The online version contains supplementary material available at 10.1007/s13205-026-04833-9.

Static headspace (SHS) sampling, prior to a gas chromatography (GC) separation, is an interesting approach in food analysis inasmuch that the isolated volatile fraction reflects the compounds that reach the human nose. Additionally, the fraction analyzed is free of less volatile compounds and, hence, contamination of the GC system is avoided. Further, such a sample preparation method is environmentally-friendly because organic solvents are not used. The main disadvantage of SHS sampling is a reduced analyte detectability, due to the lack of a pre-concentration step. The investigation is based on the use of SHS sampling prior to cryogenic modulation enantioselective comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (CM eGC×GC-ToFMS). The samples subjected to analyses were two Citrus essential oils, namely bergamot and sweet orange. A chiral-apolar combination of columns was used, enabling both general analyte profiling and the determination of enantiomer ratios. A direct comparison was made between SHS and the direct injection (DI) of sample solutions. The use of CM counterbalanced, to a certain extent, the SHS reduced analyte detectability. A total of 239 and 84 compounds were tentatively characterized in bergamot essential oil using DI and SHS, respectively, whereas 174 and 58 analytes were tentatively identified in sweet orange essential oil using the same techniques, respectively. The method was further used to investigate the enantiomeric ratios of several chiral components. Both sampling methodologies yielded comparable chiral profiles, although slight variations in enantiomeric distributions were observed. The use of SHS sampling combined with CM GC×GC has been rarely described. The results obtained through SHS eGC×GC-ToFMS appear to be of interest and, in principle, such an option can be applied to food analysis in general. The untargeted information can be used to confirm authenticity and define geographical origin, along with the determination of products of transformation.

To evaluate the endodontic retreatment of S-shaped mesial root canals of mandibular molars using the Reciproc Blue R25 and R40 instruments, with or without the use of an orange oil solvent, and to assess the effect of additional apical enlargement with the HyFlex EDM 50/0.03 instrument on root canal cleaning after retreatment. Eighteen mesial root canals with double curvature from mandibular molars were prepared up to size 40/0.04 using HyFlex EDM instruments and obturated. Specimens were anatomically matched and allocated into two groups (n = 9) according to the retreatment protocol: Reciproc Blue R25 and R40 without solvent and Reciproc Blue R25 and R40 with orange oil solvent. Following filling removal, all canals underwent additional apical enlargement using the HyFlex EDM 50/0.03 instrument. Micro-computed tomographic scans were performed before and after obturation, after filling removal, and after apical enlargement. The percentage of remaining filling material, canal transportation, and centering ability were quantified by root canal thirds and in all root canal. Data were analysed using Student's t-test or Mann-Whitney U test for intergroup comparisons and paired Student's t-test or Wilcoxon signed-rank test for intragroup analyses (α = 0.05). No significant differences were observed between retreatment protocols, regardless of the use of orange oil solvent, for any evaluated parameter (p > 0.05). Additional apical enlargement with the HyFlex EDM 50/0.03 instrument significantly reduced the overall volume of remaining filling material in both groups (p < 0.05). However, complete removal of the filling material was not achieved in any specimen. Apical enlargement did not result in significant changes in canal transportation or centering ability (p < 0.05). The use of an orange oil solvent did not improve filling material removal or influence canal shaping in S-shaped mesial root canals of mandibular molars. Additional apical enlargement with the HyFlex EDM 50/0.03 instrument enhanced root canal cleanliness without compromising canal anatomy, although residual filling material persisted.

Sniffing the context: divergent effects of odor valence on intertemporal choice in loss vs. gain frames.

The protective influence of orange essential oil nano-emulsion on growth performance, antioxidant activity, immune status, inflammatory response, and hepato-renal function in heat-stressed growing rabbits.

Aphis gossypii (Glover 1877) remains a major constraint to cotton production worldwide, necessitating effective, resistance-conscious management strategies. This study systematically evaluated three emerging insecticide chemistries: flupyradifurone, flonicamid, and cyantraniliprole, both individually and in binary mixtures with a commercial orange oil formulation against adult A. gossypii. The evaluation integrated laboratory toxicity bioassays, biochemical enzyme profiling, computational (in silico) docking, and multiseason field validation. Probit analysis revealed pronounced differences in insecticidal potency, with LC50 values ranging from 0.095 mg L-1 for flupyradifurone to 2.210 mg L-1 for cyantraniliprole, and corresponding toxicity indices (TI) of 100 and 11.1, respectively, confirming flupyradifurone as the most active compound. Biochemical assays demonstrated treatment-specific modulation of major detoxification enzymes. Orange oil alone significantly induced esterase, glutathione S-transferase, cytochrome P450, and acetylcholinesterase activities at LC25, whereas most insecticides and their mixtures markedly suppressed esterase activity at LC50. Molecular docking analyses corroborated these findings, showing that cyantraniliprole exhibited the highest binding affinity toward the esterase active site (-6.6949 kcal mol-1), followed by flupyradifurone and flonicamid, while d-limonene displayed the weakest affinity (-4.3736 kcal mol-1), consistent with its limited direct enzymatic interaction. Critically, two-season field trials demonstrated consistently high aphid suppression (>90% population reduction) across all treatments, with no significant interannual variation, proving that laboratory-detected antagonism in mixtures did not compromise field efficacy. Collectively, these results demonstrate the robust field performance of emerging insecticide chemistries and support their strategic integration with botanical products as sustainable components of resistance-aware integrated pest management (IPM) programs targeting A. gossypii.

Propolis and plant-derived oils are currently being investigated as alternative sources against increasing antibiotic resistance. For this purpose, in this study, the antifungal activity of propolis ethanol extract and lemon oil, orange oil (obtained from 2 different producers), garlic oil, black grape seed oil, grape seed oil, pomegranate seed oil, black cumin oil, rosemary and thyme oils was evaluated against Candida albicans and Pichia manshurica and Candida albicans ATCC 10231 yeasts isolated from the human oral cavity. Antifungal activity was determined by the agar well diffusion method, and the results were statistically evaluated. Among the oils tested, rosemary and oregano oil exhibited the highest antifungal activity, forming inhibition zones ranging from 15.53 ± 3.28 to 39.25 ± 2.02 mm against the tested yeasts. No activity was detected in the other oils tested. Propolis was found to be as effective as amphotericin B antifungal (with inhibition zones between 16.31 ± 0.16 and 25.44 ± 1.34 mm), with inhibition zones ranging from 20.85 ± 0.95 to 25.95 ± 1.22 mm. In 1:1 mixtures of oils with propolis, antifungal activity increased compared to the oils used individually but decreased compared to propolis alone. Indeed, in mixtures of rosemary and oregano oils with propolis, inhibition zones ranged from 16.88 ± 2.75 to 34.06 ± 1.57 mm, with inhibition zones reduced compared to those observed with the oils used individually. Therefore, a potential antagonistic interaction was determined between the tested oils and propolis (P&amp;lt;0.001). In conclusion, while it might be assumed that combinations of natural substances strategically increase activity, this is not always the case. Therefore, it is necessary to investigate the effects of combining natural substances on biological activity.

Poly(ℇ-caprolactone)/gelatin nanofibers loaded with orange peel essential oils for wound healing: Upcycling of a food waste into a wound dressing material

Use of non-steroidal anti-inflammatory drugs may be associated with peptic ulcers. Asiatic acid, the active ingredient of Centella asiatica, is well-known for its antioxidant, anti-inflammatory, and wound-healing effects. Therefore, the aim of the study was to investigate the potential gastroprotective effects of asiatic acid dissolved in orange oil against indomethacin-induced peptic ulcer in rats. Rats were assigned to six groups as follows: Group 1: orally received the vehicle of asiatic acid (0.5% CMC-Na) followed by the vehicle of indomethacin (0.5% DMSO, i.p.); Group 2: gavaged with CMC-Na followed by indomethacin (25 mg/kg, i.p.); Group 3: given orange oil (10 mg/kg) before indomethacin; Group 4: received oral asiatic acid (10 mg/kg) prior to indomethacin; Group 5: received oral asiatic acid (10 mg/kg) in orange oil (10 mg/kg) prior to indomethacin. Group 6: administered oral omeprazole (30 mg/kg) prior to indomethacin. Indomethacin induced reduced secretion of mucin, decreased levels of prostaglandin E2 (PGE2) and cyclooxygenase 1 (COX-1), heightened oxidative stress, and elevated levels of the proinflammatory mediators. Pretreatment with asiatic acid in orange oil almost restored the normal macroscopic and microscopic features, increased mucin secretion, increased COX-1 and PGE2 levels, and reduced oxidative stress and inflammation. Also, asiatic acid in orange oil significantly restored the levels of transforming growth factor β1 (TGF-β1) in the gastric tissue of rats. Asiatic acid in orange oil shows significant protective effects against indomethacin-induced gastric ulcers in rats. It improves both macroscopic and microscopic gastric mucosal features while restoring TGF-β1 levels, promoting tissue repair and healing.

Multidrug-resistant (MDR) bacteria pose a threat to publichealthworldwide. In this context, disinfectants are used to prevent andcontrol the spread of these pathogens in hospital and industrial environments.The objective of this study was to determine minimum bactericidalconcentrations (MBC) for 10 traditional and innovative active ingredientsagainst 11 bacterial species. At the same time, the efficiency testwas applied in vitro and the effect on hospital surfaceswas analyzed in situ. The most promising compoundswere selected to determine their mechanism of action in the Gram-positivebacterium (Staphylococcus aureusMRSA)and the Gram-negative bacterium (Pseudomonas aeruginosaPA) by metabolomic analysis. Resistance to 50% of the activeingredients was observed in the five strains, and PA was resistantto 70% of them. Peracetic acid, chlorhexidine digluconate, and neemextract eliminated all strains within 1 min in MBC. In efficiencytests, traditional products killed bacteria, with an average reductionof 7.07 ± 0.331 log cycles. Neem extract achieved an averagereduction of 6.60 ± 0.33 log across all strains. In situ, peracetic acid did not allow bacterial growth, while biguanide,neem extract, tea tree oil, and orange oil achieved a reduction ofmore than 4 cycles of bacterial control on the surface. The exposureof MRSA and PA to the most promising compounds promoted distinct alterationsin intra- and extracellular metabolism, which were modulated by thebacterial cell wall structure. The study highlights the importanceof evaluating the practical efficacy of disinfectants, emphasizingthe diversity of approaches including natural compounds as alternativesin critical environments.

The rose stem girdler has been identified as the primary economic pest affecting oil-bearing rose plants. A mass attack can reduce the yield of rose flowers by up to 40%. The current study examines the effectiveness of three organic pesticides on the Agrilus cuprescens population. The field experiment was conducted in the village of Kliment, located in Bulgaria's Rose Valley, using a five-year-old organic rose plantation. The following products have been included in the investigation: Limocide® (60 g/L orange oil), NeemAzal® T/C (2.5% Neem substance), and a 4% bee glue solution applied individually and in the following combinations: Limocide® + 4% bee glue solution, and NeemAzal® T/C + 4% bee glue solution. These products were sprayed twice before flowering in an interval of 10 days and once in the postharvest period. The study was designed using a randomized block method with four replications, and each plot had a size of 18 m², containing 21 plants per variant. During the testing period, the combined treatment with Limocide® and propolis solution showed the highest effectiveness, managing to reduce the population of adult insects by up to 83%. When applied individually, Limocide® demonstrates 72% effectiveness against the pest, followed by the standalone application of propolis solution with an effectiveness of 64%. Moreover, the product Limocide® was able to reduce the formation of new galls by up to 92%. More research is needed to investigate the exact mechanism of action of orange oil and propolis extract at different stages of the enemy's development.

Feed additives have been used in high-concentrate diets to modulate ruminal fermentation; however, information on the metabolic effects of orange essential oil (OEO) under this dietary condition remains limited. The study aimed to evaluate the effects of increasing levels of orange essential oil as a source of D-limonene on nutrient intake, apparent digestibility, nitrogen balance, and ruminal fermentation characteristics in sheep fed high-concentrate diets, compared with sodium monensin. Ten rumen-cannulated Dorper × Santa Inês wethers were assigned to a 5 × 5 Latin square design and fed diets containing 90% concentrate. Treatments consisted of four OEO inclusion levels (0, 100, 500, and 1000 mg/kg dry matter [DM]) and sodium monensin (25 mg/kg DM; M25). Nutrient intake, apparent digestibility, nitrogen balance, ruminal pH, and short-chain fatty acid (SCFA) concentrations were evaluated. The OEO inclusion did not affect overall nutrient intake (P > 0.05). However, intake of dry matter, organic matter, crude protein, neutral detergent fiber, non-fiber carbohydrates (NFC), and total digestible nutrients was higher for OEO treatments compared with M25 (P < 0.05). Apparent digestibility of NFC decreased at the highest OEO level (1000 mg/kg DM; P < 0.05), although values remained higher than those observed with M25. Digestibility of other nutrients, nitrogen balance, ruminal pH, and SCFA profiles were not affected by OEO inclusion (P > 0.05). Under the conditions of this study, orange essential oil did not improve nutrient digestibility, nitrogen balance, or ruminal fermentation in sheep fed high-concentrate diets, although high inclusion levels negatively affected NFC digestibility. These results contribute to understanding the metabolic effects of limonene-rich essential oils as alternatives to ionophores in intensive feeding systems.

Enhancing essential oil extraction from orange peels using ultrasound-assisted hydro-distillation: A sustainable approach

Innovative active wrapping paper with spent coffee grounds and orange oil for delaying ripening and controlling anthracnose in mangoes stored at room temperature

Efficacy of orange oil as an alternative postharvest management strategy of <i>Botrytis cinerea</i> on plums and strawberries

Exposure to pesticides partly depends on the foraging behavior of bees, which may exhibit indifference, deterrence, or attraction to contaminated food. In the present study, we conducted laboratory experiments to test the foraging avoidance of Bombus terrestris for honey syrup contaminated with field-realistic concentrations of the neonicotinoid acetamiprid (ACE), herbicide glyphosate (GLY), and fungicide metalaxyl-M (MET). Tests were also conducted with the recommended field concentration of a biopesticide, the sweet orange essential oil (EOE). Bees’ behavior, and lethal and sublethal effects of the pesticides on bumble bees were assessed at the individual (isolated foragers) and colony (colony exposure) levels. Bees did not display any avoidance for contaminated or uncontaminated food at the individual or colony levels in the ACE, GLY, and MET treatments. However, the EOE treatment reduced the consumption of honey syrup in relation to non-treated bees, resulting in lower survival of individual bees. At the individual level, no behavioral differences were observed between non-treated and treated bees. At the colony level, however, pesticide treatments modified bees’ walking behavior. In general, pesticides increased resting time and meandering, while reducing speed, movement, distance walked, and time spent moving fast. Our results demonstrate that bumble bees did not reduce food consumption of syrup contaminated with realistic concentrations of different common pesticides, resulting in detrimental effects on their behavior. Furthermore, bumble bees treated with the biopesticide field concentration reduced food consumption both at individual and colony levels. This treatment caused negative behavioral changes on bees and decreased the survival of isolated individuals.

The growing demand for environmentally benign lubricants has intensified research into bio-based alternatives derived from non-edible and underutilized oil resources. In this study, oils extracted from Strychnos spinosa (monkey orange), Jatropha curcas, and Lagenaria sphaerica (wild calabash) sourced from Taraba State, Nigeria, were investigated as potential feedstocks for high-performance bio-lubricant production. Crude oils were obtained via Soxhlet extraction, characterized for physicochemical properties, and subsequently subjected to acid-catalyzed esterification followed by base-catalyzed transesterification to produce lubricant-grade ester base stocks. The modified oils were formulated into neat bio-lubricants and further enhanced with zinc oxide (ZnO) nanoparticles to obtain nano-lubricant formulations. Chemical modification markedly reduced acid values to below 1 mg KOH g⁻¹ and improved kinematic viscosity and viscosity index, indicating enhanced rheological stability. Tribological evaluation revealed significant reductions in coefficient of friction and wear scar diameter upon ZnO incorporation, accompanied by substantial improvements in extreme-pressure performance. Thermal analysis (TGA/DSC) demonstrated increased onset degradation temperatures and higher residual mass for ZnO-enhanced formulations, confirming improved thermal stability. Among the investigated feedstocks, wild calabash and monkey orange oils exhibited superior responses to nano-enhancement. Overall, the results demonstrate that chemically modified, ZnO-reinforced bio-lubricants derived from underutilized non-edible seed oils can achieve tribological and thermal performance comparable to conventional synthetic lubricants, offering a sustainable and environmentally friendly alternative for industrial lubrication applications.

Topical cream loaded with upcycled citrus bioactive chitosan-pectin nanoparticle protects skin from UV-induced photoaging.

Solvent-free chemoenzymatic epoxidation of raw orange essential oil: Process development and evaluation of antimicrobial and antiviral activities

Objective: To evaluate and compare the dissolution effectiveness of three organic solvents-xylene, tetrachloroethylene, and refined orange oil-on four root canal sealers: AH Plus, AVUE A+, Endoseal, and Bio-C.Methodology: The solubility of AH Plus (Dentsply Sirona), Avue A+ (Calcium Hydroxide Based Root Canal Sealer, Dental Avenue India Pvt. Ltd. ss), Endoseal (Zinc Oxide Eugenol Based Root Canal Sealer, Prevest Denpro), Bio-C Sealer (Angelus Bio-C Sealer, Bioceramic Root Canal Sealer) was assessed in xylene (Merck PVT LTD), tetrachloroethylene (Qualikems PVT LTD), refined orange oil, and distilled water.A total of forty-eight samples of root canal sealers were prepared and divided into four equal groups, each corresponding to one of the selected solvents.Several commercially available root canal sealers exhibit unique physicochemical properties.The selected samples (n = 12) were immersed separately in each solvent for 10 minutes at room temperature.The means of weight loss were determined for each material in each solvent pre-and post-immersion.Data were analyzed using one-way ANOVA and Tukey post-hoc test.Results: Bio-C Sealer exhibited significantly distinct solubility across all tested solvents.It differed from all other sealers in Xylene and Orange Oil.In Tetrachloroethylene, Bio-C, Avue A+, and ZnOE varied significantly, while AH Plus did not.Conclusion: Dissolution efficacy is both sealer and solvent-specific: Xylene works best on epoxy-resin-based sealers, while tetrachloroethylene is superior for calcium-silicate-based sealers.Refined orange oil, a biocompatible alternative, showed intermediate effectiveness.