and esters, while the latter group shows more intense peaks for ethyl benzoate. Moreover, ethyl benzoate appears to predominantly influence samples from chestnut barrels. Due to the highly complex production process of ABTM, where each battery is influenced by several factors, this study's findings are specific to the current experimental conditions. [ABSTRACT FROM AUTHOR]

Featured Application: The findings of this study shed light on the intricate relationship between the cooking techniques, volatile compound formation, and consumer acceptance of beef meat. By employing Solid-Phase Microextraction (SPME) and gas chromatography–mass spectrometry (GC-MS) methods to analyze volatile "marker" compounds, the study delineates significant disparities in flavor profiles arising from roasting versus stewing methods. The objective of this study is to determine the effect of two distinct cooking techniques, namely roasting and stewing, on the formation of volatile compounds in various beef muscles (Semimembranosus, Biceps femoris, and Rectus femoris) and how this relates to consumer acceptance. The research employs the concept of volatile "marker" compounds to discern the influence of cooking techniques on the flavor profile of beef. Eighteen "marker compounds" were selected to represent a number of the mechanisms of formation and quantified in beef subjected to two different cooking methods. While no statistically significant differences were observed in consumer evaluations between the two cooking methods, notable disparities emerged in the consumer assessments of specific muscle cuts. Notably, the Rectus femoris muscle received the highest ratings (p < 0.05) among other evaluated muscles. The utilization of Solid-Phase Microextraction (SPME) and gas chromatography–mass spectrometry (GC-MS) methods for the analysis of volatile "marker compounds" in beef proved effective in highlighting significant differences in flavor compound classes between cooking methods, and these differed between muscles. The main effect was of the cooking method with stewed beef aroma having approximately 39× more dimethyl trisulphide, 9× more dimethyl disulphide, 7× more pentanal, 3× more hexanal, and twice as much benzaldehyde and 2-methylthiophene. Dimethyldisulphide, dimethyltrisulphide, hexanal, and heptanal, therefore, emerged as characteristic volatile compounds associated with the stewing cooking technique, suggesting their potential as markers for lipid and other oxidation reactions. This work indicates that certain lipid oxidation compounds, Strecker aldehydes, and sulfur compounds can be markers for the undesirable and/or desirable flavors of cooked beef, but that this depends on the cooking method chosen. It shows that flavor differences may be understood through the analysis of volatile flavor compounds in association with palatability and other chemical measurements. [ABSTRACT FROM AUTHOR]

Headspace solid-phase microextraction (HSSPME) of volatile organic compounds (VOCs) from aqueous samples under vacuum conditions (Vac-HSSPME) allows increasing extraction rates and decreasing detection limits compared to HSSPME under atmospheric pressure. The positive effect of the vacuum on HSSPME of an analyte can be quickly estimated using its Henry's law constant (HLC). According to the two-layer model of evaporation, substantial positive effect of the vacuum can be expected for analytes with HLC lower than 1.6·10−4 atm m3 mol−1 (0.0065 at 25 °C), but the model does not consider possible effects of other important extraction parameters. This research was aimed at the evaluation of the possible effect of vacuum on the equilibration time and extracted amounts of analytes with various HLC and fiber coating-headspace distribution constants (Kfh) using the computational model recently developed in COMSOL Multiphysics® software. It has been proven that HSSPME under vacuum provides faster equilibration of VOCs with all studied Kfh and HLC. The largest vacuum effect on the extracted analyte amount was 3.9–4.0 times at logKfh = 6 and HLC = 10−6–10−3. The substantial (≥1.5 times) vacuum impact should not be expected for analytes with logKfh < 5 for 15-min extraction and logKfh < 5.5 for 30-min extraction. The vacuum impact should be more pronounced when using fiber coatings with a stronger affinity to analytes. The obtained results will be useful for the development of new methods based on Vac-HSSPME and evaluation whether HSSPME is reasonable to conduct under vacuum conditions for faster equilibration and/or lower detection limits.

In this study, a novel methodology has been developed for the rapid and sensitive analysis of bongkrekic acid (BA), a highly toxic bacterial metabolite, using a molecularly imprinted polymer-coated wooden-tip coupled with electrospray ionization mass spectrometry (MIPWT-ESI-MS). A MIPWT solid phase microextraction (SPME) probe specifically tailored for BA was fabricated, by employing dummy template molecules/functional monomers in the imprinting coating modification. This approach exhibits an enrichment factor (EF) of 683 ± 53 for efficient extraction of BA from aqueous matrices, demonstrating the utility of dummy templates in enhancing the selectivity and sensitivity of the MIPWT-ESI-MS method. The analytical performance of the MIPWT-ESI-MS method was evaluated, demonstrating a desirable linear correlation (r = 0.9988), along with remarkable sensitivity by a limit of detection (LOD) and limit of quantitation (LOQ) at 0.05 μg/L and 0.16 μg/L in pure water, respectively. Additionally, the method demonstrated high repeatability with a relative standard deviation (RSD) < 3.9 % (n = 6) and reproducibility with an RSD < 13.4 %. The practical application of the method was confirmed through the successful analysis of real-world samples, including tap water, wastewater from a food processing factory, and the aqueous extracts of food samples, with BA detected at 0.296 µg/L in Tremella. Spiking experiments further validated the accuracy of the method, with recoveries ranging from 81 % to 97 %. This study integrates MIP with ambient mass spectrometry, offering a robust, selective, and sensitive tool for the monitoring of trace BA levels in complex food and environmental samples, contributing significantly to public health safety and food quality control.

Assessing the greenness of sample preparation techniques is essential due to the use of various solvents, chemicals, reagents, sorbents, pH adjustments, and energetic inputs. Solid-Phase Microextraction (SPME) is preferred over traditional flavor extraction methods such as Simultaneous Distillation Extraction (SDE) and Solvent-Assisted Flavor Evaporation (SAFE) because of its sensitivity, efficiency, speed, versatility, and economy. SPME fibers coated with stationary phases can extract volatile and semi-volatile flavor compounds from food samples, which are then desorbed and analyzed by Gas Chromatography-Mass Spectrometry (GC–MS). This article provides an assessment of the greenness of 50 SPME techniques for flavor analysis using the AGREE Prep and Sample Preparation Metric of Sustainability (SPMS) tools. This evaluation offers valuable insights into the environmental impact and sustainability of SPME as sample preparation techniques for flavour analysis. As per AGREE Prep, method 34 was found to be environmental friendly with score of 0.66, attributed to safe solvents, minimized waste, high sample throughput, and low energy consumption where as method 7 with SPMS scores of 7.05 is more sustainable due to miniaturization, fewer steps, and low energy use.

Solid-phase microextraction (SPME) coupled with electrospray ionization mass spectrometry (ESI-MS) was developed for rapid and sensitive determination of endogenous androgens. The SPME probe is coated with covalent organic frameworks (COFs) synthesized by reacting 1,3,5-tri(4-aminophenyl)benzene (TPB) with 2,5-dioctyloxybenzaldehyde (C8PDA). This COFs-SPME probe offers several advantages, including enhanced extraction efficiency and stability. The analytical method exhibited wide linearity (0.1–100.0 µg L−1), low limits of detection (0.03–0.07 µg L−1), high enrichment factors (37–154), and satisfactory relative standard deviations (RSDs) for both within one probe (4.0–14.8%) and between different probes (3.4–12.7%). These remarkable performance characteristics highlight the reliability and precision of the COFs-SPME-ESI-MS method. The developed method was successfully applied to detect five kinds of endogenous androgens in female serum samples, indicating that the developed analytical method has great potential for application in preliminary clinical diagnosis. [ABSTRACT FROM AUTHOR]

Transplant centers are currently facing a lack of tools to ensure adequate evaluation of the quality of the available organs, as well as a significant shortage of kidney donors. Therefore, efforts are being made to facilitate the effective use of available organs and expand the donor pool, particularly with expanded criteria donors. Fulfilling a need, we aim to present an innovative analytical method based on solid-phase microextraction (SPME) - chemical biopsy. In order to track changes affecting the organ throughout the entire transplant procedure, porcine kidneys were subjected to multiple samplings at various time points. The application of small-diameter SPME probes assured the minimal invasiveness of the procedure. Porcine model kidney autotransplantation was executed for the purpose of simulating two types of donor scenarios: donors with a beating heart (HBD) and donors after cardiac death (DCD). All renal grafts were exposed to continuous normothermic ex vivo perfusion. Following metabolomic and lipidomic profiling using high-performance liquid chromatography coupled to a mass spectrometer, we observed differences in the profiles of HBD and DCD kidneys. The alterations were predominantly related to energy and glucose metabolism, and differences in the levels of essential amino acids, purine nucleosides, lysophosphocholines, phosphoethanolamines, and triacylglycerols were noticed. Our results indicate the potential of implementing chemical biopsy in the evaluation of graft quality and monitoring of renal function during perfusion. [ABSTRACT FROM AUTHOR]

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. [ABSTRACT FROM AUTHOR]

A solid-phase microextraction (SPME) method had been applied to speciate chromium in natural and wastewater samples. MWCNTs@CuAl2O4@SiO2 nanocomposite was synthesized by sol–gel and calcination methods and then characterized using SEM, FTIR, and XRD techniques. MWCNTs@CuAl2O4@SiO2 was used to extract Cr(VI) as pyrrolidine dithiocarbamate chelates. Some analytical parameters involving pH, ligand (APDC) and adsorbent amounts, sample initial and final volume, and the effects of matrices were tested and optimized. For the oxidation of Cr(III) to Cr(VI), potassium permanganate was used, and after that, the presented method was applied to determine the total chromium levels. The calculations were carried out to obtain Cr(III) concentration by finding differences between total chromium and Cr(VI) concentrations. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 6.2 µg L−1 and 20.8 µg L−1, respectively. The proposed method was successfully applied for chromium speciation in wastewater samples. [ABSTRACT FROM AUTHOR]

Nowadays, molecularly imprinted polymers (MIPs) are well established and are considered excellent materials for performing selective extractions. However, with the progressive implementation of the principles of green chemistry, it is necessary to find greener alternatives for both the synthesis and further use of MIPs in sample preparation. Accordingly, in the present work, different deep eutectic solvents (DES, both hydrophilic and hydrophobic), as an alternative to conventional organic solvents (i.e., toluene), were evaluated as porogens for the synthesis of imprinted fibers (monoliths), using fused silica capillaries as molds, for solid-phase microextraction (SPME). From this study, the polymer prepared with propazine (dummy template), methacrylic acid (monomer), ethylene glycol dimethacrylate (cross-linker), and a formic acid:L-menthol (1:1) DES (porogen) showed the best performance for selective rebinding of triazines. After optimization of the different variables involved in SPME, the new imprinted fibers were successfully applied to the extraction of target analytes (desisopropylatrazine, desethylatrazine, simazine, and atrazine) from soil sample extracts, providing relative recoveries ranging from 75.7 to 120.1%, reaching limits of detection within the range of 6.2–15.7 ng g−1, depending upon the analyte. [ABSTRACT FROM AUTHOR]

Mono‐varietal virgin olive oils were obtained from Olea europaea L. olives grown in the National Olive Germplasm Bank in the same agronomic conditions for two harvesting years. Samples were characterized according to fatty acid composition, volatile profile, and sensory attributes, and varieties were compared using Pearson correlation, principal component analysis (PCA), and cluster analysis. Odor activity values (OAVs) of the volatiles were calculated to discuss relationships between individual sensory properties and volatiles. Although most of the samples overlapped on the score plots, some samples were located away from the others. The sample groupings on the dendrogram plotted using Ward's linkage were generally suitable with PCA results. Ethanol had a negative correlation with 9 out of 14 pleasant attributes. According to OAVs, trans‐2‐hexenal content had the most important effect on sensory attributes and positively correlated with flower odor, whereas hexenal content contributed to sweet attributes. Similarly, the effect of 1‐hexanol content strengthened the flower attribute but weakened the bitter taste. These findings were also confirmed by separating some varieties rich in those volatiles on the PCA bi‐plot of sensory attributes. Samples were grouped on a dendrogram in accordance with total ester and total C3, C5, and C6 acid contents. Practical Application: Most olive production in Turkey is based on a few varieties, whereas 95 different endemic varieties were registered by Turkish National Germplasm Bank. This study provides information on the volatile composition, sensory profile, and fatty acid composition of virgin olive oils produced from some rare varieties with high oil content. Moreover, relationships and correlations between individual volatiles and sensory attributes were evaluated, and the main differences in fatty acid composition, volatile profile, and sensory attributes of these Turkish virgin olive oils and those produced from well‐known varieties from major producing countries were compared. Thus, data on the main characteristics of extra virgin olive oils produced from Turkish olives were provided to the literature, these varieties were promoted internationally, and their cultivation was encouraged. [ABSTRACT FROM AUTHOR]

In this work, four metal-organic frameworks (MOFs) including DUT-4, DUT-8, IRMOF-8, and MIL-140B were synthesized using 2,6-naphthalene dicarboxylic acid as organic ligand and Al3+, Co2+, Zn2+, and Zr4+as metal centers, then coated on stainless steel wires as solid-phase microextraction (SPME) fiber coatings. Five aldehyde biomarkers (hexanal, heptanal, octanal, decanal, and nonanal) in exhaled breath of lung cancer patients were used as the target analytes, and extracted using four MOFs fiber coatings, followed by thermal desorption and quantitative analysis using GC–MS. The DUT-4 was found to be the most appropriate sorbent. The developed SPME-GC–MS method has large enrichment factors (877–1711), wide linear ranges (0.5–1000 μg L−1), and low detection limits (0.056–0.138 μg L−1). The relative standard deviation for six replicate cycles using one DUT-4 coated fiber were 2.0–7.7 % (intra-day) and 2.2–4.6 % (inter-day), respectively. The fiber-to-fiber reproducibility for three parallel prepared fibers was in the range of 3.7–13.7 % (RSD). The fabricated DUT-4 coated fiber can withstand at least 100 cycles of extraction/desorption/conditioning without significant loss of extraction efficiency and precision. The high enrichment factors of the DUT-4 coatings are attributed to the high specific surface area, unique porous structure, and abundant aluminum coordinated unsaturated metal sites of the DUT-4 material. Moreover, the 2,6-naphthalene dicarboxylic acid has two benzene rings with a 180° orientation, which not only increases the hydrophobicity of the MOFs material to avoid water molecules occupying adsorption sites and helps to form a rigid skeleton structure with a large number of functional adsorption sites on the surface, thereby improving the enrichment factor of target analytes. Ultimately, the developed DUT-4 coated SPME fibers was sucessfully used for the analysis of exhaled breath samples, and the recoveries for the spiked analytes were in the range of 89–105 %.

This paper proposes an all-in-one microextraction-based protocol capable of determining and quantifying fentanyl, methadone, and zolpidem in plasma, urine, and saliva at concentrations below those required by international regulatory organizations. A homemade thin-film microextraction device featuring an octyl–cyanopropyl stationary phase was coupled with LC-MS/MS. The proposed method was developed and validated according to FDA criteria, providing extraction efficiency values ranging from 26.7% to 76.2% with no significant matrix effects (2.6% to 15.5% signal suppression). The developed protocol provided low limits of quantification (mostly equal to 1 ng mL−1) and good reproducibility (intra- and inter-day RSDs of less than 9.6% and 12.0%, respectively) and accuracy (89% to 104% of the test concentration). An assessment of the protocol's environmental impact indicated that attention must be devoted to eliminating the use of toxic reagents and developing its capability for in situ sampling and in-field analysis using portable instruments. The proposed TFME-based protocol provides clinical laboratories with a versatile, one-step tool that enables the simultaneous monitoring of fentanyl, methadone, and zolpidem using the most popular biological matrices. [ABSTRACT FROM AUTHOR]

The qualitative and semi-quantitative composition of aroma compounds in plum-, pear-, and quince-based spirits from Serbia was determined and mutually compared by liquid-liquid extraction and solid-phase microextraction (HS-SPME) coupled with GC/MS analysis. Based on economic considerations, HS-SPME was suggested as the preferred method for the aroma analysis. The main volatile compounds in all three liquid-liquid extracts belonged to the group of alcohols (3-methyl-1-butanol and 2-methyl-1-butanol, as representatives) and esters (ethyl lactate, as the most abundant). 3-Methyl-1-butanol, 2-methyl-1-butanol, and ethyl lactate dominated in plum spirit; 3-methyl-1-butanol, 2-methyl-1-butanol, isobutanol, ethyl lactate, and ethyl-(E,Z)-2,4-decadienoate—in pear spirit; and 3-methyl-1-butanol, isobutanol, ethyl lactate, and (E,E)-α-farnesene—in quince spirit. The main volatile compounds in all three HS-SPME extracts belonged to alcohols, esters, and terpenes. 3-Methyl-1-butanol, ethyl decanoate, and ethyl octanoate dominated in plum spirit; (E,E)-α-farnesene, 3-methyl-1-butanol, ethyl decanoate, and ethyl-(E,Z)-2,4-decadienoate—in pear spirit; and (E,E)-α-farnesene, 3-methyl-1-butanol, ethyl decanoate, and ethyl octanoate—in quince spirit. [ABSTRACT FROM AUTHOR]

Metal–organic framework-derived carbon materials have shown extensive application in the sensitive extraction of polycyclic aromatic hydrocarbons (PAHs), but more active sites for its adsorption were still a tireless pursuit. In this study, ZIF-nanoleaf-derived carbon (NLCs) was synthesized and developed as a solid-phase microextraction (SPME) fiber (NLCs-F). The extraction performance was compared with ZIF-dodecahedron-derived carbon (DHCs) coated fiber (DHCs-F), which was prepared by only changing the ratio of the reactants. The unique morphology of NLCs provided abundant adsorption active sites for the selected PAHs, while the large average aperture facilitated selective extraction of high molecular weight analytes. Additionally, the high carbon content enhanced the strong enrichment capability for hydrophobic PAHs. Hence, the prepared NLCs-F coupled with GC–MS showed a good correlation coefficient (0.9975) in a wide linear range, low limits of detection (0.3–1.8 ng L−1), satisfactory repeatability, and reproducibility, which made it apply in the enrichment of PAHs in actual tea and coffee samples. [ABSTRACT FROM AUTHOR]

Premise: Chemical composition of floral volatiles can be an important complement to morphological characters in describing and identifying species. Four of the five species of western sessile‐flowered Trillium are challenging to distinguish morphologically due to wide intraspecific variation and overlapping characters among taxa. Characterizing their floral volatile compositions could aid future taxonomic, ecological, and evolutionary studies of Trillium and related taxa. We addressed two major questions: How do western sessile Trillium taxa vary in floral chemistry? Can floral scent be used to distinguish species? Methods: We collected petals from 600 individuals at 42 wild populations of four sessile Trillium species across California, Oregon, and Washington. Volatile organic compounds from the petals were extracted using solid‐phase microextraction, and the volatiles were identified and quantified by gas chromatography–mass spectrometry. The utility of floral scent composition in distinguishing species was tested using nonmetric multidimensional scaling and random forest analysis. Results: Floral volatiles of the white‐petaled T. albidum were dominated by oxygenated monoterpenes and showed considerable geographic variation that paralleled morphological variation. The maroon‐petaled T. angustipetalum and T. kurabayashii produced floral scents characterized by aliphatic esters, but each had a distinct chemical composition. Petal color of Trillium chloropetalum is highly variable, as were its scent compositions, which were blends of volatiles from both white‐petaled and maroon‐petaled congeneric taxa. Conclusions: Differences in floral scent compositions are consistent with current taxonomy of the western sessile Trillium group. In cases where species delimitations are difficult based on morphology, floral scent composition provides taxonomic insight and suggests a potential hybrid origin for T. chloropetalum. [ABSTRACT FROM AUTHOR]

Several methods have been used to determine the volatile organic compounds emitted by Ophrys orchids. The use of different methods results in incomparable data. Solid-phase microextraction (SPME) has not been used extensively on Ophrys orchids. The main components found in the SPME analysis of the scent in Ophrys orchids were as follows: O. apifera: benzyl benzoate and α-copaene; O. crabronifera subsp. biscutella: pentadecane, heptadecane, and nonadecane; O. bertolonii subsp. bertolonii: pentadecane and heptadecane; O. passionis subsp. garganica: i-propyl palmitate and heptadecane; O. holosericea subsp. apulica: α-copaene, pentadecane, and heptadecane; O. lacaitae: α-copaene, pentadecane, and heptadecane; O. bombyliflora: cyclosativene, pentadecane, and ethyl dodecanoate; O. insectifera: 8-heptadecene and pentadecane; O. lutea: heptadecane and docosane; O. tenthredinifera subsp. neglecta: α-copaene, caryophyllene, and i-propyl palmitate. [ABSTRACT FROM AUTHOR]

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Conjugated microporous polymers (CMPs) have been widely used in various fields as a new class of porous materials. In this study, a quinoxaline-based CMP (BQP-CMP) was prepared and used as the coating in SPME for the extraction and enrichment of nine phthalate esters (PAEs) in juice, soya sauce, cooking wine, and blended edible oil samples. Several parameters affecting solid-phase microextraction (SPME) were optimized. The feasibility of the developed method was verified using real samples, which showed low LODs (0.014–0.032 µg L−1), wide linearities (0.05–50 µg L−1), good repeatability (2.8–6.6%), and a long service life. The real liquid samples were successfully analyzed using this proposed method and spiked recoveries of 70.16–96.36% were obtained. Moreover, the interaction model and binding energies between BQP-CMP and the PAEs were explored using molecular docking. Satisfactory extraction efficiency was achieved owing to the high specific surface area (601.62 m2 g−1), high hydrophobicity, and the conjugated planar structural unit distribution of BQP-CMP. This study demonstrates that BQP-CMP is excellent as a rapid and sensitive analysis material for PAEs at trace levels in various types of samples and that CMP materials are also excellent candidates for SPME coatings. [ABSTRACT FROM AUTHOR]

IntroductionNormothermic ex vivo kidney perfusion (NEVKP) is designed to replicate physiological conditions to improve graft outcomes. A comparison of the impact of hypothermic and normothermic preservation techniques on graft quality was performed by lipidomic profiling using solid-phase microextraction (SPME) chemical biopsy as a minimally invasive sampling approach.MethodsDirect kidney sampling was conducted using SPME probes coated with a mixed-mode extraction phase in a porcine autotransplantation model of the renal donor after cardiac death, comparing three preservation methods: static cold storage (SCS), NEVKP, and hypothermic machine perfusion (HMP). The lipidomic analysis was done using ultra-high-performance liquid chromatography coupled with a Q-Exactive Focus Orbitrap mass spectrometer.ResultsChemometric analysis showed that the NEVLP group was separated from SCS and HMP groups. Further in-depth analyses indicated significantly (p < 0.05, VIP > 1) higher levels of acylcarnitines, phosphocholines, ether-linked and longer-chain phosphoethanolamines, triacylglycerols and most lysophosphocholines and lysophosphoethanolamines in the hypothermic preservation group. The results showed that the preservation temperature has a more significant impact on the lipidomic profile of the kidney than the preservation method’s mechanical characteristics.ConclusionHigher levels of lipids detected in the hypothermic preservation group may be related to ischemia-reperfusion injury, mitochondrial dysfunction, pro-inflammatory effect, and oxidative stress. Obtained results suggest the NEVKP method’s beneficial effect on graft function and confirm that SPME chemical biopsy enables low-invasive and repeated sampling of the same tissue, allowing tracking alterations in the graft throughout the entire transplantation procedure.

The primary objective of this contribution is to offer insights into fundamentals associated with typical sample preparation, facilitating rational design of new analytical technologies and effective optimization of existing techniques. Sample preparation stands a pivotal stage in the analytical process. Unfortunately, the optimization of associated parameters often relies on trial and error rather than systematic scientific methodologies. If an extraction method provides good recovery of spikes of standards, it is assumed that it works well and no further consideration is given to the underlying principles driving its performance. In the realm of sample preparation, the fundamentals of method optimization are not accorded the same significance as in other technologies, such as chromatography or mass spectrometry. Consequently, the fundamentals of sample preparation are typically overlooked in analytical chemistry curricula.A notable impediment to progress in the sample preparation area is underdeveloped understanding of the fundamentals of extraction, particularly when dealing with natural, often complex samples, where native analyte-matrix interaction is different compared to spikes. This stands in contrast to the physiochemically simpler systems employed in separation and quantification steps, such as chromatography and mass spectrometry.A careful consideration of the underlying principles of sampling and sample preparation can lead to the creation of more efficient and environmentally friendly technologies. Embracing these principles aligns with global shift towards more sustainable future, challenging the perception that sample preparation is solely an artistic endeavour and highlighting its potential as a scientifically grounded discipline.

Several methods have been used to determine the volatile organic compounds emitted by Ophrys orchids. The use of different methods results in incomparable data. Solid-phase microextraction (SPME) has not been used extensively on Ophrys orchids. The main components found in the SPME analysis of the scent in Ophrys orchids were as follows: O. apifera: benzyl benzoate and α-copaene; O. crabronifera subsp. biscutella: pentadecane, heptadecane, and nonadecane; O. bertolonii subsp. bertolonii: pentadecane and heptadecane; O. passionis subsp. garganica: i-propyl palmitate and heptadecane; O. holosericea subsp. apulica: α-copaene, pentadecane, and heptadecane; O. lacaitae: α-copaene, pentadecane, and heptadecane; O. bombyliflora: cyclosativene, pentadecane, and ethyl dodecanoate; O. insectifera: 8-heptadecene and pentadecane; O. lutea: heptadecane and docosane; O. tenthredinifera subsp. neglecta: α-copaene, caryophyllene, and i-propyl palmitate.

In vivo lung perfusion (IVLP) is a novel isolated lung technique developed to enable the local, in situ administration of high-dose chemotherapy to treat metastatic lung cancer. Combination therapy using folinic acid (FOL), 5-fluorouracil (F), and oxaliplatin (OX) (FOLFOX) is routinely employed to treat several types of solid tumours in various tissues. However, F is characterized by large interpatient variability with respect to plasma concentration, which necessitates close monitoring during treatments using of this compound. Since plasma drug concentrations often do not reflect tissue drug concentrations, it is essential to utilize sample-preparation methods specifically suited to monitoring drug levels in target organs. In this work, in vivo solid-phase microextraction (in vivo SPME) is proposed as an effective tool for quantitative therapeutic drug monitoring of FOLFOX in porcine lungs during pre-clinical IVLP and intravenous (IV) trials. The concomitant extraction of other endogenous and exogenous small molecules from the lung and their detection via liquid chromatography coupled to high resolution mass spectrometry (LC-HRMS) enabled an assessment of FOLFOX's impact on the metabolomic profile of the lung and revealed the metabolic pathways associated with the route of administration (IVLP vs. IV) and the therapy itself. This study also shows that the immediate instrumental analysis of metabolomic samples is ideal, as long-term storage at −80 °C results in changes in the metabolite content in the sample extracts.

The endocannabinoid system (ECS), particularly its signaling pathways and ligands, has garnered considerable interest in recent years. Along with clinical work investigating the ECS’ functions, including its role in the development of neurological and inflammatory conditions, much research has focused on developing analytical protocols enabling the precise monitoring of the levels and metabolism of the most potent ECS ligands: exogenous phytocannabinoids (PCs) and endogenous cannabinoids (endocannabinoids, ECs). Solid-phase microextraction (SPME) is an advanced, non-exhaustive sample-preparation technique that facilitates the precise and efficient isolation of trace amounts of analytes, thus making it appealing for the analysis of PCs and ECs in complex matrices of plant and animal/human origin. In this paper, we review recent forensic medicine and toxicological studies wherein SPME has been applied to monitor levels of PCs and ECs in complex matrices, determine their effects on organism physiology, and assess their role in the development of several diseases.

Solid-phase microextraction (SPME) has been widely proposed for the extraction, clean-up, and preconcentration of analytes of environmental concern. Enrichment capabilities, preconcentration efficiency, sample throughput, and selectivity in extracting target compounds greatly depend on the materials used as SPME coatings. Supramolecular materials have emerged as promising porous coatings to be used for the extraction of target compounds due to their unique selectivity, three-dimensional framework, flexible design, and possibility to promote the interaction between the analytes and the coating by means of multiple oriented functional groups. The present review will cover the state of the art of the last 5 years related to SPME coatings based on metal organic frameworks (MOFs), covalent organic frameworks (COFs), and supramolecular macrocycles used for environmental applications.

The study examines the unique production process of Aceto Balsamico Tradizionale di Modena PDO (ABTM), emphasizing its complex phases and the impact of raw materials and artisanal skill on its flavor characteristics. Analytical tests focused on the volatile composition of vinegars from different wood barrels at different aging stages, using solid-phase micro-extraction (SPME) coupled with gas chromatography, either with mass spectrometry (GC/MS) or flame ionization detector (FID). Multivariate analysis, including principal component analysis (PCA), was employed to investigate the presence of peculiarities among the volatile profiles of samples of different barrel origin. The research focuses on characterizing the volatile composition of vinegars sourced from individual wood barrels, such as Cherry, Chestnut, Mulberry, Juniper, and Oak. Although it was not possible to identify molecules directly connected to the woody essence, some similarities emerged between vinegar samples from mulberry and cherry barrels and between those of juniper and oak. The former group is characterized by analytes with high molecular weights, such as furfural and esters, while the latter group shows more intense peaks for ethyl benzoate. Moreover, ethyl benzoate appears to predominantly influence samples from chestnut barrels. Due to the highly complex production process of ABTM, where each battery is influenced by several factors, this study’s findings are specific to the current experimental conditions.

The effect of ultrasonic pre-treatment on moisture removal characteristics of ginger in a convective dryer was investigated. The slabs were dried by practicing sonication durations of 0, 15 and 30 min at different levels of the air temperature and velocity. Following increasing the sonication duration and air temperature, required time and energy to dehydrate the samples were decreased. The pre-treatment played important role in improving rehydration capability and surface color retention in the dried gingers. Content of the main volatile component (α-Zingiberene) was not influenced by the sonication. Mean values for the phenolic contents and antioxidant activity at sonication duration of 0, 15 and 30 min were determined to be 18.93, 18.15 and 17.49 GAE/g dry matter and 83.57, 78.33 and 74.58 %, respectively. The desired values for the temperature, velocity and sonication duration were revealed to be about 66 °C, 3 m/s and 20 min, respectively.

Phosphatidylcholine (PC) and lysophosphatidylcholine (LPC), two types of phospholipids (PLs), have been reported to be closely correlated with head and neck cancers of laryngeal cancer (LC) and thyroid cancer (TC), which make their analysis crucial. TiO2@COF-based solid-phase microextraction (SPME) coupled to UHPLC-MS/MS was developed for the rapid and accurate detection of seven potential PL biomarkers from small amounts of serum in this work. The combination of TiO2 and COF proves to be effective for the extraction of the target analytes. Under optimal conditions, the developed TiO2@COF-based SPME-UHPLC-MS/MS method revealed good linearity (R2 ≥ 0.997) with LODs ranging from 0.05 to 0.38 ng/mL for PLs, the extraction recoveries and matrix effects ranging from 83.09–112.03% and 85.38–113.67%, respectively. As a high-throughput pretreatment method, satisfactory probe-to-probe reproducibility rates of 2.7–10.1% were obtained. Finally, the TiO2@COF-based SPME-UHPLC-MS/MS method was applied to analyze LPC 14:0, LPC 16:0, LPC 18:0, LPC 18:1, LPC 19:0, PC 16:0/18:1, and PC 18:0 in serum samples from early LC patients (n = 15), early TC patients (n = 15), and healthy volunteers (n = 15). The results indicated that cancer patients could be effectively differentiated from healthy controls using orthogonal partial least squares discriminant analysis (OPLS-DA). In conclusion, the established TiO2@COF-based SPME-UHPLC-MS/MS method is reliable for the rapid determination of the seven PLs in serum samples, which is promising for early diagnosis of head and neck cancers. [ABSTRACT FROM AUTHOR]

Conductive polymers as composite materials have been attracted tremendous attention due to their versatile and excellent features such as tunable conductivity, facile synthesis and fabrication, high chemical and thermal stability etc. These characteristics make them versatile and let them being used in numerous fields including microelectronics, optics and biosensors. Throughout the mentioned fields, conductive polymers particularly perform as effective sorbents. Although tremendous efforts have been put into this topic, to the best of our knowledge, a comprehensive up-to-date review on the applications of conductive polymers as efficient sorbents has not been reported. The main objective of this paper is to make a significant contribution to the recent literature toward the synthesis and extraction applications of conductive polymers as efficient sorbents. [ABSTRACT FROM AUTHOR]

Objectives] To understand the quality safety of vegetables produced in vegetable planting bases around Lhasa City. [Methods] Four vegetable planting bases in the east, west, south, and north of Lhasa City were randomly selected for testing using rapid measuring instru- ment for agricultural residues and solid-phase microextraction-gas chromatography-mass spectrometer, with 120 vegetable samples selected. The testing samples included seven categories: green leafy vegetables, eggplants, melons, onions and garlic, root vegetables, beans, and fungi, totaling 29 types of vegetables. The samples were tested for 8 common prohibited and restricted pesticides in organic phosphorus and carbamate esters, including methamidophos, parathion, methyl parathion, monocrotophos, isocarbophos, methamidophos, aldicarb, and carbofuran. [Results] The pesticide inhibition rate of 6 kinds of vegetables detected by the rapid measuring instrument for agricultural residues was relatively high, with green leafy vegetables being the majority, reaching over 25%. By further establishing a solid-phase microextraction-gas chromatography-tandem mass spectrometry method, the accuracy of the data was verified experimentally. The experimental results indicated that the inhibition rate of vegetable samples in this experiment did not exceed 15%, and it was determined as a pollution-free vegetable. [Conclusions] According to the restriction standard of national pesticide use, the inhibition rate of vegetable samples was less than or equal to 40%, indicating that the quality of vegetables was qualified. [ABSTRACT FROM AUTHOR]

The aim of this study was to characterize aroma compounds from Moso bamboo (Phyllostachys edulis Mazel ex Houz. De ehaie) stem powders with a headspace solid phase microextraction – gas chromatography/mass spectrometry method and reconstruct the fresh stem aroma. A total of 32 aroma compounds were identified from the powders, comprising monoterpene hydrocarbons (40.03%), hydrocarbons (26.27%), aliphatic aldehydes (13.82%), norisoprenoids (7.93%), sesquiterpene hydrocarbons (3.40%), aliphatic ketones (2.47%), an aromatic alcohol (1.34%) and an acid (1.30%). The most abundant aroma compound was limonene (32.95%) and the absolute configuration and optical purities were determined as (R)-form with 98.17 ± 0.27% enantiomeric excess. The odor active values (OAVs) showed thirteen aroma active compounds (OAVs > 1.00) were determined, including seven aliphatic aldehydes, three monoterpene hydrocarbons, two norisoprenoids and one aliphatic ketone. We have compared the aroma profiles between the Moso bamboo stem powders and a reconstructed one on the basis of quantitative data and characterized the active compounds that can be responsible for the fresh stem aroma by sensory evaluation. [ABSTRACT FROM AUTHOR]

Acetophenone is a reagent used in various consumer products, including fragrance chemicals in toys and childcare products. Contact with acetophenone-containing materials can harm human health, and therefore acetophenone migration levels should be controlled. A new procedure for the quantification of acetophenone migrated to air and water from toys and school supplies using solid-phase microextraction and gas chromatography with mass spectrometric detection is proposed. The optimal combination of acetophenone response and its relative standard deviations was achieved for air samples after 10-min extraction at 25°C and for water samples after the addition of 3.5 g of salt, agitation/preincubation at 500 rpm for 5 min at 60°C, and 20-min extraction by polydimethylsiloxane/divinylbenzene fiber. The developed procedure provided linear calibration with R2 > 0.996 at 1–50 µg/m3 in air and 1–20 µg/L in water, and low limits of detection and quantification of acetophenone in the air (0.01, 0.04 µg/m3) and water (0.01, 0.03 µg/L). Spike recoveries of acetophenone were 109–116% for air and 90–111% for water. Acetophenone concentrations migrated from toys and school supplies into the air ranged from 0.6 to 1.5 µg/m3, except for eraser type II (9.7 µg/m3) which exceeded the maximum permissible concentration by 3.2 times. Acetophenone concentrations migrated to water were 1.3–3.5 µg/L. [ABSTRACT FROM AUTHOR]

Lipid peroxidation, the most aggressive reaction in food, results in the formation of reactive organic compounds that detrimentally impact food sensory qualities and consumers' health. While controlled lipid peroxidation can enhance flavors and appearance in certain foods, secondary peroxidation products lead to sensory deterioration in a variety of products, such as oils, alcoholic beverages, and meat. This publication reviews the use of modern analytical techniques for detecting and quantifying carbonyl compounds, i.e., secondary lipid peroxidation products. The paper focuses specifically on microextraction-based methods: dispersive liquid-liquid microextraction (DLLME), solid-phase microextraction (SPME), and gas-diffusion microextraction (GDME). These techniques offer efficient and sensitive approaches to extracting and quantifying lipid oxidation products and contribute to the understanding of oxidative deterioration in various food products. The review outlines recent advancements, challenges, and limitations in these microextraction techniques, as well as emphasizes the potential for further innovation and improvement in the field of food analysis. [ABSTRACT FROM AUTHOR]

In order to improve the extraction ability of carbon fibers (CFs) for microextraction of polycyclic aromatic hydrocarbons (PAHs), biochar nanospheres derived from glucose were in-situ grown onto the surface of CFs via hydrothermal synthesis. The surface morphology and elemental composition of biochar nanospheres-CFs were investigated by scanning electron microscopy and X-ray photoelectron spectroscopy. Thereafter, the biochar nanosphere-CFs were pulled into the polyetheretherketone tube for solid-phase microextraction, and the tube was combined with high-performance liquid chromatography-diode array detector to online detect PAHs. With the help of π-stacking, hydrophobic, and hydrophilic effect of biochar nanospheres, the extraction efficiency of CFs was greatly enhanced (enrichment factor increased by 293% compared with the original). The conditions affecting the analytical performance (sampling volume, sampling rate, methanol content, and desorption time) were investigated. Under the optimal conditions, an online analytical method for microextraction and determination of several PAHs was developed, and satisfactory results were achieved. The limits of detection were 0.003-0.010 ng mL-1 owing to high enrichment effect (2973-3600), linearity ranged from 0.010-15.0 ng mL-1, and relative standard deviations were 0.4%-1.6% (intra-day) and 2.4%-4.4% (inter-day), respectively. The method was applied to analyze environmental water samples (rain water, snow water, and river water), and spiked recoveries within 80.0%-119% were obtained. [ABSTRACT FROM AUTHOR]

The endocannabinoid system (ECS), particularly its signaling pathways and ligands, has garnered considerable interest in recent years. Along with clinical work investigating the ECS' functions, including its role in the development of neurological and inflammatory conditions, much research has focused on developing analytical protocols enabling the precise monitoring of the levels and metabolism of the most potent ECS ligands: exogenous phytocannabinoids (PCs) and endogenous cannabinoids (endocannabinoids, ECs). Solid-phase microextraction (SPME) is an advanced, non-exhaustive sample-preparation technique that facilitates the precise and efficient isolation of trace amounts of analytes, thus making it appealing for the analysis of PCs and ECs in complex matrices of plant and animal/human origin. In this paper, we review recent forensic medicine and toxicological studies wherein SPME has been applied to monitor levels of PCs and ECs in complex matrices, determine their effects on organism physiology, and assess their role in the development of several diseases. [Display omitted] • Various solid-phase microextraction protocols for isolation of phytocannabinoids in plant material and animal/human matrices. • Applications of solid-phase microextraction for the analysis of trace levels of endocannabinoids animal and human tissues. • Advantages and limitations of solid-phase microextraction in the analysis of phyto- and endocannabinoids in complex matrices. [ABSTRACT FROM AUTHOR]

In vivo lung perfusion (IVLP) is a novel isolated lung technique developed to enable the local, in situ administration of high-dose chemotherapy to treat metastatic lung cancer. Combination therapy using folinic acid (FOL), 5-fluorouracil (F), and oxaliplatin (OX) (FOLFOX) is routinely employed to treat several types of solid tumours in various tissues. However, F is characterized by large interpatient variability with respect to plasma concentration, which necessitates close monitoring during treatments using of this compound. Since plasma drug concentrations often do not reflect tissue drug concentrations, it is essential to utilize sample-preparation methods specifically suited to monitoring drug levels in target organs. In this work, in vivo solid-phase microextraction (in vivo SPME) is proposed as an effective tool for quantitative therapeutic drug monitoring of FOLFOX in porcine lungs during pre-clinical IVLP and intravenous (IV) trials. The concomitant extraction of other endogenous and exogenous small molecules from the lung and their detection via liquid chromatography coupled to high resolution mass spectrometry (LC-HRMS) enabled an assessment of FOLFOX's impact on the metabolomic profile of the lung and revealed the metabolic pathways associated with the route of administration (IVLP vs. IV) and the therapy itself. This study also shows that the immediate instrumental analysis of metabolomic samples is ideal, as long-term storage at −80 °C results in changes in the metabolite content in the sample extracts. [Display omitted] • Use of in vivo SPME during FOLFOX administration in pre-clinical IVLP and IV trials. • Therapeutic drug monitoring of FOLFOX and metabolites in porcine lung. • Pharmacometabolomic fingerprinting of porcine lung during FOLFOX administration. • In vivo SPME facilitates in situ monitoring of lung function with no tissue biopsy. [ABSTRACT FROM AUTHOR]

Since the outbreak of COVID‐19, many antiviral drugs have been used to treat infected patients. Excessive drug concentrations may not only damage patients' organs, but also lead to increased mortality. The lack of data makes it difficult for them to be treated with these drugs under proper and safe dosage. However, due to the complexity of fluid matrixand structures of the antiviral drugs, it is still difficult to detect the drugs in biofluids. Herein, solid‐phase microextraction (SPME) is applied for the detection of biological matrix, which has the advantages of simplicity, efficiency and environmental protection. With abundant hydrogen bond sites and appropriate molecular volume, biocompatible graded‐pore HOF10x series materials are selected as the fiber coating for exploration. Consequently, HOF101 could achieve high enrichment effect of drugs due to the commensurate mesopores and hydrogen bond non‐covalent interaction. Moreover, the excellent extraction capacity of the HOF101 fiber is verified to be consistent in various interfering conditions. The obtained limits of detections (LODs) are 0.24–0.66 ng L−1, and the recoveries of the biofluids in three concentration levels ranged from 80.30% to 120.1%. It shows the low LODs and satisfactory recoveries of this analytical method, which is expected to be applied in medical systems for drug monitoring. [ABSTRACT FROM AUTHOR]

Currently, the leaves of the hop plant (Humulus lupulus L.) are an unexploited and still little-investigated agricultural by-product. In our study, with the aim of exploring the metabolome of dried hop leaves (Chinook cultivar), a metabolomic approach was applied using multiple analytical tools such as SPME/GC–MS, GC–MS, PTR-ToF-MS, and NMR to identify the secondary metabolites. The obtained results showed the presence of a high number of components belonging to different chemical classes. In fact, thanks to the multi-methodological approach, volatile organic compounds (VOCs) with low molecular weight, terpenic compounds, fatty acids, sugars, amino acids, organic acids, and alcohols have been detected and identified. Among the revealed terpenes in the untreated matrix, the sesquiterpenes α-humulene, β-caryophyllene, and α-copaene were the most abundant. Among the saturated and unsaturated fatty acids, palmitic and linolenic acids, respectively, were those with the highest relative percentages. Particularly relevant was the sugar content, where sucrose was the main exponent while glutamate and asparagine were the principal detected amino acids. Conversely, alcohols and organic acids were the least abundant compound classes, and xanthohumol was also identified in the methanolic extract. [ABSTRACT FROM AUTHOR]

Copyright of Journal of Food Safety & Quality is the property of Journal of Food Safety & Quality Editorial Department and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)