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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 set of mixed metal oxide catalysts, MO x -Co 3 O 4 (M: Fe, Mn, Cu, Ni, Cr, and Zn) enveloped in polymer nanofilms was fabricated using the solid-phase synthesis method. These catalysts were subsequently studied for their catalytic performance in the low-temperature oxidation of carbon monoxide. Characterization of the catalysts was accomplished using various techniques, including X-ray diffraction (XRD), N 2 adsorption-desorption, temperature-programmed reduction (H 2 -TPR), temperature-programmed desorption of oxygen (O 2 -TPD), Fourier transform infrared spectroscopy (FTIR), thermogravimetric and differential thermal analyses (TGA and DTA) and scanning electron microscopy (FESEM). The outcomes of these investigations indicated that the composite oxides possess different characteristic features. The catalytic activity of these catalysts exhibited a decreasing trend as follows: Fe-Co > Mn-Co > Cu-Co > Ni-Co > Zn-Co > Cr-Co. Among the catalysts prepared, Fe-Co nanoparticles revealed the greatest specific surface area (138 m 2 .g − 1 ) and the largest pore volume (0.45 cm 3 .g − 1 ), resulting in the most superior catalytic activity, achieving total CO conversion at 72 °C. Additionally, the Fe-Co catalyst demonstrated exceptional long-term stability at low temperature (60 °C). Furthermore, the study investigated the impact of various parameters such as calcination temperature, CO content, gas hourly space velocity (GHSV), and pretreatment conditions.

Solid-phase microextraction (SPME) possesses unique features that allow it to be used in analyses that would not be possible with traditional sample-preparation methods. The simplicity of SPME protocols and extraction devices makes it a uniform platform for analyzing biological samples, either via the headspace or in direct immersion mode. Furthermore, flexible probe design enables SPME to be applied to target objects of different sizes, offering analysis on a scale ranging “from single cell to living organs”. SPME microfibers are minimally invasive, which enables them to be applied for the spatial and temporal monitoring of target analytes or to assess changes in the entire metabolome or lipidome. Furthermore, SPME permits the capture of the elusive portion of the metabolome, thus complementing exhaustive methods that are biased towards highly abundant and stable species. Significantly, SPME can be interfaced with analytical instrumentation to create a rapid diagnostic tool. However, despite these advantages, SPME has some limitations that must be well-understood and addressed. This paper presents examples of up-to-date applications of SPME, challenges related to particular studies, and future perspectives regarding the application of SPME in biomedical analysis.

Aflatoxins (AFs), an important category of pollutants, are formed in many foods and adversely affect human health. Therefore, their determination is critical to ensuring human food health. An efficient dispersive solid-phase microextraction technique was developed as a simple and straightforward sample preparation technique for determination of four aflatoxins using a high-performance liquid chromatography (HPLC) fluorescence detector. A novel efficient, green sorbent for extracting AFs was synthesized based on hydrothermal and chemical strategies. The amounts of three sorbent components were optimized using a mixture design (simplex lattice design), including 14 experiments. The optimal amount of amino-bimetallic Fe/Ni-MIL-53 nanospheres, chitosan, and magnetic Fe 3 O 4 nanoparticles as sorbent components was 0.87, 0.67, and 0.47 g, respectively. Also, various factors affecting the process of AF determination were studied and optimized in two successive experimental designs, including the definitive screening design and the Box–Behnken design. Under optimal conditions, the linear ranges for measuring aflatoxin B1, aflatoxin B2, aflatoxin G1, and aflatoxin G2 were 0.05–82.6, 0.07–86.4, 0.08–85.7, and 0.07–89.5 ng mL −1 , respectively. The relative standard deviations under inter-day and intra-day conditions for measuring AFs at three analyte concentrations were determined in triplicate analysis and were in the ranges of 3.7–4.6% and 4.9–6.1% for water sample analysis, respectively. The qualitative detection limits for determining AFs were between 0.01 and 0.05 ng mL −1 . The pre-concentration factor of the method for measuring AFs ranged from 739.7 to 802.1. The proposed method was used for determining AFs in several real samples, including herbal distillate, black tea, corn, and real water samples. The relative recovery and standard deviation were 87.8–97.8% and 4.10–6.82%, respectively. Graphical abstract

The abuse and residues of antibiotics have a great impact on the environment and organisms, and their determination has become very important. Due to their low contents, varieties and complex matrices, effective recognition, separation and enrichment are usually required prior to determination. Molecularly imprinted polymers (MIPs), a kind of highly selective polymer prepared via molecular imprinting technology (MIT), are used widely in the analytical detection of antibiotics, as adsorbents of solid-phase extraction (SPE) and as recognition elements of sensors. Herein, recent advances in MIPs for antibiotic residue analysis are reviewed. Firstly, several new preparation techniques of MIPs for detecting antibiotics are briefly introduced, including surface imprinting, nanoimprinting, living/controlled radical polymerization, and multi-template imprinting, multi-functional monomer imprinting and dummy template imprinting. Secondly, several SPE modes based on MIPs are summarized, namely packed SPE, magnetic SPE, dispersive SPE, matrix solid-phase dispersive extraction, solid-phase microextraction, stir-bar sorptive extraction and pipette-tip SPE. Thirdly, the basic principles of MIP-based sensors and three sensing modes, including electrochemical sensing, optical sensing and mass sensing, are also outlined. Fourthly, the research progress on molecularly imprinted SPEs (MISPEs) and MIP-based electrochemical/optical/mass sensors for the detection of various antibiotic residues in environmental and food samples since 2018 are comprehensively reviewed, including sulfonamides, quinolones, β-lactams and so on. Finally, the preparation and application prospects of MIPs for detecting antibiotics are outlined.

All known methods for solid-phase synthesis of molecular arrays exploit positioning techniques to deposit monomers on a substrate preferably high densely. In this paper, stochastic patterning of molecule spots (250 000 spots monomers/cm 2 ) via random allocation of the microbeads on a microstructured glass is presented. The size and shape of the microbeads and the microcavities are selected in such a way so that only one microbead can fit into the respective microcavity. Each microbead can be loaded with a certain type of molecule e.g. amino acids and is brought in the microcavities stochastically. Applying solvent vapor and heating the substrate, the molecules are released from the microbeads and coupled to the functionalized substrate. To differentiate between the microbeads carrying different molecules, quantum dot labels are preliminary introduced into the microbeads. Fluorescence imaging and subsequent data analysis enable decoding of the molecule deposition patterns. After the coupling step is completed, the microbeads are mechanically removed from the microwells. The composition of the monomer microbeads, their deposition and the conditions of the monomer extraction are studied. The stochastic monomer patterning may be used to design novel molecular arrays.

Recent advances in end-to-end continuous-flow synthesis are rapidly expanding the capabilities of automated customized syntheses of small-molecule pharmacophores, resulting in considerable industrial and societal impacts; however, many hurdles persist that limit the number of sequential steps that can be achieved in such systems, including solvent and reagent incompatibility between individual steps, cumulated by-product formation, risk of clogging and mismatch of timescales between steps in a processing chain. To address these limitations, herein we report a strategy that merges solid-phase synthesis and continuous-flow operation, enabling push-button automated multistep syntheses of active pharmaceutical ingredients. We demonstrate our platform with a six-step synthesis of prexasertib in 65% isolated yield after 32 h of continuous execution. As there are no interactions between individual synthetic steps in the sequence, the established chemical recipe file was directly adopted or slightly modified for the synthesis of twenty-three prexasertib derivatives, enabling both automated early and late-stage diversification.Although strategies for the automated assembly of compounds of pharmaceutical relevance is a growing field of research, the synthesis of small-molecule pharmacophores remains a predominantly manual process. Now, an automated six-step synthesis of prexasertib is achieved by multistep solid-phase chemistry in a continuous-flow fashion using a chemical recipe file that enables automated scaffold modification through both early and late-stage diversification.

According to green analytical chemistry principles, the use of agricultural byproducts as sorbent phases is an interesting topic due to their lignocellulosic origin, as they are biodegradable and inexpensive. To the best of our knowledge, this is the first study in which avocado seed and avocado seed activated carbon are proposed as sustainable sorbents for solid-phase microextraction technologies, which were used to assess the proof of concept. Rotating disk sorptive extraction (RDSE) was used as a model technology and ibuprofen (Ibu) and 1-hydroxy-ibuprofen (1-OH-Ibu) as representative analytes. It was found that activated carbon (AC) prepared at 600 °C with an impregnation ratio (raw material/activating agent (ZnCl2), w/w) of 1:1.2 had better extraction efficiency than other ACs obtained at different temperatures, impregnation ratios, and activating agents (K2CO3). Characterization revealed several differences between natural avocado seed, biochar prepared at 600 °C, and selected AC since the typical functional groups of the natural starting material begin to disappear with pyrolysis and increasing the surface area and pore volume, suggesting that the main interactions between analytes and the sorbent material are pore filling and π-π stacking. By using this AC as the sorbent phase, the optimal extraction conditions in RDSE were as follows: the use of 50 mg of sorbent in the disk, 30 mL of sample volume, pH 4, 90 min of extraction time at a rotation velocity of the disk of 2000 rpm, and methanol as the elution solvent. The extracts were analyzed via gas chromatography coupled to mass spectrometry (GC–MS). The method provided limits of detection of 0.23 and 0.07 µg L−1 and recoveries of 81% and 91% for Ibu and 1-OH-Ibu, respectively. When comparing the extraction efficiency of the selected activated carbon with those provided by Oasis® HLB and C18 in RDSE, nonsignificant differences were observed, indicating that avocado seed activated carbon is a suitable alternative to these commercial materials.

Formaldehyde (HCHO) is a human toxin that is both a pollutant and endogenous metabolite. HCHO concentrations in human biological samples are reported in the micromolar range; however, accurate quantification is compromised by a paucity of sensitive analysis methods. To address this issue, we previously reported a novel SPME–GC–MS-based HCHO detection method using cysteamine as an HCHO scavenger. This method showed cysteamine to be a more efficient scavenger than the widely used O -(2,3,4,5,6-pentafluorobenzyl)hydroxylamine, and enabled detection of aqueous HCHO in the nanomolar range and quantification in the micromolar range. However, quantification in this range required immersive extraction of the HCHO-derived thiazolidine, while a high background signal was also observed. Following on from these studies, we now report an optimised head-space extraction SPME–GC–MS method using cysteamine, which provides similarly sensitive HCHO quantification to the immersive method but avoids extensive wash steps and is therefore more amenable to screening applications. However, high background HCHO levels were still observed A Complementary GC–MS analyses using a 2-aza-Cope-based HCHO scavenger also revealed high background HCHO levels; therefore, the combined results suggest that HCHO exists in high (i.e. micromolar) concentration in aqueous samples that precludes accurate quantification below the micromolar range. This observation has important implications for ongoing HCHO quantification studies in water, including in biological samples.

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