Search Results (130)

Volatile sulfur compounds (VSCs) are important contributors to mango volatile profiles but are challenging to analyze due to their trace concentrations, susceptibility to transformation, and interference from the complex fruit matrix. This study investigated how key extraction parameters—material chemistry, surface area-to-volume ratio, sorbent volume, temperature, and time—affect VSC extraction using mango as a complex botanical model. Three sorptive extraction configurations were evaluated: HiSorb (PDMS and DVB/CWR/PDMS) and a high-capacity combined headspace thin-film solid-phase microextraction and stir bar sorptive extraction (HS-TFSPME-SBSE) system. The optimized HS-TFSPME-SBSE configuration (40 °C, 150 min) provided the broadest VSC coverage, achieving limits of detection of 0.1–0.6 μg/kg and good linearity (R² > 0.9927). In spiked mango puree (10 μg/kg), HS-TFSPME-SBSE detected methyl mercaptan and diallyl trisulfide, which were not recovered using HiSorb (PDMS). Application to three mango cultivars (Golden Honey, Sindhura, and Palmer) revealed broader VSC profiles and enabled differentiation of cultivars and tissues (flesh and peel) through principal component analysis (PCA). Distinct cultivar-associated VSC patterns were observed, including elevated dimethyl disulfide in Golden Honey and ethyl 3-(methylthio)-cis-2-propenoate in Sindhura. These findings demonstrate the suitability of HS-TFSPME-SBSE for sensitive profiling of trace VSCs in complex fruit matrices. Full article

Toxicological testing for drugs of abuse (DOAs) is an essential tool for healthcare practitioners and law enforcement agencies. Oral fluid (OF) is an alternative biological fluid for detecting recent DOA intake and is widely employed in forensic investigations. In the current study, a relatively novel and “green” fabric phase sorptive extraction (FPSE) procedure for sample preparation was coupled to liquid chromatography–tandem mass spectrometry (LC–MS/MS) to provide simplicity, cost-effectiveness, rapidity, low solvent consumption, and high analytical performance for the quantitative determination of ten commonly encountered DOAs and metabolites: amphetamine, benzoylecgonine, cocaine, codeine, ecgonine methyl ester, methadone, methamphetamine, 3,4-methylenedioxyamphetamine, 6-monoacetylmorphine, and morphine. The FPSE procedure was optimized by testing different filters, pH, extraction time, and solvents. The validated method demonstrated excellent linearity for all analytes, selectivity, acceptable precision, and high sensitivity (ranges for limits of detection (LODs) and quantification (LOQs) were 0.01–2 ng/mL and 0.03–6 ng/mL, respectively). Autosampler and short-term freeze stability exceeded 95% and 90% for all analytes, respectively. Overall, the combination of FPSE with LC–MS/MS provided a sensitive, selective, and environmentally friendly innovative analytical approach for the determination of DOA in OF and is suitable for both screening and confirmatory forensic and clinical applications. Full article

Depletion of reserves of rich copper–porphyry ore deposits necessitates the development of highly efficient methods for Mo (VI) extraction from complex, corrosive hydro-metallurgical media. The present study undertakes a comprehensive assessment of sorptive concentration of Mo (VI) from strongly acidic sulfate solutions (120 g/L H₂SO₄) by employing a spectrum of commercially available strong- and weak-base anion-exchange resins. It has been established that the macroporous weak-base anion exchanger Purolite A-100 demonstrates decisive superiority over gel-type analogs (Lewatit M-800, AB-17), facilitating unimpeded intra-gel diffusion of bulky molybdenyl sulfato-complexes anions, thereby circumventing the obstructive “sieve effect.” Thermodynamic and kinetic investigations revealed that the sorption process exhibits pronounced concentration- and pH-dependent characteristics. Peak extraction efficiency (up to 95.91%) is achieved at pH ≈ 1, a finding that correlates with the region of maximal protonation of tertiary amino groups within the resin matrix. Kinetic acceleration of mass transfer upon heating to 80 °C has been experimentally confirmed, yielding 94.6% extraction within 60 min. The obtained results corroborate the prospective integration of macroporous weak-base anion exchangers into operational hydro-metallurgical schemes as an environmentally benign and efficacious alternative to conventional solvent extraction of molybdenum. Full article

Rakı, a traditional distilled beverage produced from grapes, holds significant economic importance in Türkiye; however, comprehensive consumer-focused sensory research remains limited. This study aims to determine the aroma profile, sensory characteristics, and consumer preferences of commercial rakı to guide producers in aligning product characteristics with consumer expectations. Nine commercial rakı samples were evaluated. The aroma composition was analyzed using SBSE-GC-MS. Sensory attributes were assessed by a trained panel through descriptive analysis (DA) and by 100 consumers utilizing the Check-All-That-Apply (CATA) method alongside a liking test. Eighty-one aroma compounds were identified, predominantly the phenylpropanoids trans-anethole and estragole, with monoterpenes and sesquiterpenes dominating the secondary profile. Integrating instrumental data with DA evaluations suggests that anethole and sesquiterpenes likely contribute to the attributes related to visual coating, body, creamy, mastic, persistency, and complexity. Consumer profiling revealed two distinct preference groups. Older, frequent consumers preferred complex, high-alcohol profiles with trigeminal harshness and visual glass coating, whereas younger, casual consumers preferred smoother rakı with a traditional white appearance, reacting negatively to “boiled aniseed” flavors and the yellowish tint of oak-aged versions. The CATA technique effectively distinguished these profiles. To enhance overall product quality, producers should eliminate “boiled” defects and adjust sensory profiles: complex products for experienced consumers and visually traditional, smooth profiles for younger consumers. According to current knowledge, this is the first study to employ the CATA method alongside consumer profiling and preference mapping in the sensory evaluation of rakı. Full article

This study investigated the aroma characteristics of three grades of raw tea leaves and their corresponding jasmine tea products from Guangxi, China. Aromatic profiles of jasmine tea varieties were analysed using two-dimensional gas chromatography-olfactory-mass spectrometry (GC×GC-O-MS), stir bar sorptive extraction (SBSE), and descriptive sensory evaluation. Chemometric methods were applied to compare sensory scores with instrumental data. Volatile compound concentrations and relative odour activity values (r-OAVs) were calculated. The results indicated significant differences in base tea leaf quality: high-grade tea leaf G1 exhibited pure, sweet characteristics, serving as an excellent aroma-absorbing carrier. The scenting process significantly imparted jasmine fragrance to the finished product, although its efficacy was constrained by tea leaf grade. GH1 finished tea exhibited a fresh, vibrant, and rich aroma with a sweet, mellow fragrance and high floral integration. In contrast, GH3, due to its inferior base material quality, yielded a weak aroma after scenting with limited quality improvement. The initial quality of the tea base is the fundamental determinant of the upper limit of the finished jasmine tea’s sensory quality, while the scenting process is the core means of shaping its signature floral aroma. The combination of high-quality tea leaves and precise scenting techniques is essential for developing the fresh, vibrant, and rich flavour profile of premium jasmine tea. This study reveals that the flavour formation of jasmine tea originates from the foundational quality of the tea leaves, providing a theoretical basis for monitoring the aroma quality of jasmine tea produced from different grades of tea leaves. Full article

The rapid growth and diversification of the cosmetic industry have led to increasingly complex formulations containing numerous bioactive ingredients, excipients, and synthetic additives, often delivered through advanced nanostructured systems. Ensuring product safety, efficacy, and regulatory compliance requires analytical approaches capable of accurately detecting both declared components and hazardous contaminants such as heavy metals, phthalates, nitrosamines, and banned preservatives or dyes. Traditional sample preparation methods are often solvent-intensive, time-consuming, and environmentally burdensome, prompting a shift toward green microextraction strategies aligned with the principles of green analytical chemistry. Techniques including solid-phase microextraction (SPME), stir bar sorptive extraction (SBSE), and dispersive liquid–liquid microextraction (DLLME) offer miniaturized, solvent-efficient workflows with improved selectivity and sensitivity for complex cosmetic matrices. This review summarizes advances from the past five years in green microextraction methods for the determination of organic and inorganic species in cosmetic products. Emphasis is placed on their integration with separation techniques and applicability across product categories. Emerging trends, analytical challenges, and future directions toward more sustainable cosmetic safety assessment are also highlighted. Full article

Pesticide contamination poses significant threats to both humans and the environment, with residues frequently detected in surface waters worldwide. This study compares the effectiveness of passive samplers (POCIS and Chemcatcher) and grab sampling coupled with Stir-Bar Sorptive Extraction (SBSE) and Solid-Phase Extraction (SPE) for monitoring pesticides in surface waters. The comparative study was conducted at three sites in Victoria, Australia, representing different land uses. A total of 230 pesticides were screened, with 79 different pesticides detected overall. SBSE extracted the highest number of pesticides from grab samples, followed by SPE and passive samplers. The study highlights the complementarity of different sampling and extraction techniques in detecting a wide range of pesticides. The study also explores the suitability of these techniques for citizen science applications, emphasizing the importance of selecting appropriate methods based on specific research objectives and available resources. The findings underscore the need for a tiered approach, combining passive samplers for initial screening and grab sampling for quantitative analysis, to develop a robust monitoring strategy for protecting water quality. Full article

The growing interest in sustainable and structurally diverse sorbent materials has intensified the search for effective biosorbents that can complement or replace conventional adsorbents. This work presents the potential use of Chlorella vulgaris dried biomass and its modifications (ultrasound-treated, lipid-extracted, and combined forms) for diclofenac (DCF) sorption from aqueous solutions. It was demonstrated that sorption efficiency significantly depends on the solution’s pH. Lowering the pH from 6 to 2 increases the sorption from 5% to 68%, while 99% desorption occurred at pH 9. The adsorption isotherms for intact biomass and after lipid extraction (CV-E2) are best described by the Langmuir and Freundlich models; for ultrasonically treated biomass (CV-E1) by the Temkin model; and for ultrasound-assisted solvent extraction (CV-E3) by the Dubinin–Radushkevich model. These findings demonstrate that cellular lipids and particle characteristics critically govern sorption mechanisms, highlighting dried Chlorella biomass as a structurally and chemically tunable biosorbent. Importantly, the key sorption experiments were performed under strongly acidic conditions (pH 2), which differ from typical wastewater or surface water matrices. Therefore, the presented results should be regarded as a proof of concept illustrating the mechanistic potential of dried Chlorella biomass as a tunable sorptive material, with prospective relevance for separation science and laboratory-scale analytical applications rather than direct environmental remediation. Full article

Apple aroma is an important factor influencing consumers’ preferences. To understand the overall flavor characteristics of apples (Ruixue, Liangzhi, Grystal Fuji, and Guifei), volatile compounds and aroma profiles were investigated by headspace–gas chromatography–ion mobility spectrometry (HS-GC-IMS) combined with stir bar sorptive extraction (SBSE) and gas chromatography–mass spectrometry (GC-MS). The results showed that a total of 56 aroma compounds were identified by SBSE-GC-MS, and 39 aroma-active compounds were screened out using aroma intensity (AI) and odor activity value (OAV). Aroma recombination experiments showed enhanced ‘fruity’ and ‘sweet’ notes, whereas ‘floral’, ‘woody’, and ‘green’ aromas were weaker compared to the Crystal Fuji sample. Additionally, GC-IMS coupled with principal component analysis (PCA) was used to distinguish the apple samples, and partial least squares regression (PLSR) was applied to explore the correlation between sensory attributes and characteristic aroma compounds. The results indicated that Crystal Fuji exhibited the greatest correlation with the “woody” attribute, and Ruixue was highly correlated with “fruity”, “green”, and “sour” attributes, while butanoic acid, β-damascenone, butyl acetate, pentyl acetate, furfuryl alcohol, γ-decalactone, and vanillin had a significant impact on the “flower” and “sweet” attributes of Guifei. This study clarified the characteristic aroma composition of the four apple cultivars, providing data support for apple flavor quality evaluation and cultivar optimization. Full article

The volatile profiles of beef steaks (Longissimus lumborum) were analysed both raw and grilled to five different internal temperatures, 55 °C, 60 °C, 71 °C, 77 °C, and 85 °C, representing very-rare, rare, medium rare, well-done, and very well-done, respectively. Volatile organic compounds (VOCs) were extracted using direct immersion high-capacity sorptive extraction (DI-HiSorb) and analysed by gas chromatography–mass spectrometry (GC–MS). A total of ninety-one VOCs were detected with forty-two significantly impacted by the degree of doneness, thirty of which had Variable in Projection score > 1. Principal Component Analysis produced three distinct clusters, (i) raw, (ii) very-rare, rare, and medium-rare, (iii) and well-done and very well-done. Direct immersion high-capacity sorptive extraction (DI-HiSorb) provided a comprehensive volatile profile of grilled beef steak across different degrees of doneness and revealed that the abundance of methyl esters. The main findings were that in relation to the degree of doneness methyl esters were significantly reduced, with both aldehydes and pyrazines increasing due to thermal lipid oxidation, Strecker degradation, and Maillard reaction, highlighting the significance of internal temperature on the volatile profile of steak during grilling. Full article

Background/objectives: Prostate cancer (PCa) is the most common cancer among males. Approximately 20–40% of patients with clinically localized PCa will present with a biochemical recurrence after a radical prostatectomy (RP), while some will present with recurrent metastasis. Monitoring the disease post-treatment is crucial for detecting a potential cancer recurrence early. Urinary volatile organic compounds (VOCs) have shown potential to detect PCa. However, their application in disease monitoring remains unexplored. Methods: A total of 165 urine samples were collected from male adults with biopsy-designated PCa-positive results before (n = 55) and after a RP (n = 55), and with biopsy-designated PCa-negative diagnosis (n = 55). The post-RP cohort was subdivided into three groups based on their health status after surgery as recovered healthy, biochemical recurrence, and recurrent metastasis. VOCs in the urine samples were extracted by stir bar sorptive extraction and analyzed using gas chromatography and mass spectrometry. We explored the use of metabolomics and a machine learning algorithm tool to investigate the potential of using VOCs for differentiating PCa diagnoses before and after the RP procedure with different outcomes. Results: Over 100 potential VOCs were identified to differentiate PCa patients before and after a RP, and those with biochemical recurrence and recurrent metastasis. Conclusions: Urinary VOCs are promising biomarkers that could be used to differentiate PCa patients pre- and post-RP. The findings from this research provide preliminary insights and could aid future investigations in developing tools for PCa patients after treatment. The absence of a validation cohort limits the reproducibility and translational impact of these findings; therefore, the results should be considered exploratory and require confirmation in larger, independent cohorts. Full article

This paper constitutes a preliminary study that evaluates the organic pollutants desorbed from “fresh” plastic litter, i.e., recently stranded items, on three beaches in Cadiz (SW Spain): Bajo de Guia, La Jara, and La Puntilla. Beach litter items were collected and classified in laboratory according to their composition and use. Leachates were obtained by stir bar sorptive extraction (SBSE) and analysed with gas chromatography–mass spectrometry (GC–MS). Fifty-five target organic compounds—including polycyclic aromatic hydrocarbons (PAHs), pesticides, fragrances, insect repellents, and UV filters—were quantified. Plastics accounted for the majority of litter by both number and weight. Cigarette butts and wipes were also prevalent and served as key sources of leachable PAHs. With respect to the main pollutants found in plastic films, hard plastics, and wipes, fragrances such as OTNE1 (1-Tetramethyl Acetyloctahydronaphthalene), OTNE2 (2-Tetramethyl Acetyloctahydronaphthalene), DEET (N, N-Diethyl-Meta-Toluamide), galaxolide, and tonalide were dominant, with concentrations exceeding 100 ng/g in some cases. DEET was the most common insect repellent detected. These findings underscore the role of beach litter, especially plastic waste, as a vector for persistent and emerging organic pollutants, highlighting the urgent need for improved waste management and monitoring practices to mitigate ecological risks associated with plastic pollution. Full article

In this study, a magnet-integrated fabric phase sorptive extraction (MI-FPSE) protocol was developed in combination with high pressure liquid chromatography—diode array detection (HPLC-DAD) for the simultaneous determination of five phenylurea pesticides (i.e., chlorbromuron, diuron, linuron, metoxuron, monuron) in environmental water samples. To produce the MI-FPSE device, two individual sol-gel coated carbowax 20 M (CW 20 M) cellulose membranes were fabricated and stitched to each other, while a magnetic rod was inserted between them to give the resulting device the ability to spin and serve as a stand-alone microextraction platform. The adsorption and desorption step of the MI-FPSE protocol was optimized to achieve high extraction efficiency and the MI-FPSE-HPLC-DAD method was validated in terms of linearity, sensitivity, selectivity, accuracy, and precision. The limits of detection (LODs) were found to be 0.3 μg L⁻¹. The relative recoveries were 85.2–110.0% for the intra-day and 87.7–103.2% for the inter-day study. The relative standard deviations were better than 13% in all cases. The green character and the practicality of the developed procedure were assessed using ComplexGAPI and Blue Analytical Grade Index metric tools, showing good method performance. Finally, the developed method was successfully used for the analysis of tap, river, and lake water samples. 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

In this study, weekly grab samples extracted by solid-phase extraction (SPE) and stir bar sorptive extraction (SBSE) were compared for the analysis of 230 pesticides in surface waters. Samples were collected from three different locations around Melbourne, Australia. Analysis was performed using Gas Chromatography Quadrupole Time of Flight High Resolution Mass Spectrometry (GC-QToF-HRMS). The two extraction techniques were compared, among others, for their limits of detection, recovery, extraction, and quantification efficiency of pesticides, as well as spatial and temporal differences in detected compounds. The target compounds screened were pesticides belonging mainly to the categories of fungicides, insecticides, and herbicides. Although SBSE extracted more pesticides at two out of three sites, SPE extracted total concentrations up to four times higher than SBSE over all sampling sites. The log K_OW of detected pesticides only partially explained the differences in detection, with SBSE performing better in the absorption of hydrophobic compounds. In addition, matrix effects, in particular turbidity, appeared to hinder extraction of contaminants, especially for SBSE. Spatially, SBSE detected 10 pesticides more than SPE at two locations, while the opposite was true at the third location, where turbidity was higher. The types of pesticides detected varied slightly between techniques and locations. The study highlights the complementarity of SBSE and SPE for monitoring pesticides in natural environments. SBSE is an easy-to-use technique and allows for extraction of a higher number of pesticides at trace level, but it might not be the preferred option for highly turbid waters. SPE requires more tedious and complex sample processing but allows for a more accurate quantification of a broader range of pesticides. Full article