Analytica

Sulforaphane (SFN), an isothiocyanate abundant in cruciferous vegetables, possesses well-documented anticancer, antioxidant, and anti-inflammatory properties, and has attracted interest as a dietary chemopreventive agent. However, sensitive and fully automated methods for its quantification in foods remain limited. In this study, we developed an automated analytical system coupling in-tube solid-phase microextraction (IT-SPME) with high-performance liquid chromatography–tandem mass spectrometry (LC–MS/MS) to determine SFN in vegetable samples. Vegetable samples were autohydrolyzed in aqueous solution at 37 °C to generate SFN, which was then extracted with methanol by sonication. The extract was concentrated onto a Carboxen 1006 capillary column by IT-SPME, separated within 5 min on an Inertsil C8 column, and detected in positive electrospray ionization mode using multiple reaction monitoring. The detection limit was 5.6 pg/mL, with good linearity (R² = 0.9995) over 0.1–100 ng/mL, intra- and inter-day precisions below 2.9% and 3.9%, respectively, and accuracy of 98–102%. SFN was detected at concentrations of 600 μg/g or higher in broccoli sprouts, florets, and stems, but was found at less than one-tenth of these levels in other vegetables tested. This method provides a simple, sensitive, and solvent-efficient tool for SFN quantification in vegetables, with potential application in food functionality assessment and chemopreventive research. Full article

Density measurement with vibrating tube density meters is a fundamental technique in biotechnology, for example, as the metrological base for spectroscopy calibrations. However, conventional multi-point adjustments frequently rely on hazardous halogenated solvents. In this work, green alternatives for density calibration are evaluated with a focus on replacing hazardous substances while maintaining analytical performance. Propylene carbonate is identified as an intrinsic candidate standard for densities up to 1.20 g/mL, eliminating reliance on conventional halogenated liquids. For routine verification and system suitability testing, binary aqueous solutions of sodium chloride and guanidine hydrochloride are proposed as secondary standards. Guanidine hydrochloride solutions provide particular advantages due to their moderate viscosity and high refractometric sensitivity, allowing independent verification of composition and extended usability. In addition, historical density data for NaCl and CsCl solutions were re-evaluated to showcase that in silico modeling can derive density–temperature–composition relations with reasonable overall accuracy. Overall, the proposed approach demonstrates that accurate density calibration in bioanalytical laboratories can be achieved using low-toxicity, non-halogenated substances thereby reducing environmental impact while supporting fit-for-purpose analytical performance. Full article

Synthetic azo dyes are relevant paprika adulterants and a food-safety concern when used in undeclared or non-authorized forms. This study investigated the quantification of three representative dyes—Allura Red (E129), Orange II, and Ponceau 4R (E124)—spiked into paprika powder from 0 to 6% w/w using a benchtop Fourier-transform NIR (FT-NIR) Büchi NIRFlex N-500 spectrometer and a handheld ASD QualitySpec Trek Vis-NIR spectrometer. The experimental design included 17 concentration levels per dye, 3 independently prepared spiked batches per level, randomized measurements over approximately 3 months, and 3 replicate spectral acquisitions per filled cuvette. Measurements were performed in the 10,000–4000 cm⁻¹ region with the benchtop FT-NIR instrument and in the 20,408–4000 cm⁻¹ region with the handheld Vis-NIR instrument. Spectra were evaluated by principal component analysis (PCA) and partial least squares (PLS) regression, with robustness assessed by grouped cross-validation and independent test-set validation using held-out concentration levels. To support model interpretation, anharmonic NIR spectra of the dyes were simulated using DVPT2 calculations and compared with the experimentally relevant loading regions. For FT-NIR, independent test-set validation gave RMSEP values of 0.315, 0.205, and 0.338% w/w and R²_TSV values of 0.970, 0.987, and 0.965 for Allura Red, Orange II, and Ponceau 4R, respectively. For Vis-NIR, the corresponding RMSEP values were 0.328, 0.262, and 0.334% w/w, with R²_TSV values of 0.968, 0.979, and 0.964. The models required only two to three latent variables. Orange II gave the strongest FT-NIR model, reflecting its more distinct NIR spectral response, while all Vis-NIR models remained compact two- to three-factor models due to the additional visible-region absorption of the azo chromophores. The simulated spectra supported assignment of the main FT-NIR model-relevant regions to aromatic C–H overtones and dense combination-band manifolds, while the Vis-NIR models were driven mainly by visible chromophore absorption. Full article

Microplastic contamination has become an emerging environmental concern in marine ecosystems worldwide. This study investigated the occurrence, abundance, size, color, and polymer composition of microplastics in surface water, marine sediments, and the gastrointestinal tracts of commercially important fish species collected from the coastal regions of Sousa and Alhaniyah along the northeastern Mediterranean coast of Libya. Microplastics were detected in 10 of 15 (66.7%) surface water samples from Sousa and in 5 of 15 (33.3%) samples from Alhaniyah. In bed sediments, microplastics were detected in 5 of 15 samples (33.3%) at both study sites. Microplastics were detected in 46.73% (71/149) of the fish specimens collected from Sousa and in 20.30% (25/123) of those collected from Alhaniyah. The mean microplastic abundance in surface water was 2.5 ± 2.6 particles/L in Sousa and 0.7 ± 1.3 particles/L in Alhaniyah. Mean sediment abundances were 254 ± 57 and 212 ± 23 particles/kg dry weight, respectively. These findings indicate microplastic contamination at both study sites, with spatial variation in abundance. Microplastic abundance in fish gastrointestinal tracts varied among species, with the highest mean values observed in Epinephelus marginatus (3.0 ± 1.6 particles/fish), followed by Alepes djedaba (2.7 ± 1.2 particles/fish) and Pagrus pagrus (2.3 ± 0.6 particles/fish). This variability revealed the species-specific exposure associated with the feeding behavior and habitat use. The microplastic particles observed were in sizes from 1.0 to 5.0 mm, with larger particles more prevalent in the sediments and smaller particles in fish. Nine different microplastic colors were seen, with blue being the most common, followed by black, green, white, transparent, yellow, glossy, red, and brown. Rayon, alkyd resin, polyamide, and poly(acrylonitrile) were identified at both study sites, whereas poly (ethylene terephthalate) (PET) was detected only at Alhaniyah. The overall similarity in polymer composition suggests that the two locations share common sources of microplastic contamination, while the occurrence of PET exclusively at Alhaniyah may indicate additional local inputs. However, further investigations are required to identify and confirm the specific sources of these polymers. This study provides the first baseline assessment of microplastic contamination in the coastal environments of Alhaniyah and Sousa, northeastern Libya. It offers a valuable reference for future monitoring and mitigation strategies. Full article

Liquid chromatography–hydrogen/deuterium exchange–mass spectrometry (LC-HDX-MS) provides orthogonal structural information that complements conventional LC-MS and improves confidence in small-molecule structural elucidation. Although HDX-MS is well established in protein research, its application to small molecules remains less developed, and practical guidance for experimental implementation and data interpretation is limited. Here, we evaluate major LC-HDX-MS strategies, including post-column co-infusion, partial HDX, and full HDX approaches, and assess their analytical performance using reference standards and NIST SRM 1950 human plasma. The effects of deuterated mobile phases on background contamination, labeled/unlabeled signal ratios, retention-time shifts, adduct chemistry, and mass spectral interpretation are examined, and currently available software tools for LC-HDX-MS data processing are discussed. Full HDX provided the most complete deuterium incorporation, whereas deuterated mobile phases increased background signals and generally reduced analyte responses. Retention-time shifts were typically small but should be considered when matching features. HDX-derived information provides an additional experimental structural descriptor by defining the number of exchangeable hydrogen atoms and refining adduct assignments, thereby reducing ambiguity during structural annotation. These findings provide practical recommendations for implementing LC-HDX-MS in untargeted LC-MS workflows and demonstrate its value as an orthogonal tool for small-molecule structural elucidation. Full article

During forest exploitation, large amounts of wood biomass are left as residues after harvesting, even though this material could be valuable in reducing greenhouse gas emissions by replacing fossil fuels and serving as a source of bioactive compounds. Within the context of the European Union’s circular bioeconomy strategy, enhancing the efficacy and rational application of forest logging residues constitutes a critical future objective. To evaluate the possible use of the stumps as forest residue-derived woody biomass for the first time, the chemical composition and presence of bioactive compounds in the xylem and bark of F. angustifolia Vahl. ssp. pannonica Soó & Simon stumps were analyzed, including the content of cellulose, acid-insoluble lignin, acid-soluble lignin, ash, and extractives soluble in toluene–ethanol and hot water. In hot water extracts, total phenolic content, the antioxidant activity determined by scavenging capacity toward DPPH and HPTLC, the content of elements by ICP-OES, and the identification of bioactive compounds by UHPLC-DAD-ESI MS/MS were assessed. Considering the chemical composition, the quality of the xylem of the F. angustifolia (cellulose: 42.46 ± 0.45%; lignin: 25.05 ± 0.02%; hemicelluloses: 19.74 ± 0.46%) was similar to that of the stem. Hot water extracts of the bark of F. angustifolia stumps showed high total phenolic content (33.94 ± 1.43 mg GAE/g DW) and strong antioxidant potential (198.48 ± 3.33 μmol TE/g DW), while toxic metals were not detected. UHPLC-DAD-ESI-MS/MS analysis indicated phenylethanoid glycosides as the dominant compounds in the extracts. The analyzed stumps of Fraxinus angustifolia Vahl. in the “Morović” Forest Administration represent a valuable biomass with potential for further valorization. Full article

Mercury contamination in aquatic environments poses significant risks to ecosystems and human health, underscoring the need for effective remediation technologies. This research examines the physicochemical properties of the synthesised polymer materials, and DFT calculations were used as an initial step for material development to validate our experimental outcomes for the prepared polymers: polyaniline (PANI), polyethersulfone (PES), and polyamidoamine (PAMAM). Furthermore, DFT studies were used to elucidate structure–property relationships in polymers, serving as performance predictors for mercury adsorption and selectivity, as well as for their applicability in electronic sensors. The characterisation techniques indicated the high functional group densities of PAMAM dendrimers for effective chelation, while the semi-crystalline structure of PANI improves metal binding. DFT calculations reveal that PAMAM exhibits the smallest HOMO–LUMO energy gap, indicating a high reactivity towards mercury ions. Binding energies indicate that PAMAM forms the most stable single-ion complex; PAM1Hg (0.242 eV, 23.37 kJ mol⁻¹), whereas PES exhibits enhanced interaction at elevated mercury concentrations, resulting in stable multi-Hg complexes, PES3Hg (0.136 eV, 13.13 kJ/mol). The findings indicate that nitrogen-rich functional groups and aromatic systems play a crucial role in mercury binding, highlighting the promise of conductive polymers for creating effective adsorbents aimed at mercury remediation in industrial wastewater. Full article

Supercritical carbon dioxide extraction (SFE-CO₂) is an efficient and environmentally friendly process for extracting bioactive compounds from plant material. This investigation examined the combined effects of air-drying temperature of the leaves and SFE-CO₂ operating conditions on the extraction yield, volatile compound composition, and antimicrobial activity of Pistacia lentiscus leaf extracts. Extractions were performed at pressures ranging from 100 to 200 bar and temperatures ranging from 35 to 55 °C. Extraction yield increased with extraction pressure and temperature, while fresh leaves yielded the highest extract, highlighting the importance of pretreatment on extractability. Chemical analysis revealed notable variations in monoterpene hydrocarbons, oxygenated monoterpenes, sesquiterpene hydrocarbons, and oxygenated sesquiterpenes depending on drying temperature and extraction parameters, confirming the high sensitivity of the volatile compound composition to processing conditions. Response surface methodology (RSM) was used to optimize process variables in order to enhance antimicrobial activity. The extracts inhibited both bacterial and fungal strains, confirming that the extraction conditions exert a direct influence on biological properties. The quadratic model identified the optimal combinations of drying and supercritical CO₂ extraction parameters, thereby providing a rational strategy to maximize the antimicrobial potency of P. lentiscus extracts. Overall, controlling pretreatment and supercritical extraction conditions allows for targeted modulation of chemical composition and bioactivity, thereby promoting the development of natural antimicrobial agents and valuable functional components. Full article

Reliable determination of macro- and micronutrients in cereal plant tissues is essential for agronomic management, environmental monitoring, and interlaboratory data comparability. However, most existing plant certified reference materials (CRMs) are derived from temperate-region matrices and do not adequately represent cereals cultivated under semi-arid conditions, where differences in mineral composition may lead to matrix-related analytical bias. In this study, a new multi-element plant reference material, Cereal Plant Powder 2023 (CPP-23), was developed from composite wheat (Triticum aestivum and T. durum) samples collected across major Moroccan agro-ecological zones. The material was processed, homogenized, and evaluated for homogeneity and stability in accordance with ISO 33405:2024, with no significant short- or long-term variability observed. Elemental characterization was performed using microwave-assisted acid digestion followed by ICP-OES for major and trace elements, while total nitrogen was determined using the Kjeldahl method. Method validation demonstrated satisfactory linearity (R² > 0.995), precision, and trueness against established reference materials. Certified values were assigned through an interlaboratory comparison involving eight ISO/IEC 17025-accredited laboratories using robust statistical estimators (ISO 13528:2022). Expanded uncertainties (k = 2) were below 15% for all analytes. While these results indicate acceptable internal consistency, the relatively limited number of participating laboratories and the absence of independent analytical validation techniques represent important constraints. CPP-23 provides a matrix-representative material suitable for quality control and method validation in semi-arid agricultural systems. Nevertheless, its ability to reduce analytical bias relative to existing CRMs and its applicability to specific use cases require further experimental validation. Full article

The evaluation of analytical methods has evolved beyond traditional validation parameters to encompass environmental sustainability, analytical reliability, and practical applicability. While numerous assessment tools exist for individual dimensions, integrated multicolor frameworks often impose rigid parameter selection, assign equal weights to all dimensions regardless of analytical context, or lack the granular diagnostic feedback necessary for method improvement. To address these limitations, we present the Triple-Color Assessment (TriCA) tool, a web-based platform that integrates three validated metrics into a unified scoring system with a hierarchical weighting scheme. TriCA combines the Analytical Green Star Area (AGSA) for greenness assessment, the Click Analytical Chemistry Index (CACI) for blueness evaluation, and the Analytical Method Reliability Index (AMRI) for redness scoring. While these metrics are provided as defaults, users may select alternative assessment tools within each dimension according to their specific preferences or requirements. TriCA features a user-customizable weighting system with recommended defaults (red = 3, blue = 2, green = 1), reflecting the logical priority that a method must first be valid, then practical, and finally green. Users can adjust these weights for specific contexts, while the underlying metric scoring protocols (AGSA, CACI, and AMRI) remain fixed to ensure reproducibility. Beyond composite scoring, TriCA generates three detailed pictograms, 12 segments for AGSA, eight segments for CACI, and 10 segments for AMRI, each color-coded to show performance at the individual criterion level. This diagnostic capability enables analysts to identify exactly which green chemistry principles, practicality criteria, or validation parameters are deficient, transforming assessment from an opaque scoring exercise into actionable guidance for method improvement. Seven case studies encompassing diverse analytical techniques demonstrate TriCA’s discriminative power and diagnostic utility. The tool is freely accessible at bit.ly/TriCA, offering the analytical community a transparent, reproducible, and diagnostically rich framework for method evaluation, development, and optimization. Full article

Urinary urea is a key biomarker for tracking protein oxidation and nitrogen balance. A persistent analytical limitation is that conventional total-nitrogen assays do not deconvolute urinary urea from urinary ammonia, and direct measurement still requires capital-intensive clinical analyzers. Here, we implement and independently validate two cost-effective methods that resolve urinary urea by pairing the presence and absence of urease: Method 1 is a urease-coupled potentiometric assay using an ammonium ion-selective electrode (ISE method); Method 2 is a microplate Berthelot–salicylate colorimetric assay employing a repurposed consumer-grade aquarium ammonia test kit (API^®) (API method). Each method was validated against the Roche Cobas C311 clinical analyzer (ISE for urinary ammonia and API for urinary urea) in healthy adult volunteers (n = 10 each), and API–ISE were then compared head-to-head for urinary urea. ISE vs. Cobas yielded R² = 0.967, slope 95% CI [0.867, 1.173], and Bland–Altman bias of −1.02 mM (95% LoA [−7.40, +5.36] mM). API vs. Cobas yielded R² = 0.973, slope 95% CI [0.790, 1.039], and bias of −1.55 mM (95% LoA [−11.56, +8.46] mM). API–ISE urinary urea comparison confirmed mutual agreement (R² = 0.9976, slope 95% CI [0.946, 1.024]; bias of +3.47 mM; 95% LoA [−14.60, +21.53] mM), with mean recoveries near 100% (API: 100.7 ± 2.9%; ISE: 100.6 ± 5.4%; 20–350 mM). Both methods agreed with the clinical analyzer, supporting their potential for decentralized, resource-limited testing; clinical and point-of-care validations are needed. Full article

Metabolomic aging clocks—quantitative models that estimate biological age based on small-molecule profiles in biological fluids—have become dynamic tools for assessing individual aging trajectories and predicting the risk of age-related diseases. Although NMR-based approaches have been previously reviewed, the analytical landscape of mass spectrometry (MS)-based metabolomic clocks has not been systematically assessed. This review examines the key components of the MS-based analytical workflow underlying the development of metabolomic aging clocks, including biological matrix selection, chromatographic separation strategies, MS instrumentation, data preprocessing, metabolite annotation, and machine learning-based modeling approaches. Twelve published studies on MS-based metabolomic clocks were identified and systematically compared. These clocks provide predictions of chronological age with mean absolute errors of 3.5–10 years and demonstrate robust associations between metabolomic age acceleration and cardiometabolic risk, frailty, and mortality. Recurrent age-related metabolite classes include tryptophan–kynurenine pathway metabolites, acylcarnitines, sphingolipids, modified nucleosides, and tricarboxylic acid (TCA) cycle intermediates. Currently, liquid chromatography with electrospray ionization (LC-ESI) coupled to high-resolution QTOF or Orbitrap instruments dominates current workflows, with elastic net regression being the most commonly applied modeling strategy. Significant heterogeneity in analytical conditions, incomplete methodological descriptions, and limited cross-study validation remain key obstacles to clinical application. Standardization of pre-analytical protocols, the use of certified reference materials, and harmonized validation frameworks are identified as critical priorities for advancing mass spectrometry-based metabolomic clocks toward clinical translation. Full article

Sulfated polysaccharides from red algae are multifunctional hydrocolloids whose properties depend strongly on molecular structure, sulfate content, and chain conformation. In this study, a sulfated galactan extracted from Gracilaria vermiculophylla collected from a coastal region of northwestern Mexico was investigated to elucidate its structural and functional properties. The polysaccharide was extracted by enzymatic treatment and characterized by monosaccharide analysis, FTIR, 1D/2D NMR spectroscopy, and size-exclusion chromatography coupled with multi-angle light scattering and viscometry. The extracted polysaccharide exhibited high carbohydrate (97%) and sulfate (28%) contents, with galactose as the predominant monosaccharide. It showed a moderate molecular weight (Mw = 2.39 × 10⁵ g/mol), a relatively narrow molar mass distribution (Mw/Mn = 1.23), a high intrinsic viscosity (420.9 mL/g), and an Rg/Rh ratio of 2.2, consistent with an expanded macromolecular conformation in solution. The sulfated polysaccharide also exhibited measurable antioxidant activity, particularly in the ABTS⁺ assay (IC₅₀ = 31.8 ± 2.5 mg/mL) compared with the DPPH assay (IC₅₀ = 51.1 ± 3.0 mg/mL), and showed Fe³⁺-responsive association, leading to the formation of microgel-like structures. These findings indicate that the sulfated galactan characterized in this study is a structurally complex and functionally active hydrocolloid with potential relevance for functional food systems and related biomaterial applications. Full article

Serum albumin binding plays a critical role in determining the pharmacokinetic and pharmacodynamic behavior of many drugs. Despite extensive studies on human and bovine serum albumin, quantitative binding data for rabbit serum albumin remain limited for several therapeutically important compounds. In this study, the binding interactions of three oxicam-class non-steroidal anti-inflammatory drugs (meloxicam, tenoxicam, and piroxicam) with rabbit serum albumin were investigated using circular dichroism spectroscopy and fluorescence quenching measurements. Binding parameters were estimated using nonlinear mixed-effects models that simultaneously incorporated data from multiple spectral channels and experimental replicates while accounting for residual correlation and heteroscedastic variance. Fluorescence-based analyses produced estimates consistent with the combined models and showed substantially lower uncertainty compared with CD-only analyses. These findings demonstrate that fluorescence quenching provides more reliable quantitative estimates of albumin binding affinity, whereas CD measurements exhibit higher variability in this context. The results represent the first systematic report of oxicams binding to rabbit serum albumin, with stability constants of meloxicam (logK = 4.840 ± 0.009), piroxicam (logK = 5.068 ± 0.007 and tenoxicam (logK = 4.668 ± 0.004) and highlight the importance of experimental determination of binding parameters even within closely related drug classes. The modeling framework employed here provides a robust statistical approach for analyzing spectroscopic titration data and may be broadly applicable to studies of drug–protein interactions. Full article

Synthetic azo dyes may be fraudulently added to paprika powder to intensify color, creating a need for rapid, at-line screening before confirmatory chromatographic analysis. This study evaluated handheld laser-induced breakdown spectroscopy (LIBS) for the screening of sodium-salt azo dye adulteration represented by Allura Red (E129), Ponceau 4R (E124), and Orange II in paprika powder. Paprika was spiked at 17 levels (0–6% w/w) in three independent batches, mixed with Al₂O₃ binder, dried, pelletized, and measured with a portable SciAps Z-903 under argon in the broad 190–950 nm region. The calibration models were developed using SNV-pretreated spectra and partial least squares regression with test-set validation based on a 70/30 split by concentration level. The main concentration-related response was increased Na emission, consistent with the sodium-salt form of the dyes, while Al emission showed an inverse matrix-/plasma-coupled trend despite the constant binder fraction. Full-spectrum models gave R²_TSV values of 0.845–0.875 and RMSETSV values of 0.638–0.716% (w/w), using 4–5 latent variables. Outlier trimming improved prediction for Allura Red and Orange II, while regression coefficient-uncertainty variable selection reduced model complexity to 2–3 latent variables with dye-dependent effects. Since sodium-salt azo dyes are commonly used as adulterants in paprika powder, the Na-dominated LIBS response demonstrates good potential for rapid at-line screening. Nevertheless, as LIBS does not directly confirm dye identity, complementary confirmatory analysis using spectroscopic or chromatographic methods remains necessary. Full article

Candida spp. can cause systemic infections with high mortality in immunocompromised patients. Phytotherapy may be an alternative for adjunctive treatment of fungal infections. This study evaluated the phytochemical profile, cytotoxicity, genotoxicity, and antibiofilm activity of the hydroalcoholic extract of Origanum vulgare L. against Candida albicans, Candida tropicalis, and Candida dubliniensis. The extraction and quantification (flavonoids and phenols) were performed, and its antioxidant activity (DPPH) and the presence of bio-active compounds were investigated using high-performance liquid chromatography with Diode Array Detection (HPLC-DAD). Cytotoxicity and genotoxicity tests were conducted using HaCat cell lines. Antifungal activity on planktonic cultures was evaluated using the standard (CLSI M27-S4). The analysis of the extract on biofilms was verified with different exposure times. The extract demonstrated the presence of bioactive molecules, and antioxidant activity. The cytotoxicity test showed viability >70%. Genotoxicity revealed the presence of a few micronuclei in some dilutions. The Minimum Fungicidal Concentration was obtained for C. albicans and C. tropicalis. In the biofilm analysis, there was a reduction of more than 60% in all Candida spp. species at the 24 h exposure time. The findings suggest that the O. vulgare extract exhibits activity against Candida spp. and shows biocompatibility in human keratinocytes. Full article

This study developed and validated a modified QuEChERS extraction procedure for the determination of 32 pesticide residues in tea (Camellia sinensis) found in Moroccan market originating from China and rosemary (Salvia rosmarinus) leaves using UPLC-MS/MS. A total of 202 pesticide residues were initially screened using the NF EN 15662 method, and 32 compounds showed satisfactory recovery and precision in tea. The optimized method, based on freezing before extraction and using PSA + BCG as purification sorbents, achieved recoveries of 70–120% for 97% of analytes. Calibration linearity ranged from 0.001 to 0.2 mg/kg (R² ≥ 0.980), with spiking levels at 0.01–0.1 mg/kg analyzed in duplicate per level and per matrix. Results of LOQ and LOD are compared to multiple MRL databases of Tea (EU, USA, Canada, Codex Alimentarius) despite the scarcity of tea MRLs in most databases, providing an accurate representation of the complexity of the analysis. Uncertainty was evaluated through both validation-based and Horwitz-based approaches, allowing a robust comparison of theoretical and experimental variability. The optimized method was also applied to rosemary, where 31 of the 32 pesticides validated in tea showed satisfactory performance. Similar recoveries, precision, and LOQs were obtained for both matrices, demonstrating the robustness of the method across chemically diverse herbal substrates. Only carbofuran exhibited reduced performance in rosemary, requiring an increased functional LOQ because of matrix-induced ion suppression. This dual-matrix approach provides a reliable and reproducible method for pesticide monitoring in herbal products. This dual-matrix approach provides a reliable and reproducible method for pesticide monitoring in herbal products. Full article

The utilisation of cosmetic plant waxes as sustainable functional ingredients in personal care formulations is on the rise. This is due to their emollient, structuring and film-forming properties. Nevertheless, the intricate lipid composition of these substances engenders considerable analytical difficulties, impeding the reliable characterisation and quality assessment thereof. In this study, an optimised gas chromatography–mass spectrometry (GC–MS) workflow was developed and evaluated for the compositional profiling of waxes derived from R. succedanea and R. verniciflua, two East Asian botanical species that have historically been utilised in cosmetic and lacquer-related applications. Wax samples originating from China, Vietnam, Korea, and Japan were extracted using solvents of different polarity, including petroleum ether, dichloromethane (DCM), ethyl acetate, and acetone. Following the process of BSTFA derivatisation, the extracts were subjected to analysis by GC–MS to evaluate the efficiency of the extraction process and the chemical composition of the extracts. DCM was found to provide the highest extraction yields and the most representative compositional profiles. Across all samples, palmitic acid was identified as the predominant constituent (80–90%), followed by lower amounts of oleic acid, stearic acid, and minor monoacylglycerols. The proposed analytical workflow exhibited satisfactory reproducibility and effective discrimination of lipid constituents, thereby substantiating its application in comparative compositional evaluation, potential support for future quality assessment studies, and formulation development of cosmetic plant waxes. Full article

This article describes the development of a compact and affordable variable-temperature NMR instrument designed primarily to measure dynamic molecular motion in solids and liquids. The instrument consists of Lab-Tools’ Mk4 palm-top time-domain NMR spectrometer fitted with a Peltier-cooled variable-temperature probe inside a shimmed Halbach magnet. Measurement of NMR relaxation times T₁, T₂, and ${\mathrm{T}}_1\rho$ is possible over the temperature range −20 °C to 70 °C with cooling and heating rates, and data acquisition is controlled from an integrated mini-PC. The overall footprint of the instrument is roughly that of a shoe box, making both in-the-field and bench-top measurements possible. Applications of this instrument include measuring pore-size distribution in porous rocks, the viscosity of oils and tars trapped in porous rock, the properties of polymers, and the viscosity of the liquid components of foods (e.g. fruits, vegetables and seeds). Results of test measurements for calibrated oils and olive oil are presented together with measurements of molecular mobility in a solid polymer. Full article