Background Lepidium sativum (LS) seeds, which are renowned for their abundance of bioactive compounds, have been used to regulate blood glucose levels. The present study was conducted to evaluate the effect of LS seed fixed oil on the protection of pancreatic β-cells, inhibition of α-glucosidase, and mitochondrial protection. Materials and methods The fixed oil was extracted from LS seeds using n-hexane, and its composition was characterized. The α-glucosidase inhibitory activity was assessed using standard enzyme inhibition assays. In vitro experiments were performed using NIT-1 cells to evaluate the protective effects of LS-fixed oils on mitochondrial depolarization and early stress induced by diabetogenic agents. Results LS-fixed oil contains high levels of triacylglycerols, saturated fatty acids, and sterols, such as β-sitosterol, campesterol, and stigmasterol. LS-fixed oil exhibited a strong α-glucosidase inhibitory effect (IC₅₀ = 9.375µg/mL). LS-fixed oil protected against mitochondrial depolarization and enhanced mitochondrial membrane potential (ΔΨm). It also alleviated early stress markers in β-cells induced by streptozotocin (STZ) and Carbonyl Cyanide m-Chlorophenyl Hydrazone (CCCP) in vitro and improved insulin secretion. Conclusion LS seed fixed oil has significant antidiabetic potential and acts through multiple mechanisms. These findings suggest that lipophilic compounds in LS seeds may play a key role in protecting pancreatic β-cells and offer a promising therapeutic agent for diabetes management.
This review examines natural plant resins, wood tars and pitches in heritage science, focusing on their historical uses, chemical composition and analytical characterisation. Particular attention is given to diterpenoid and triterpenoid resins and to chemical transformations induced by ageing, degradation and thermal processing. The identification of diagnostic molecular markers supports the determination of botanical origins and technological practices, while an overview of complementary analytical methods highlights current challenges and perspectives.
The volatile organic compound (VOC) content of a total of 88 extra virgin olive oil (EVOO) samples was investigated over two consecutive years in two cooperative mills. The oils were analysed by solid phase microextraction gas chromatography coupled with mass spectrometry (SPME-GC/MS) identifying 82 VOCs. PLS-DA models enabled good clustering emphasizing the importance of seasonality in the VOC profile. Many VOCs seem to keep the same behaviour between the two years independently from the mill. When both the year and the mill were used as response variables the model explained only 50% of the variance within the dataset. Therefore, the weight of the multifactorial “season” variable seems to be higher than the multifactorial variable “milling”. Some VOCs showed correlations with the fruit temperature before milling as well as with the health status of the olives. Valencene appeared to be positively correlated with the acidity of the oil samples. Therefore, the elevated valencene levels observed in some of the samples may be linked to the health status of the olives before milling. (E)-3-hexenyl acetate could be used as a distinctive marker of the oils produced with the autochthonous Tuscan cultivar Olivastra di Seggiano.
This study explores the geographical distribution and molecular composition of adhesive substances employed by Neolithic communities in north-central Italy. By applying advanced mass spectrometric techniques—specifically Pyrolysis-Gas Chromatography/Mass Spectrometry (Py-GC/MS) and Gas Chromatography/Mass Spectrometry (GC/MS)—we chemically characterized organic residues recovered from flint blades and complete and fragmentary wooden sickles, across multiple archaeological sites. The dual analytical approach proved especially effective in detecting and identifying molecular markers in samples where the preserved adhesive was present only in trace amounts, thus overcoming limitations imposed by minimal sample volumes and potential contamination. Our comprehensive analysis revealed a diverse portfolio of adhesive materials, notably birch bark tar, Pinaceae resin, and bitumen. The coexistence of these substances within the same chronological framework suggests a complex technological and procurement strategy among Neolithic groups. Local resources, such as pine resins, were likely exploited alongside non-local materials, implying the existence of well-established exchange networks and adaptive responses to regional environmental conditions. By coupling archaeological investigation with molecular characterization, this research demonstrates that even minimally preserved organic residues can yield significant compositional data, thereby contributing to a more nuanced reconstruction of prehistoric technological networks and socio-economic interactions.
Multidisciplinary micro- and bioarchaeological analyses of late medieval deposits from suburban Cártama, Málaga, Spain, have, for the first time, confidently identified open air fumier deposits, which are supported by preliminary analysis of the faunal assemblage. This demonstrates that Andalusi livestock husbandry practices included periodically burning animal dung within corrals and pens, which is a long-standing practice in the Mediterranean region also observed in prehistoric transhumance. These techniques have commonly been applied to prehistoric fumier or pastoral sites and now demonstrate the importance of expanding micro- and bioarchaeological work to fumier sequences from other periods. This research from Cártama offers a window into the so-called medieval “Green Revolution” associated with Arab migrations and highlights the necessity of identifying in situ penning deposits on archaeological sites and of applying high resolution analyses to examine them. The analyses reveal data on animal feeds, including pearl millet (Pennisetum glaucum) and sorghum (Sorghum bicolor) which are rare in the Iberian Peninsula at this time, the use of plant resources in livestock husbandry, and the preparation of fertiliser, which are central to understanding farming practices in Al-Andalus.
Two methods based on double-shot analytical pyrolysis-GC/MS (DSPy-GC/MS) and evolved gas analysis-MS (EGA-MS) were developed to quantify polyethylene (PE) in biodegradable plastics (BPs). BPs are widely used to produce short-lived goods such as shopping bags, packaging, and disposable tools. Small amounts of non-biodegradable plastics, namely PE, are added to BP formulations to reduce costs and improve processability. Current European regulations allow for a maximum 1% PE content by weight in biodegradable plastics, but no information is provided on how this content should be measured. The methods presented here were developed using a set of reference samples composed of common BP formulations with known added amounts of PE. The methods were tested for linearity, accuracy, matrix effect, and limits of detection and quantification. In the EGA-MS method, a new strategy based on mid-run split switch was developed, resulting in a significant increase of the signal of PE. Both methods proved capable of quantifying PE in concentrations of 1% or lower and showed negligible matrix interference. The EGA-MS method is faster, while the DSPy-GC/MS method provides lower limits of quantification. The results indicate that both methods could be used for routine quality control and conformity analysis of BPs. This is the first work describing quantification of PE in BPs using analytical pyrolysis-based techniques. The use of EGA-MS for quantitative analysis, and the use of mid-run split switch, are also presented in this paper for the first time.
Transforming industrial by-products into new resources is a fundamental principle of sustainable agriculture and circular bioeconomy. Waste products from rosemary (Rosmarinus officinalis L.) essential oil extraction, such as exhausted biomass and water residues (WRs), are rich in bioactive compounds like phenols and terpenes. These by-products may represent a promising and economically viable option for agricultural management, particularly in weed control. This study evaluates the potential use of WR as a bioherbicide. In vitro experiments were conducted to assess the inhibitory effects of WR on the germination and seedling morphology (root and shoot development) of four detrimental weed species for temperate cropping systems: two monocotyledonous (Alopecurus myosuroides and Lolium multiflorum) and two dicotyledonous (Sinapis alba and Amaranthus retroflexus). WR was tested at four concentrations (0, 25, 50, and 100), corresponding to an increasing gradient of WR, with 100 representing pure WR. The results showed that WR did not significantly inhibit germination in A. myosuroides, L. multiflorum and S. alba, whereas A. retroflexus exhibited a dose-dependent inhibition, with germination reduced by 37.5%, 64.5%, and 91.6% at doses of 25, 50, and 100, respectively, compared with the control (dose 0). Furthermore, germination delays were observed across all tested species with promising application of WR for regulating weed–crop competitive interactions in the early crop growth stages. Results on the morphological traits of weed seedlings showed that WR application affected root more than shoot growth inhibition. In particular, WR demonstrated a pronounced root inhibitory effect in A. myosuroides, L. multiflorum, and A. retroflexus. In contrast, a dose-dependent increase in root length was observed for S. alba (21.41 mm at dose 0 and 25.77 mm, 30.97 mm and 35.96 mm, respectively, at doses 25, 50, and 100). The results of this study highlight the potential application of WR as a sustainable solution to be included in an integrated weed management (IWM) toolbox and underscore their role in promoting the valorization of waste from essential oil production.
Olfactory cultures shape how societies perceive, value, and use scents in daily life, ritual, and social practice, embedding specific smells within collective identity. Mobility exposes these cultures to new environments, where scents may act as markers of heritage and belonging for migrants while also prompting diverse reactions—ranging from appreciation to disruption—within host or newly established communities. The Iron Age Mediterranean, marked by intense cultural encounters, offers key insights into how fragrances contributed to an increasingly interconnected world, with the Phoenicians playing a central role in disseminating Near Eastern aromatic practices westward. Despite the frequent association between the Phoenicians and scented substances, the contents of vessels traditionally assumed to have held unguents remain largely unknown. This study presents the first systematic, interdisciplinary analysis of the composition, technology, and contents of over fifty “Phoenician oil bottles” from the island of Motya, off the west coast of Sicily, Italy. This assemblage represents a significant sample of these plain-ware, slow-pouring juglets that circulated throughout and beyond the Mediterranean. The results suggest that aromatic unguents were likely produced and bottled in southern Phoenicia during the eighth–sixth centuries BCE and circulated to the western Mediterranean. While focused in scope, this evidence contributes to broader discussions of Phoenician involvement in the production, trade, and consumption of fragrant substances. The study also highlights the potential for such vessels to inform future research into the sensory, social, and cultural dimensions of mobility and interaction in the ancient Mediterranean.
Rhamnus alaternus L. (Rhamnaceae) is a medicinal plant traditionally used for treating a range of inflammatory diseases. This study aimed to characterize the methanolic extract of Rhamnus alaternus L. stem bark (MRAB) using LC-MS and to investigate its in vitro antioxidant activity as well as its in vivo analgesic, anti-inflammatory, and wound-healing effects. Thirteen compounds were identified, including 7 glycosylated flavonoids, two non-glycosylated flavonoids, two phenolic acids and two chromones. The IC50 of MRAB for DPPH and ABTS radical scavenging activity were 58.31 ± 3.07 μg/mL and 22.33 ± 0.35 μg/mL, respectively. MRAB also demonstrated a high total antioxidant capacity and reducing power (242.8 ± 17.96 mg Asc E/g extract and 143.74 ± 1.18 mg Asc E/g extract, respectively). The MRAB showed notable analgesic and anti-inflammatory effects. In the acetic acid-induced abdominal writhing test, MRAB at 500 mg/kg exhibited a significant reduction in writhing (66.19 %), comparable to diclofenac (76.66 %). The extract also showed potent analgesic effects in the formalin test, with a 79.54 % inhibition in the inflammatory phase, similar to salicylic acid (84.9 %). MRAB exhibited strong anti-inflammatory activity in both the carrageenan-induced hind paw edema test (58.74 % and 66.73 % inhibition at 250 and 500 mg/kg, respectively) and the xylene-induced ear edema test (49.72 % and 59.81 % inhibition). Furthermore, MRAB indicated significant wound-healing effects, with retraction percentages of 89.56 ± 0.93 % and 93.45 ± 0.83 % at 250 and 500 mg/kg, respectively, comparable to the Cicatryl group (95.91 ± 0.62 %) on day 12. These findings highlight the therapeutic potential applications of MRAB for analgesic, anti-inflammatory, and wound-healing treatments.
The National Museum of Transylvanian History in Cluj-Napoca, Romania, features a History of Pharmacy Collection that documents the evolution of pharmacies in the region since the 16th century. Within the “Pharmatrans” project (2021–2023), we investigated the chemical composition of ointments from fourteen historical pharmaceutical containers dating back to the 18th and 19th centuries. Most samples were from an aristocratic traveling medicine chest, a key artifact in the collection. This study marks the first extensive analysis of historical pharmaceutical formulations in Romania, enhancing our understanding of these valuable items. The main ingredients of formulations were characterized using gas chromatography–mass spectrometry (GC–MS), solid-phase microextraction–GC–MS (SPME–GC–MS), and pyrolysis–GC–MS (Py–GC–MS). Additionally, high-performance liquid chromatography coupled with high-resolution mass spectrometry (HPLC-ESI-Q-ToF) was employed for the detailed analysis of lipid materials and polar compounds. Elemental analysis was conducted using field emission gun–scanning electron microscope (FEG–SEM) with energy-dispersive spectroscopy (EDS). The results revealed that twelve out of fourteen mixtures contained interpretable organic content, often aligning with the vessels’ labels. The findings indicate that Transylvanian elites in the late 18th century had access to both rare drugs and traditional remedies, reflecting contemporary trends in pharmacy.
This study describes the development of a laboratory-scale extraction method for polyphenols in vine pruning residues (VPR) using eutectic solvents and microwave heating. Grape VPR are an abundant waste biomass that is currently underexploited. VPR are rich in valuable extractives such as polyphenols, and their extraction with green and sustainable processes could constitute a promising valorization strategy. Microwave-assisted heating was used to obtain high extraction yields under relatively mild conditions. The performances of three eutectic solvents based on choline chloride and polyols (ethylene glycol, propylene glycol, and glycerol) were compared against a conventional water/ethanol solvent. These solvents were particularly effective at extracting stilbenoid polyphenols such as resveratrol, whose low water solubility usually requires high amounts of organic solvents. The solvent based on choline chloride and ethylene glycol provided the best results, and was chosen for further optimization by experimental design. Optimal performances were obtained under mild conditions (30 min, 85 degrees C). The effects of controlled amounts of water on the extraction efficiency of this solvent were also evaluated. Small amounts of water (approximately 10 %) led to an increase in the extraction yield, while higher water contents led to lower yields. Total polyphenol yields of up to 22 mg/g of substrate were obtained. The mild extraction conditions also allowed recovery of oligomeric stilbenoids such as epsilon-viniferin, which are often degraded when harsh conditions or water-based solvents are used. The developed method constitutes a fast and reliable technique for the recovery of polyphenols in VPR, and a promising laboratory-scale study of a potential valorization pathway for this biomass.
The aim of this paper is to characterize materials belonging to one of the masks coming from the Lord of Ucupe's tomb in the region of Lambayeque in Peru. The mask belongs to the Moche culture which lived in the north of Peru since 100 CE. Along with the study of the extraordinary metal alloy technique using X-ray fluorescence (ED XRF) integrated with the Monte Carlo simulation, this paper investigates the blackish material used as an adhesive for its inlaid eyes. This material was analysed through the ATR FT-IR and characterized through Py-GC/MS and GC/MS for the organic components and SEM-EDS for the inorganic components. The chemical characterization of the adhesive material coming from this type of artefact, based on our knowledge of current literature, is the first on this material and allows us to take a further step into the understanding of the constituents used for this purpose. (c) 2023 Consiglio Nazionale delle Ricerche (CNR). Published by Elsevier Masson SAS. All rights reserved.
Bioplastics are produced in growing amounts due to their environmental benefits, but their disposal routes remain ambiguous. A hydrothermal treatment (HT) may be a sustainable process to improve the fate of waste bioplastics, but nearly no information is available on how they respond to it. In this work, HT of biodegradable bioplastics was performed, and the resulting solid and liquid products were characterized by elemental analysis, analytical pyrolysis-based techniques, ion chromatography, and gas chromatography coupled with mass spectrometry. We selected tableware based on polylactic acid (PLA), cellulose, and Mater-Bi (MB) and performed HT at 160-200 degrees C. MB was identified as a mixture of PLA and polybutylene succinate (PBS). Higher treatment temperatures enhanced the solubilization, which was very marked for PLA and MB and minor for cellulose. Characterization of the solid residues revealed that PLA and MB were quantitatively degraded at 180 degrees C and above, while cellulose could never be fully degraded. The analysis of the aqueous phases from the HT of PLA and MB revealed the presence of an array of oligomers of PLA and PBS at low temperatures and of the corresponding monomers (lactic acid and succinic acid) at high temperatures: their recovery could represent a way to give new life to waste bioplastics.
An array of analytical techniques (GC–MS, SPME–GC–MS, RP–HPLC–MS, FIA–MS, HPLC–UV, ICP–MS) was used to study the molecular composition of six ointment residues from the first third of the twentieth century. The objectives of the study were (i) to validate the applicability of a previously proposed strategy for the identification of lipids and active pharmaceutical ingredients in remains of historical pharmaceuticals and (ii) to shed light on early twentieth-century pharmaceutical practice. Although no further information on the composition of the samples studied was available (all were marked by a period pharmacist with the general label “Ointment” only), it was possible to identify the likely lipidic ointment bases as well as quantify the main likely active substances in all samples. This allowed us to partially reconstruct the composition of each ointment and to estimate its original purpose.
Alkyl levulinates (ALs) are strategic compounds for the development of sustainable energy transition. In this regard, the direct alcoholysis of fructose and inulin for the selective ethyl levulinate (EL) production was investigated with a One-Factor-At-a-Time (OFAT) approach employing diluted H2SO4 as catalyst to clarify the role of the main reaction parameters (substrate and acid loadings, temperature, reaction time). The OFAT investigation on fructose ethanolysis allowed to reach the EL yield of 91.5 mol%. The inulin ethanolysis was then optimized adopting the multivariate approach based on the Response Surface Methodology (RSM), which highlighted the interplay of the reaction parameters on the selective EL production. This allowed to identify the optimal conditions to reach the highest EL yield (up to 89.3 mol%) and also those which ensured the highest EL concentration, adopting a substrate loading (14 wt%) higher than the majority ones reported in the literature according to the high gravity approach, and the lowest diethyl ether (DEE) by-product yield. The DEE formation is scarcely investigated in the literature, but it can negatively influence the alcoholysis process, thus it was considered in this work. Moreover, the humin solid residue was deeply characterized to envisage its possible applications, under a circular economy perspective. One-Factor-At-a-Time (OFAT) approach and the multivariate approach were adopted for the optimization of fructose and inulin one-pot ethanolysis, respectively, allowing to systematically elucidate the role of key reaction parameters (temperature, H2SO4 and inulin loadings, reaction time) and aiming at the maximisation of EL yield and concentration while minimising the formation of by-products, such as diethyl ether and solid char. image
The COST EU-PoTaRCh Action establishes a network focused on the past, present, and future significance, production, and use of major forest by-products in Europe and beyond. The Action centers around forest by-products-primarily potash, tar, resin, and charcoal (PoTaRCh), along with plant extracts-which have been produced and utilized for over 100,000 years due to their unique chemical, biological, and therapeutic properties. The primary goal of the Action is to demonstrate the importance of these products for the socio-economic development of European countries and beyond, as well as their impact on biodiversity and the natural environment. The Action's objectives are organized into five Working Groups (WGs), each aligned with specific areas of interest: heritage, chemical characterization, archaeology, environmental history, and future perspectives of PoTaRCh materials. A key aspect of the Action is its support for stakeholders outside the scientific community who possess knowledge of PoTaRCh products through their use in industries such as production, education, and the promotion of forests' natural and cultural heritage. In doing so, the Action brings together stakeholders with diverse activity profiles, including museums, state forests, the forestry industry, associations dedicated to preserving traditions, and the tourism sector. The EU-PoTaRCh Action adheres to the three key principles of COST's inclusiveness policy: participation of inclusiveness target countries, gender balance, and the involvement of young researchers, including in leadership positions.
The dynamics of our species’ dispersal into the Pacific remains intensely debated. The authors present archaeological investigations in the Raja Ampat Islands, north-west of New Guinea, that provide the earliest known evidence for humans arriving in the Pacific more than 55 000–50 000 years ago. Seafaring simulations demonstrate that a northern equatorial route into New Guinea via the Raja Ampat Islands was a viable dispersal corridor to Sahul at this time. Analysis of faunal remains and a resin artefact further indicates that exploitation of both rainforest and marine resources, rather than a purely maritime specialisation, was important for the adaptive success of Pacific peoples.