Search Results (359)

Sea pollution caused by anthropological activities represents a risk both for the organisms that inhabit it and for humans themselves. Great attention is paid to plastic waste because it takes decades to decompose and fragments into microscopic pieces that can be easily dispersed and ingested by marine fauna. Polymeric materials, in general, are rich in plasticizers (phthalates, PAEs; and bisphenol A, BPA), substances recognized as toxic both for aquatic organisms and for humans who could ingest them once contaminated marine organisms were to enter their diet. In this work, effective analytical protocols based on the use of solid phase microextraction (SPME) coupled with chromatography techniques were employed to evaluate the presence of PAEs and BPA in the extracted pulp of shrimps of the commercial species Aristaemorpha foliacea from four different fishing stations in the Mediterranean Sea. In addition to chemical analysis, a comprehensive microbiological characterization was carried out to assess microbiological risk due to shrimps’ consumption. This dual approach provides a more complete evaluation of the impact of human pollution on these crustaceans, revealing both chemical contamination and potential biological disruptions that could pose a danger to food safety. Full article

Wastewater analysis plays a central role in monitoring patterns of drug use within specific populations. It provides objective and real-time estimates of consumption, with minimal ethical concerns. In the current European context, drugs of abuse continue to be detected in wastewater, with varying incidences across countries. Their monitoring enables the prioritisation of public health and legal interventions by healthcare professionals and drug monitoring agencies. Therefore, the development and implementation of efficient methodologies for monitoring drugs of abuse in wastewater samples is of critical importance. This systematic review aims to explore the use of miniaturised sample extraction techniques based on solid-phase microextraction for the determination of drugs of abuse in wastewater. In fact, the extraction procedure must be fast, effective, and selective in order to retain the analytes of interest. Miniaturised techniques have thus emerged as promising alternatives to conventional methods. Magnetic solid-phase extraction (MSPE) and molecularly imprinted polymers (MIPs) represent the most widely applied solid-phase microextraction techniques in recent years for the analysis of drugs of abuse in wastewater. Looking ahead, future perspectives include the development of eco-friendly workflows, automated and time-efficient techniques, increasingly selective sorbents, and robust analytical methods. Full article

Theophylline represents a significant public health challenge due to its dual acute and chronic toxicity resulting from therapeutic, environmental, and dietary exposures. Effective monitoring across the bio-environmental–food triad requires analytical methods that are highly sensitive, universally applicable, and capable of overcoming complex matrix interferences. This study introduces a flat membrane-based liquid-phase microextraction (LPME) technique combined with LC–MS/MS for the determination of theophylline in diverse matrices. The method eliminates the need for specialized adsorbents or equipment, offering a simple and cost-effective solution for high-throughput sample clean-up. Under optimized conditions, the method demonstrated exceptional sensitivity (LOD: 0.2 ng mL⁻¹) and a wide linear range (0.01–10 μg mL⁻¹). It was successfully applied to plasma, urine, hospital sewage, and green tea, providing accurate (recoveries of 86.7–111.3%) and reproducible (RSD < 10%) results across all matrices. This unified and robust approach effectively addresses matrix interferences and provides a reliable tool for the monitoring and risk assessment of theophylline across multiple domains. Full article

Volatile organic compounds (VOCs) play critical roles in broccoli’s sensory attributes, defense mechanisms, and ecological interactions, yet comprehensive profiling of its volatilome remains limited. This study aimed to construct a robust and inclusive volatile metabolite database for broccoli using advanced analytical techniques. A pooled sample comprising florets from 191 cultivars was prepared to capture broad chemical diversity and analyzed using solid-phase microextraction–gas chromatography–high-resolution mass spectrometry (SPME-GC-HRMS) under dual ionization modes: electron ionization (EI) and chemical ionization (CI). A total of 206 VOCs spanning nine chemical classes were detected, with 37 compounds further confirmed through synchronized CI analysis. To validate the database, broccoli florets from seven distinct cultivars were analyzed using the same workflow. Of the 206 compounds, 187 (90.78%) were detected in at least one cultivar, while 38 were consistently found across all samples, indicating a conserved core volatilome. Principal component analysis revealed distinct VOC profiles among cultivars, and freeze-dried samples were found suitable for reproducible large-scale analysis. This study demonstrates that a pooled-sample strategy coupled with dual-ionization GC-HRMS provides comprehensive and reliable VOC coverage. The resulting database offers a valuable resource for metabolomics studies in Brassica, with applications in cultivar differentiation, flavor research, and environmental response profiling. Full article

Hydrolates are aromatic aqueous solutions saturated with volatile water-soluble compounds of essential oil. Despite their potential, hydrolates remain less explored than essential oils. In this work, the hydrolate of Pelargonium odoratissimum (L.) L’Hér. has been analyzed by multiple analytical techniques in order to describe its chemical composition. Headspace (HS-) and Direct Immersion-Solid Phase Microextraction-Gas Chromatography/Mass spectrometry (DI-SPME-GC/MS) and Proton Transfer Reaction Time-of-Flight Mass Spectrometry (PTR-ToF-MS) were employed to reveal the VOC emission from the hydrolate. Further, a direct injection of the pure hydrolate and of the hydrolate after extraction with hexane was performed by Large-Volume Injection Gas Chromatography/Mass Spectrometry (LVI-GC/MS) and GC/MS. The results obtained by HS- and DI-SPME-GC/MS highlighted a nearly overlapping chemical profile with linalool, isomenthone, and α-terpineol as the main volatiles. On the other hand, analysis of the hydrolate by GC/MS after solvent extraction revealed a lower overall number of compounds but allowed the detection of thujone and cis-linalool oxide. In comparison, LVI-GC/MS was the technique that allowed the identification of a higher number of volatiles with citronellol, linalool, and α-terpineol as the principal compounds. Finally, PTR-ToF-MS was a fundamental approach to quantify and evaluate total terpene emissions from this complex matrix starting from low-molecular-weight compounds such as acetylene, methanol, acetaldehyde, acetone, and ethanol, which were the most abundant. Among the detected compounds, dimethyl sulfide and small amounts of dimethyl-furan and 2-butylfuran were also identified. Overall, the findings showed that the hydrolate was rich in monoterpene compounds while sesquiterpene compounds were missing. A very low intensity relating to sesquiterpenes was recorded only by PTR-ToF-MS technique. Full article

Background: Colorectal cancer (CRC) remains one of the leading causes of cancer-related mortality worldwide, emphasizing the urgent need for early, non-invasive, and accessible diagnostic tools. This study aimed to evaluate the effectiveness of a microelectromechanical systems (MEMS)-based electronic nose (E-nose) in combination with gas chromatography–mass spectrometry (GC-MS) for CRC detection through sweat volatile organic compounds (VOCs). Methods: A total of 136 sweat samples were collected from 68 volunteer participants. Samples were processed using solid-phase microextraction (SPME) and analyzed by GC-MS, while a custom-designed E-nose system comprising 14 gas sensors captured real-time VOC profiles. Data were analyzed using multivariate statistical techniques, including PCA and PLS-DA, and classified with machine learning algorithms (LDA, LR, SVM, k-NN). Results: GC-MS analysis revealed statistically significant differences between CRC patients and healthy controls (COs). Cross-validation showed that the highest classification accuracy for GC-MS data was 81% with the k-NN classifier, whereas E-nose data achieved up to 97% accuracy using the LDA classifier. Conclusions: Sweat volatilome analysis, supported by advanced data processing and complementary use of E-nose technology and GC-MS, demonstrates strong potential as a reliable, non-invasive approach for early CRC detection. Full article

Nuts are nutrient-dense foods recognized for their complex chemical composition and associated health benefits. This review provides a comprehensive overview of the botanical classification, morphology, production, and consumption patterns of key nut species, including walnuts, almonds, pistachios, pecans, peanuts, cashews, bitter kola, and kola nuts. It emphasizes the fatty acid profiles, noting that palmitic acid (C16:0) is the predominant saturated fatty acid, while oleic acid (C18:1) and linoleic acid (C18:2) are the most abundant monounsaturated and polyunsaturated fatty acids, respectively. The review also details various analytical techniques employed for extracting and characterizing bioactive compounds, which are crucial for assessing nut quality and health benefits. Methods such as Soxhlet extraction, solid-phase microextraction (SPME), supercritical fluid extraction (SFE), gas chromatography (GC-FID and GC-MS), and high-performance liquid chromatography (HPLC) are highlighted. Furthermore, it discusses scientific evidence linking nut consumption to antioxidant and anti-inflammatory properties, improved cardiovascular health, and a reduced risk of type 2 diabetes, establishing nuts as important components in a healthy diet. This review underscores the role of nuts as functional foods and calls for standardized methodologies in future lipidomic and volatilomic studies. Full article

The analysis of wastewater is essential in environmental chemistry, particularly for monitoring emerging contaminants and assessing ecological impacts. In this context, hyphenated chromatographic techniques are widely used, with liquid chromatography being one of the most common. However, gas chromatography coupled with mass spectrometry (GC-MS) remains a valuable tool in this field due to its sensitivity, selectivity, and widespread availability in most laboratories. This review examines the application of validated methods for wastewater analysis using GC-MS (MS), highlighting its relevance in identifying micropollutants such as pharmaceuticals, drugs of abuse, pesticides, hormones, and industrial by-products. The validation of analytical methods is crucial to ensuring the reliability and reproducibility of data and the accurate monitoring of contaminants. Key parameters, including sample volume, recovery efficiency, and detection and quantification limits, are discussed, evaluating different approaches to optimising the identification of different classes of contaminants. Additionally, this study explores advances in sample preparation techniques, such as solid-phase microextraction (SPME), dispersive liquid–liquid microextraction (DLLME), and solid-phase extraction (SPE), which enhance efficiency and minimise interferences in the analysis. Finally, future perspectives are discussed, including the integration of emerging technologies such as high-resolution mass spectrometry, the miniaturisation of GC systems, and the development of faster and more sustainable analytical methods. Full article

The growing demand for healthy and sensorially pleasing foods is accompanied by increasing sustainability concerns among consumers and industry. Therefore, exploring native and underutilized resources for traditional preparations is important. This study evaluated the incorporation of Moringa oleifera leaves and baru almonds (Dipteryx alata) in pesto sauce, comparing them to the traditional recipe regarding composition, color, total phenolics, volatiles, sensory characteristics, and acceptability. The following four formulations were developed: basil with cashew nuts (B/CN); basil with baru almonds (B/BA); and two versions with 50% basil replaced by moringa, combined with cashew (BM/CN) or baru (BM/BA). BM/BA presented the highest protein content (9.0%), compared to B/CN (7.9%). BM/CN showed a greener color. BM/CN and BM/BA showed total phenolics and antioxidant capacities similar to B/CN. BM/BA showed elevated condensed tannins (113.28 mg CE/100 g). All samples contained 1,8-Cineole and linalool, key to the aroma of basil. Pesto with moringa and/or baru showed good sensory acceptance, rated as “liked moderately”, with no difference from the conventional version (p > 0.05). There were no differences in the basil aroma, nutty flavor, or greasiness. Pesto sauce is a promising matrix for incorporating regional, underused ingredients such as moringa leaves and baru almonds, expanding their potential in new food development. Full article

Sparkling wine is a complex alcoholic beverage with high economic value, produced through a secondary fermentation of a still wine, followed by a prolonged aging period that may last from nine months to several years. With the growing global demand for high-quality sparkling wines, understanding the biochemical mechanisms related to aroma development has become increasingly relevant. This review provides a comprehensive overview of the secondary fermentation process, with particular emphasis on yeast selection, types of closure, and the impact of aging on the volatile composition. Special attention is also given to the analytical strategies employed for the identification and quantification of target compounds in sparkling wine matrices. Due to the presence of volatile compounds at trace levels, effective extraction and pre-concentration techniques are essential. Extraction methods such as solid-phase microextraction (SPME), stir-bar sorptive extraction (SBSE), and thin-film SPME (TF-SPME) are discussed, as well as chromatographic techniques, such as gas chromatography (GC) and liquid chromatography (LC). Full article

Wuyi Shuixian tea, a premium oolong tea known for its complex floral-fruity aroma, exhibits significant quality variations across different grades. This study systematically analyzed the aroma characteristics and key fragrant compounds of four grades (Grand Prize SA, First Prize SB, Outstanding Award SC, and Non-award SD) using headspace solid-phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS), odor activity value (OAV) analysis, and multivariate statistical methods. A total of 159 volatile compounds were identified, with similar compound categories but distinct concentration gradients between grades. OAV-splitting analysis (based on OAV ≥ 1 as the threshold for aroma activity) identified β-ionone (fruity), octanal (fatty), and linalool (floral) as core aroma-active contributors, as their OAV values significantly exceeded 10 in awarded grades (SA, SB, SC), indicating dominant roles in sensory perception. Notably, linalool, a floral marker, showed a concentration gradient (SA > SB > SC) and was absent in SD, serving as a critical determinant of grade differentiation. Orthogonal partial least squares-discriminant analysis (OPLS-DA) further distinguished awarded grades (SA, SB, SC) by balanced fruity, floral, and woody notes, while SD lacked floral traits and exhibited burnt aromas. This classification was supported by hierarchical clustering analysis (HCA) of volatile profiles and principal component analysis (PCA). Electronic nose data validated these findings, showing strong correlations between sensor responses (W5S/W2W) and key compounds like hexanal and β-ionone. This study elucidates the molecular basis of aroma-driven quality grading in Wuyi Shuixian tea, providing a scientific framework for optimizing processing techniques and enhancing quality evaluation standards. The integration of chemical profiling with sensory attributes advances precision in tea industry practices, bridging traditional grading with objective analytical metrics. Full article

Cannabis remains the most widely used illicit drug worldwide, identifying it is a routine procedure in forensic toxicology. Due to its widespread use, there is a need for analytical methods that can detect it in biological samples. Hair is of particular interest in forensic toxicology as it is the only biological sample that enables retrospective analysis of consumption. In addition, collecting hair is non-invasive, and the specimens can be stored at room temperature. However, the sample preparation process for hair is tedious and multi-step. To address this issue, this study introduces a novel approach to preparing hair samples for analysis, based on air-assisted liquid–liquid microextraction (AALLME). This technique is a modification of dispersive liquid–liquid microextraction (DLLME), which eliminates the need for dispersants and chlorinated organic solvents as extractants. Both techniques offer sustainable alternatives to conventional liquid–liquid extraction (LLE) and solid-phase extraction (SPE), making them of interest in forensic toxicology. This study is the first to report the application of AALLME to the hair matrix. A mixture of cyclohexane and ethyl acetate (9:1) was used as the extractant solvent. Gas chromatography–mass spectrometry (GC–MS) was then used to determine and quantify THC. The method was validated according to FDA guidelines and demonstrated good linearity within the 0.01–4 ng/mg range. The limits of detection (LOD) and quantification (LOQ) were 0.008 and 0.01 ng/mg, respectively. Finally, the applicability of the method was evaluated by analyzing hair samples received by the Forensic Toxicology Service. Full article

Untreated olive oil mill wastewater (OOMW) from conventionally farmed olives was used in bread production to create a new functional product. Two types of bread were developed with 50% OOMW (EXP-1) and 100% OOMW (EXP-2) replacing water. Two leavening processes were tested: sourdough inoculum (S) vs. biga-like inoculum (B), with controls (CTR) without OOMW addition. The doughs were monitored throughout the acidification process by measuring pH, total titratable acidity, and the development of key fermentative microorganisms. To assess the hygienic quality during fermentation, plate count techniques were employed. After baking, the breads were evaluated for various quality parameters, including weight loss, specific volume, crumb and crust colors, image analysis, and the presence of spore-forming bacteria. Volatile compounds released from the breads were identified using solid-phase microextraction coupled with gas chromatography–mass spectrometry (SPME-GC/MS). Polyphenolic compounds were analyzed via liquid chromatography–mass spectrometry (LC-MS). To assess the functional properties of the final products, the breads were homogenized with synthetic human saliva and subjected to in vitro digestion. OOMW did not significantly affect the growth of yeasts and lactic acid bacteria (LAB) or the acidification process. However, in terms of the specific volume and alveolation, breads from the S process and OOMW had poor quality, while those from the B process had better quality. Experimental breads (EXP_B-1 and EXP_B-2) contained higher levels of alcohols (especially ethanol and isobutyl alcohol), carbonyl compounds (like benzaldehyde), esters (such as ethyl caproate and ethyl caprylate), and terpenes. OOMW introduced phenolic compounds like hydroxytyrosol, coumaric acid, caffeic acid, and trans-hydroxycinnamic acid, which were absent in CTR_B breads. Functionalization of EXP_B-1 and EXP_B-2 breads was demonstrated by a 2.4- and 3.9-fold increase in Trolox equivalents, respectively. However, OOMW did not reduce post-prandial hyper-glycemia, as starch digestibility was similar between CTR_B and EXP_B breads. The sensory analysis, which focused solely on the visual, structural, and olfactory characteristics of the breads, excluding taste testing to prevent potential health risks from residual pesticides, showed a high appreciation for EXP_B-1 and EXP_B-2 breads, scoring higher than CTR_B in the overall assessment. Full article

Background: Chemical odor profiling within forensic entomology is an emerging tool given its potential for species identification and larval aging and its ability to identify decomposition stages. A volatile analysis of larval masses across species of distinctive developmental stages was carried out with extraction techniques to identify odor signatures. However, it is unknown how larval sample handling (i.e., live samples in research vs. hot-water-killed samples in casework) affects odor signatures or the possibility of obtaining relevant volatiles from a single larva. Method: This study utilized solid-phase microextraction (SPME) with gas chromatography–mass spectrometry (GC/MS) for the analysis of odor volatiles emanating from single larval samples of Cochliomyia macellaria. Fifty (50) larvae (25 live; 25 boiled) were analyzed. Results: The SPME-GC/MS method allowed for odor volatile detection from a single maggot regardless of the sample handling group. The main compounds identified across both groups included those previously reported as emanating from larvae and decomposition substrates. When comparing treatments, the boiled larval samples had a 6-fold decrease in compound abundance compared to the live samples. The identified odor volatiles observed in the hot-water-killed treatment group included indole, p-cresol, and phenol. Conclusions: These results suggest that the handling technique impacts odor detection. Additionally, the heterocyclic aromatics and alcohols identified in the boiled samples are potentially odor markers of a higher intrinsic nature to the maggot rather than a cross-transfer from the decomposition substrate given their survival post elevated temperature treatment. This work shows the plausibility of carrying out an odor analysis of a single maggot following both common research and casework handling practices. Full article

The tomato russet mite (TRM), Aculops lycopersici, is a destructive pest of tomato crops worldwide. It poses a significant challenge to growers in both greenhouse and open-field conditions. Traditional chemical control methods are often ineffective, promote resistance, and have negative environmental impacts. This has prompted the search for alternative strategies, such as biological control and eco-friendly botanical pesticides. In this study, we evaluated the acaricidal effects of essential oils (EOs) extracted from three officinal plants, Origanum vulgare L., Salvia rosmarinus Spenn., and Salvia officinalis L., cultivated using precision aromatic crop (PAC) techniques. Their efficacy was evaluated against A. lycopersici under laboratory conditions. The chemical composition of the EOs was determined by solid-phase microextraction (SPME) coupled with gas chromatography–mass spectrometry (GC-MS). The dominant component of O. vulgare EO was carvacrol (83.42%), followed by ρ-cymene (3.06%), and γ-terpinene (2.93%). In S. rosmarinus, α-pinene (28.0%), 1,8-cineole (11.00%), and borneol (7.72%) were the major components. S. officinalis EO was characterized by high levels of 1,8-cineole (27.67%), camphor (21.91%), and crisantenone (12.87%). We tested multiple concentrations (320–5000 μL L−¹) and exposure times (1–4 days) to assess mite mortality. The results revealed both dose- and time-dependent toxic activity, with significant differences among EOs. O. vulgare EO was the most toxic, causing 90% mortality at 0.5% (w/v) concentration after 4 days. S. rosmatinus and S. officinalis EOs had more limited effects, with 46% and 42% mortality, respectively. Lethal concentration (LC₅₀) values were 2.23 mL L−¹ (95% CI: 1.74–3.05) for O. vulgare, 5.84 mL L−¹ (95% CI: 3.28–22.29) for S. rosmarinus, and 6.01 mL L−¹ (95% CI: 2.63–261.60) for S. officinalis. These results indicate that O. vulgare EO shows efficacy comparable to commercially available botanical pesticides. Our findings support the potential of O. vulgare EO as a viable alternative for the control of A. lycopersici, contributing to integrated pest management (IPM) strategies. Full article