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Food safety and quality have been gaining increasing attention in recent years. Gas chromatography coupled to tandem mass spectrometry (GC–MS/MS), a highly sensitive technique, is gradually being preferred to GC–MS in food safety laboratories since it provides a greater degree of separation on contaminants. In the analysis of food contaminants, sample preparation steps are crucial. The extraction of multiple target analytes simultaneously has become a new trend. Thus, multi-residue analytical methods, such as QuEChERs and adsorption extraction, are fast, simple, cheap, effective, robust, and safe. The number of microorganic contaminants has been increasing worldwide in recent years and are considered contaminants of emerging concern. High separation in MS/MS might be, in certain cases, favored to sample preparation selectivity. The ideal sample extraction procedure and purification method should take into account the contaminants of interest. Moreover, these methods should cooperate with high-resolution MS, and other sensitive full scan MSs that can produce a more comprehensive detection of contaminants in foods. In this review, we discuss the most recent trends in preparation methods for highly effective detection and analysis of food contaminants, which can be considered tools in the control of food quality and safety.

Polycyclic aromatic hydrocarbons (PAHs) are hydrophobic organic contaminants that have a highly carcinogenic and mutagenic nature. This study aimed to develop and validate a sensitive analytical method to determine 8 PAHs in 51 herbal medicines (HMs) using gas chromatography (GC)-tandem mass spectrometry (MS/MS). Liquid––liquid extraction and florisil SPE cartridge purification were basically adopted for pretreatment. For the samples containing essential oil, starch grain, etc., N,N-dimethyl formamide/water mixture (9:1, v/v) was added in the extraction step. The multiple reaction monitoring (MRM) conditions were newly obtained by the infusion of reference solutions of the targeted compounds at a concentration of 100 ng/mL into the GC-MS/MS system used in this study. The 51 items were classified according to whether or not they contained essential oil. Eight PAHs were not detected in 39 (8.3%) of the 459 samples monitored. The total content of 8 PAHs ranged from 0.45 μg/kg in Anemarrhenae Rhizoma to 270.94 μg/kg in Zingiberis Rhizoma. The average content of those ranged from 0.9 μg/kg in Araliae Continentalis Radix to 110.8 μg/kg in Coptidis Rhizoma Preparata cum Vinum. The results of this study prove that the proposed method is useful for determining 8 PAHs in HMs.

To determine the amount of the explosives 1,3-dinitrobenzene, 2,4-dinitrotoluene, 2,4,6-trinitrotoluene, and its metabolites in marine samples, a toolbox of methods was developed to enhance sample preparation and analysis of various types of marine samples, such as water, sediment, and different kinds of biota. To achieve this, established methods were adapted, improved, and combined. As a result, if explosive concentrations in sediment or mussel samples are greater than 10 ng per g, direct extraction allows for time-saving sample preparation; if concentrations are below 10 ng per g, techniques such as freeze-drying, ultrasonic, and solid-phase extraction can help to detect even picogram amounts. Two different GC-MS/MS methods were developed to enable the detection of these explosives in femtogram per microliter. With a splitless injector, limits of detection (LODs) between 77 and 333 fg/µL could be achieved in only 6.25 min. With the 5 µL programmable temperature vaporization—large volume method (PTV-LVI), LODs between 8 and 47 fg/µL could be achieved in less than 7 min. The detection limits achieved by these methods are among the lowest published to date. Their reliability has been tested and confirmed by measuring large and diverse sample sets.

Mixtures of gabapentin, tramadol and/or amitriptyline are usually recommended for treatment of neuropathic pain. A novel GC–MS/MS method was developed to assess the studied mixture whether in pure forms or human biological fluids (plasma/urine). The chromatographic detection was performed using MS detector applying the selected ion-monitoring mode. An (Agilent, CA, USA) GC–MS with triple axis single quadrupole detector unit was used for the analysis equipped with HP-5MS (5% phenyl methyl siloxane) column. Helium was the carrier gas and positive electron impact ionization mode was applied. The developed method was able to assess the mixture components simultaneously within six minutes. Validation of the method was assured according to US FDA guidelines and Eco-Scale assessment.

Leontodon hispidulus Boiss is a wild annual plant growing in Egypt. The present study aims for the first time, to evaluate the phytochemical profile of the main secondary metabolites of the optimized ethanolic extract of the plant using Quadrupole Time-of-Flight Liquid chromatography-mass spectrometry and Gas chromatography-mass spectrometry. It also aims to assess the anticancer activity of its different fractions against the prostate carcinoma cell line. Moreover, an in-silico docking study was performed using the Hexokinase-two enzyme. LC- q ToF-MS analysis revealed the tentative identification of 36 phenolic compounds including the glycosides of (luteolin, quercetin, kaempferol, apigenin, isorhamnetin, and daidzein), coumarines (esculin, esculetin, and daphnetin), and phenolic acids (chlorogenic, caffeic, quinic, P -coumaric, and rosmarinic). GC–MS/MS analysis revealed the presence of 18 compounds where palmitic acid, myristic acid, alpha-amyrin, and beta-amyrin were the major ones. The cytotoxic activity results revealed that methylene chloride and ethyl acetate fractions showed the highest cytotoxic activity against the PC3 cell line, with IC 50 values of 19, and 19.6 μg/ml, respectively. Interestingly, the docking study demonstrated that apigenin-7- O -glucoside, luteolin-7- O -glucoside, kaempferol-3- O -glucuronide, quercetin-4′- O -glucoside, esculin, rosmarinic acid, chlorogenic acid, and α-amyrin exhibited high affinity to the selected target, HEK-2 enzyme.

A highly sensitive and accurate multiplex gas chromatography—tandem mass spectrometry (GC-MS/MS) technique is reported for indole-3-acetic acid, abscisic acid, jasmonic acid, 12-oxo-phytodienoic acid and salicylic acid. The optimized setup allows the routine processing and analysis of up to 60 plant samples of between 20 and 200 mg of fresh weight per day. The protocol was designed and the equipment used was chosen to facilitate implementation of the method into other laboratories and to provide access to state-of-the-art analytical tools for the acidic phytohormones and related signalling molecules. Whole-plant organ-distribution maps for indole-3-acetic acid, abscisic acid, jasmonic acid, 12-oxo-phytodienoic acid and salicylic acid were generated for Arabidopsis thaliana (L.) Heynh. For leaves of A. thaliana, a spatial resolution of hormone quantitation down to approximately 2 mm2 was achieved.

There is a growing awareness of the need to reduce the negative impact of chemical analyses on the environment and to develop new eco-friendly and sustainable analytical methods without compromising performance. In this study, we developed a \"green\" analytical method enabling the accurate and simultaneous routine analysis of 21 polycyclic aromatic hydrocarbons (PAHs) in reduced quantities (100 mg and 1 g wet weight (WW)) of marine biota samples (fish muscle, mussel and oyster tissues) using alkaline digestion combined with stir bar sorptive extraction-thermal desorption-gas chromatography-tandem mass spectrometry (SBSE-GC-MS/MS). The innovative method provides good selectivity and specificity for most compounds. In 1 gWW samples, limits of quantification (LOQs) ranged from 1 to 10 mu g/kgWW in fish muscle and from 0.5 to 10 mu g/kgWW in mussel tissue. The method enables most analytes to be quantified below the restrictive limits established by the European Commission (2 and 10 mu g/kgWW in fish muscle and bivalve mollusc, respectively). Higher LOQs were obtained in 100 mgWW samples ranging from 1 to 50 mu g/kgWW. Recovery and linearity were assessed for all analytes. The results were satisfactory for most compounds with recoveries ranging from 94% to 117% in 1 gWW mussel samples at spike concentration of 10 ng/gWW with standard deviation not exceeding 12%. However, results confirmed that the SBSE efficiency is affected by the complexity of biological matrices, especially for high molecular weight compounds in lipid-rich mussel tissue. Because of the matrix effects, matrix-matched calibrations were carried out. Validation was performed using the standard reference material 1974c with recovery ranging from 71% to 119% except for naphthalene, anthracene and benzo(e)pyrene that were therefore not validated. Overall, the developed method meets analytical validation criteria for most compounds. Thanks to the combination of alkaline digestion and SBSE, which greatly simplifies sample treatment and limits solvent use to ethanol, the developed method followed most green analytical chemistry principles.

Syzygium grande (Wight) Walp., commonly known as the sea apple, is valued for its wide range of uses. This study aimed to investigate the pharmacological effects of a methanol extract obtained from the leaves of S. grande (MESG) in Swiss albino mice. The extract's anxiolytic potential was assessed using the elevated plus maze (EPM), hole‐board test (HBT), and light–dark test (LDT). Its antidepressant activity was evaluated through the forced swimming test (FST) and tail suspension test (TST). Sedative properties were measured using the open field test (OFT) and hole‐cross test (HCT), while antipyretic activity was determined through a yeast‐induced fever model. To identify active compounds in the extract, GC–MS/MS analysis was conducted. Additionally, computational approaches—including AutoDock Vina, Discovery Studio 2021, PASS online, and ADME/T platforms—were employed for PASS prediction analysis, ADME/T profiling, and molecular docking of various secondary metabolites. The findings indicated that MESG exhibited dose‐dependent anxiolytic, antidepressant, sedative, and antipyretic effects. A 400 mg/kg dose significantly enhanced anxiolytic activity (p < 0.001) in all behavioral models. It also moderately reduced immobility in the FST and TST (p < 0.01). Furthermore, MESG significantly suppressed locomotor activity in the OFT and HCT (p < 0.001), indicating strong sedative action. The same dose effectively lowered rectal temperature in the fever model (p < 0.05). Computational docking scores, which ranged from −2.6 to −10 kcal/mol, further supported these biological effects. In conclusion, S. grande shows considerable promise as a source of therapeutic agents for treating anxiety, depression, insomnia, and fever. This study was designed to explore the pharmacological effects of the methanol extract derived from S. grande leaves (MESG) on Swiss albino mice. The extract displayed significant anxiolytic, sedative, and antipyretic effects with moderate antidepressant effects. GC–MS/MS analysis identified 64 compounds in MESG, some of which, such as phytol, have been previously reported to possess important neuropharmacological activities.

Understanding the fates and impacts of microplastics requires information on their sizes, polymer types, concentrations, and spatial and temporal distributions. Here, we focused on large (LMPs, 500 µm to 5 mm) and small (SMPs, 25 to 500 µm) microplastics sampled with the exact same protocol in nine of the major European rivers during the seven months of the Tara Microplastic Expedition. Attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR) and pyrolysis coupled with gas chromatography and mass spectrometry (Py-GC–MS) analyses were used to determine the microplastics contents by number and mass. The median LMP concentration was 6.7 particles m −3 , which was lower than those in other regions of the world (America and Asia). The SMP mass concentration was much higher to the LMP concentrations, with SMP/LMP ratios up to 1000 in some rivers. We did not observe a systematic positive effect of urban areas for the two size classes or polymers; this could be explained by the fact that the transport of microplastic is highly heterogeneous in rivers. We believe that this study has important implications for predictive models of plastics distribution and fate in aquatic environments. Graphical Abstract

Bacterial diseases are a global problem that threatens human health and cause many deaths each year. The alarming rise in bacterial resistance to modern antimicrobials is particularly concerning. In practice, this necessitates increasing the dosage of antimicrobial agents, posing a potential risk of adverse effects on human health. Additionally, the development of antibiotic resistance is one of the main factors contributing to the ever-growing costs of the global healthcare system. For these reasons, natural and safe antimicrobial agents are increasingly sought after. In this study, the antibacterial activity of 31 different essential oils (EOs) was investigated against Escherichia coli and Staphylococcus aureus. The most effective EOs were further tested both individually and in dual combinations. Minimum inhibitory concentrations (MICs) and fractional inhibitory concentrations (FICs) were determined to reveal synergistic effects, suggesting potential practical applications. The main bioactive compounds of the EOs with the highest inhibitory activity were identified and quantified using GC-MS/MS analysis. Of the tested EOs, seven demonstrated a strong antimicrobial effect against E. coli, most notably oregano (MIC 128 µg/mL) and the thyme/oregano combination (MIC 64 µg/mL, FIC 0.75), while thirteen were effective against S. aureus, most notably oregano and garlic (MIC 128 µg/mL),and the pelargonium/garlic combination (MIC 32 µg/mL, FIC 0.375). The pharmaceutical, agricultural, and food industries are promising fields for the application of these safe and natural antimicrobial agents, offering a new range of solutions to combat serious bacterial pathogens.