Sample Preparation from Plant Tissue for Gas Chromatography-Mass Spectrometry (GC-MS)we.

Metabolites are intermediate products formed during metabolism. Metabolites play different roles, including providing energy, supporting structure, transmitting signals, catalyzing reactions, enhancing defense, and interacting with other species. Plant metabolomics research aims to detect precisely all metabolites found within tissues of plants through GC-MS. This chapter primarily focuses on extracting metabolites using chemicals such as methanol, chloroform, ribitol, MSTFA, and TMCS. The metabolic analysis method is frequently used according to the specific kind of sample or matrix being investigated and the analysis objective. Chromatography (LC, GC, and CE) with mass spectrometry and NMR spectroscopy is used in modern metabolomics to analyze metabolites from plant samples. The most frequently used method for metabolites analysis is the GC-MS. It is a powerful technique that combines gas chromatography's separation capabilities with mass spectrometry, offering detailed information, including structural identification of each metabolite. This chapter contains an easy-to-follow guide to extract plant-based metabolites. The current protocol provides all the information needed for extracting metabolites from a plant, precautions, and troubleshooting.

Limited exposure of captive Australian marsupials to plastics.

The global concern regarding the ubiquitous presence of plastics in the environment has led to intensified research on the impact of these materials on wildlife. In the Australian context, marsupials represent a unique and diverse group of mammals, yet little is known about their exposures to plastics. This study aimed to assess the contamination levels of seven common plastics (i.e., polystyrene (PS), polycarbonate (PC), poly-(methyl methacrylate) (PMMA), polypropylene (PP), polyethylene terephthalate (PET), polyethylene (PE), and polyvinyl chloride (PVC)) in both the diet and faeces of kangaroos, wallabies and koalas sampled from a sanctuary in Northeastern Australia. Quantitative analysis was performed by pressurized liquid extraction followed by double-shot microfurnace pyrolysis coupled to gas chromatography mass spectrometry. Interestingly, the analysis of the food and faeces samples revealed the absence of detectable plastic particles; with this preliminary finding suggesting a relatively limited exposure of captive Australian marsupials to plastics. This study contributes valuable insights into the current state of plastic contamination in Australian marsupials, shedding light on the limited exposures and potential risks, and highlighting the need for continued monitoring and conservation efforts. The results underscore the importance of proactive measures to mitigate plastic pollution and protect vulnerable wildlife populations in Australia's unique ecosystems.

Investigation on the insecticidal activities of cyanobacterial extracts as an alternative source for the management of fall armyworm, Spodoptera frugiperda (J. E. Smith) (Lepidoptera: Noctuidae).

The Spodoptera frugiperda is a notorious pest with a broad host range. It severely damages crops, mainly in areas of the globewhere maize and sorghum are grown. The pest is difficult to control due to its adaptive nature and resistance to several insecticides available in the market. So, an identification of the alternative strategy is the prime important in the present context. Insecticidal activities of cyanobacterial extracts were evaluated in the laboratory as a biocomponent against S. frugiperda. The crude extracts of Nostoc muscorum and Spirulina sp. were prepared by using ethanol, methanol and petroleum ether solvents. Soxhlet apparatus was used for extraction. S. frugiperda larvae in their second instar were given access to fragments of maize leaf that had been treated with various cyanobacterial extracts. The findings displayed that the petroleum ether extract of N. muscorum had the lowest LC50 value of 155.22 ppm, followed by petroleum ether extracts of Spirulina, ethanol extract of N. Muscorum, methanol extract of N. muscorum, ethanol and methanol extract of Spirulina with an LC50 values of 456.02, 710, 780, 1050 and 1070 ppm respectively. Later, the effect of LC50 values on many biological parameters like the larval duration and pupal stages, the percentage of pupation, the weight of the pupal stage, the malformation of the pupal and adult stages, adult emergence percentage, fertility and the longevity of the male and female adult stages of S. frugiperda was examined. The gas chromatography-mass spectrometry (GC-MS) was used to analyse the crude extract to identify the bioactive components that were responsible for the insecticidal properties. The major compounds detected were diethyl phthalate (19.87 %), tetradecane (5.03%), hexadecanoic acid, ethyl ester (4.10 %), dodecane (4.03%), octadecane (3.72%), octadecanoic acid, methyl ester (3.40 %), ethyl oleate (3.11 %), methyl ester. octadecenoic acid (3.04 %), heptadecane (3.04 %) and phytol (3.02 %). The presence of several bioactive chemicals in the cyanobacterial extracts may be the reason for their insecticidal actions, thus it can be used as an alternative and new source to combat fall armyworm and other crop pests.

Investigation of volatile profiles and odor-active compounds in Osmanthus fragrans var. aurantiacus separated by different polarities using GC/MS, GC-olfactometry and electronic-nose system.

This research investigated volatiles and odor active compounds in Osmanthus fragrans var. aurantiacus. Heterocyclics were mainly extracted from hexane and dichloromethane extracts. Ketones were mainly detected from butanol fraction, and alcohols were mainly extracted from the ethanol fraction. GC-O analysis investigated the contents and intensities of three major odor active compounds increasing by ramping up polarity Multivariate analysis, which includes principal component analysis (PCA) and hierarchical cluster analysis (HCA), by E-nose data showed 45.83% (PC1) and 29.27 (PC2) variances, respectively, and segregated two clusters. Multivariate analysis by GC-O data showed 65.64% (PC1) and 24.17% (PC2) variances, respectively, and segregated the three clusters, cluster I by ethanol extract, cluster II by dichloromethane extract, and cluster III by hexane and butanol extracts. This study demonstrates that different polarity solvents can collect various volatiles and odor active compound groups. Our findings can support basic research data as a natural and functional food additive.

Phytochemical composition of Lagenaria siceraria fruits from KwaZulu-Natal and Limpopo, South Africa.

Lagenaria siceraria (Molina) Standley is a food and medicinal source with anti-proliferative, anti-fertility, anti-HIV and anti-cancerous properties. The current study investigated the phytochemical constituents of L. siceraria fruits using gas chromatography/mass spectrometry (GC-MS). Five isoprenoids present in all investigated landraces were 1-Dodecene, 2,3-Dimethyldodecane, E-15-Heptadecenal, Eicosane, and Tridecane, 6-propyl. Lighter metabolites such as 1-Dodecene and 2,3-Dimethyldodecane were recorded at a shorter retention time range of 9.08-16.29 min over a lower relative peak area ranging from 1.09 to 6.97%. However, heavier compounds (E-15-Heptadecenal, Eicosane and Tridecane, 6-propyl) had a longer retention time range of 13.42-18.00 mins over a higher relative peak area range of 2.25-11.41%. Cluster analysis grouped landraces into 5 clusters (I -V) according to their fruit and seed attributes, and isoprenoid units significant to each cluster. Terpenoids were the prominent phytochemicals present in fruits. This is the most comprehensive study on the fruit phytochemical constituents of different L. siceraria landraces to date.

Dimethylformamide dimethyl acetal reagent for in situ chiral analyses of organic molecules on Titan with the Dragonfly mass spectrometer space instrument (Dragonfly mission).

Thanks to the Cassini-Huygens space mission between 2004 and 2017, a lot was learned about Titan, the biggest satellite of Saturn, and its intriguing atmosphere, surface, and organic chemistry complexity. However, key questions about the potential for the atmosphere and surface chemistry to produce organic molecules of direct interest for prebiotic chemistry and life did not find an answer. Due to Titan potential as a habitable world, NASA selected the Dragonfly space mission to be launched in 2027 to Titan's surface and explore the Shangri-La surface region for minimum 3 years. One of the main goals of this mission will be to understand the past and actual abundant prebiotic chemistry on Titan, especially using the Dragonfly Mass Spectrometer (DraMS). Two recently used sample pre-treatments for Gas Chromatography - Mass Spectrometry (GC-MS mode of DraMS) analyses are planned prior analysis to extract refractory organic molecules of interest for prebiotic chemistry and astrobiology. The dimethylformamide dimethylacetal (DMF-DMA) derivatization reaction offers undoubtedly an opportunity to detect biosignatures by volatilizing refractory biological or prebiotic molecules and conserving the chiral carbons' conformation while an enantiomeric excess indicates a chemical feature induced primarily by life (and may be aided on the primitive systems by light polarization). The goal of this study is to investigate the ageing of DMF-DMA in DraMS (and likely MOMA) capsules prior to in situ analysis on Titan (or Mars). The main results highlighted by our work on DMF-DMA are first its satisfactory stability for space requirements through time (no significant degradation over a year of storage and less than 30 % of lost under thermal stress) to a wide range of temperature (0 °C to 250 °C), or the presence of water and oxidants during the derivatization reaction (between 0 and 10 % of DMF-DMA degradation). Moreover, this reagent derivatized very well amines and carboxylic acids in high or trace amounts (ppt to hundreds of ppm), conserving their molecular conformation during the heat at 145 °C for 3 min (0 to 4% in the enantiomeric form change).

LDHB contributes to the regulation of lactate levels and basal insulin secretion in human pancreatic ß cells.

Using 13C6 glucose labeling coupled to gas chromatography-mass spectrometry and 2D 1H-13C heteronuclear single quantum coherence NMR spectroscopy, we have obtained a comparative high-resolution map of glucose fate underpinning ß cell function. In both mouse and human islets, the contribution of glucose to the tricarboxylic acid (TCA) cycle is similar. Pyruvate fueling of the TCA cycle is primarily mediated by the activity of pyruvate dehydrogenase, with lower flux through pyruvate carboxylase. While the conversion of pyruvate to lactate by lactate dehydrogenase (LDH) can be detected in islets of both species, lactate accumulation is 6-fold higher in human islets. Human islets express LDH, with low-moderate LDHA expression and ß cell-specific LDHB expression. LDHB inhibition amplifies LDHA-dependent lactate generation in mouse and human ß cells and increases basal insulin release. Lastly, cis-instrument Mendelian randomization shows that low LDHB expression levels correlate with elevated fasting insulin in humans. Thus, LDHB limits lactate generation in ß cells to maintain appropriate insulin release.

Measuring aliphatic hydrocarbons in sediments by direct thermal desorption-gas chromatography-mass spectrometry: Matrix effects and quantification challenges.

Direct sample introduction thermal desorption (TD) coupled to GC-MS was investigated for the analysis of paraffinic hydrocarbons (HCs) from polluted sediments. TD-GC-MS is sometimes used for analysing paraffinic HCs from atmospheric particles but rarely for their direct desorption from sediments. So, the new TD methodology, applied to sediments, required development, optimization and validation. A definitive screening experimental design was performed to discriminate the critical factors on TD efficiency, from model sediments containing various organic matter (OM) amounts. Low molecular weight HCs had extraction behaviours markedly different from high molecular ones (HMW-HCs), but a compromise was found using very few sediment amount (5 mg), high temperature rate (55 °C min-1) and final temperature (350 °C). Linear HCs (n-C10 to n-C40) could be quantified using the matrix-matched calibration method, with very low detection limits (3.8-13.4 ng). The amount of the overall paraffinic alkanes was also determined as a sum of unresolved components between predefined equivalent carbon ranges. The developed solventless methodology was compared to an optimized solvent microwave assisted extraction (MAE). Matrix effects could be higher for TD compared to MAE but it depended on sediment matrix. When matrix effect was strong, particularly on HMW-HCs signal depletion, a dilution with pure non-porous sand was favourable for accurate quantification. The sum of resolved and unresolved HCs gave comparable results between MAE and TD extractions, with an exception of alkanes greater than C30 which were less quantitatively extracted via TD. However, TD-GC-MS was more sensitive than MAE-GC-MS. So TD-GC-MS is useful for analyzing sediments containing a great range of paraffinic HCs (C9-C34) and it has the advantages of being fully automated, with few sample preparation and operator intervention, using very low amounts of solvent, and generating few wastes.

Antibacterial Activity of Oregano (Origanum vulgare L.) Essential Oil Vapors against Microbial Contaminants of Food-Contact Surfaces.

The antimicrobial effect of eight essential oils' vapors against pathogens and spoilage bacteria was assayed. Oreganum vulgare L. essential oil (OVO) showed a broad antibacterial effect, with Minimum Inhibitory Concentration (MIC) values ranging from 94 to 754 µg cm-3 air, depending on the bacterial species. Then, gaseous OVO was used for the treatment of stainless steel, polypropylene, and glass surfaces contaminated with four bacterial pathogens at 6-7 log cfu coupon-1. No viable cells were found after OVO treatment on all food-contact surfaces contaminated with all pathogens, with the exception of Sta. aureus DSM 799 on the glass surface. The antimicrobial activity of OVO after the addition of beef extract as a soiling agent reduced the Sta. aureus DSM 799 viable cell count by more than 5 log cfu coupon-1 on polypropylene and glass, while no viable cells were found in the case of stainless steel. HS-GC-MS analysis of the headspace of the boxes used for the antibacterial assay revealed 14 different volatile compounds with α-Pinene (62-63%), and p-Cymene (21%) as the main terpenes. In conclusion, gaseous OVO could be used for the microbial decontamination of food-contact surfaces, although its efficacy needs to be evaluated since it depends on several parameters such as target microorganisms, food-contact material, temperature, time of contact, and relative humidity.

Antibacterial Activity of Defensive Secretions from the Lace Bug Stephanitis svensoni (Drake) (Hemiptera: Tingidae).

Nymphs of Stephanitis svensoni (Drake) (Hemiptera: Tingidae) have numerous glandular setae on their dorsal abdomens. Chemical analysis of the exudates from these setae revealed the presence of 11 compounds, including aliphatic aldehydes, aliphatic ketones, and aromatic polyketides. Among them, 3-oxododecanal, 5-hydroxy-2-heptylchromanone, and 5-hydroxy-2-undecanylchromanone were identified for the first time in the family Tingidae. Previous research has suggested that secretions from nymphs of the genus Stephanitis, belonging to the family Tingidae, function as defensive substances against predators. The exudates of S. svensoni showed antibacterial activity against the Gram-positive bacterium Staphylococcus aureus. Antibacterial tests conducted using preparations of the 10 identified compounds showed antibacterial activity in 3-oxododecanal, 2,6-dihydroxyacetophenone, and 1-(2,6-dihydroxyphenyl)dodecan-1-one. In addition, antibacterial tests against the Gram-negative bacterium Escherichia coli showed activity in 2,6-dihydroxyacetophenone and 1-(2,6-dihydroxyphenyl)dodecan-1-one. Therefore, 2,6-dihydroxyacetophenone and 1-(2,6-dihydroxyphenyl)dodecan-1-one exhibited a wide antibacterial spectrum. Particularly, 1-(2,6-dihydroxyphenyl)dodecan-1-one, which showed antibacterial activity even at low concentrations, holds promise as lead drug compound.

Gastric Fluid Metabolomics Predicting the Need for Surfactant Replacement Therapy in Very Preterm Infants Results of a Case-Control Study.

Respiratory distress syndrome (RDS) is a major morbidity of prematurity. In this case-control study, we prospectively evaluated whether untargeted metabolomic analysis (gas chromatography-mass spectrometry) of the gastric fluid could predict the need for surfactant in very preterm neonates. 43 infants with RDS necessitating surfactant (cases) were compared with 30 infants who were not treated with surfactant (controls). Perinatal-neonatal characteristics were recorded. Significant differences in gastric fluid metabolites (L-proline, L-glycine, L-threonine, acetyl-L-serine) were observed between groups, but none could solely predict surfactant administration with high accuracy. Univariate analysis revealed significant predictors of surfactant administration involving gastric fluid metabolites (L-glycine, acetyl-L-serine) and clinical parameters (gestational age, Apgar scores, intubation in the delivery room). Multivariable models were constructed for significant clinical variables as well as for the combination of clinical variables and gastric fluid metabolites. The AUC value of the first model was 0.69 (95% CI 0.57-0.81) and of the second, 0.76 (95% CI 0.64-0.86), in which acetyl-L-serine and intubation in the delivery room were found to be significant predictors of surfactant therapy. This investigation adds to the current knowledge of biomarkers in preterm neonates with RDS, but further research is required to assess the predictive value of gastric fluid metabolomics in this field.

Comprehensive Two-Dimensional Gas Chromatography-Mass Spectrometry as a Tool for the Untargeted Study of Hop and Their Metabolites.

Since hop secondary metabolites have a direct correlation with the quality of beer and other hop-based beverages, and the volatile fraction of hop has a complex composition, requiring effective separation, here we explore the application of headspace solid-phase microextraction as a sample preparation method, coupled with comprehensive two-dimensional gas chromatography-mass spectrometry (GC×GC-MS) analysis. The methodology involved the use of a DVB/PDMS fibre with 500 mg of hop cone powder, extracted for 40 min at 50 °C, for both GC-MS and GC×GC-MS. The varieties Azacca, Cascade, Enigma, Loral, and Zappa were studied comprehensively. The results demonstrate that GC×GC-MS increases the number of peaks by over 300% compared to classical GC-MS. Overall, 137 compounds were identified or tentatively identified and categorised into 10 classes, representing between 87.6% and 96.9% of the total peak area. The composition revealed the highest concentration of sesquiterpene hydrocarbons for Enigma, whilst Zappa showed a relatively significant concentration of monoterpene hydrocarbons. Principal component analysis for all compounds and classes, along with hierarchical cluster analysis, indicated similarities between Zappa and Cascade, and Azacca and Loral. In conclusion, this method presents an optimistic advancement in hop metabolite studies with a simple and established sample preparation procedure in combination with an effective separation technique.

Monitoring and Risk Assessment of Pesticide Residues in Fishery Products Using GC-MS/MS in South Korea.

The aim of this study was to assess the risk of pesticide contamination in aquaculture and its impact on fishery products. We conducted an assessment of 300 samples collected from nine regions in South Korea, including various types of seafood, such as freshwater fish, marine fish, crustaceans, and shellfish. Pesticide residues in seafood were analyzed using GC-MS/MS after sample preparation using a modified QuEChERS method, revealing the presence of eight pesticides (4,4'-DDE, 4,4'-DDT, boscalid, isoprothiolane, oxadiazon, pendimethalin, thifluzamide, and trifluralin) across seven fish species (carp, far eastern catfish, crucian carp, eel, Chinese muddy loach, mirror carp, and sea bass). Following the grouping of DDE with DDT, a risk assessment of fishery products was conducted. After the estimated daily intake (EDI) of fish was calculated and compared with the acceptable daily intake (ADI), the health risk index (HI, %ADI) of the detected pesticides was evaluated and found to be 1.07% or lower. The results suggest that the consumption of domestically farmed fish products in South Korea poses minimal health risks associated with pesticide residues.

Integrated untargeted and targeted testicular metabolomics to reveal the regulated mechanism of Gushudan on the hypothalamic-pituitary-gonadal axis of kidney-yang-deficiency-syndrome rats.

Modern studies have shown that neuroendocrine disorders caused by the dysfunction of the hypothalamic-pituitary-gonadal (HPG) axis are one of the important pathogenetic mechanisms of kidney-yang-deficiency-syndrome (KYDS). The preventive effect of Gushudan on KYDS has been reported, but its regulatory mechanisms on the HPG axis have not been elucidated. In this study, we developed an integrated untargeted and targeted metabolomics analysis strategy to investigate the regulatory mechanism of Gushudan on the HPG axis in rats with KYDS. In untargeted metabolomics, we screened 14 potential biomarkers such as glycine, lysine, and glycerol that were significantly associated with the HPG axis. To explore the effect of changes in the levels of potential biomarkers on KYDS, all of them were quantified in targeted metabolomics. With the quantitative results, correlations between potential biomarkers and testosterone, a functional indicator of the HPG axis, were explored. The results showed that oxidative stress, inflammatory response, and energy depletion, induced by metabolic disorders in rats, were responsible for the decrease in testosterone levels. Gushudan improves metabolic disorders and restores testosterone levels, thus restoring HPG axis dysfunction. This finding elucidates the special metabolic characteristics of KYDS and the therapeutic mechanism of Gushudan from a new perspective.

Isolation and characterization of bioactive alkaloids and GC-MS based identification of volatile oil metabolites from fruits of Glycosmis pentaphylla and evaluation of their cytotoxic activity.

Glycosmis pentaphylla, a member of the Rutaceae family, has been extensively studied for its pharmacological activities, focusing mainly on the cytotoxic properties of its roots and stems. Conversely, limited researched has been done in terms of the phytochemical composition of the fruits. The objective of this study is to isolate and identify the bioactive compounds found in the fruits of G. pentaphylla and then evaluate their potential for anti-cancer activity in oral cancer CAL 27 cell lines. The extraction of bioactive compounds from fruits was done by maceration, and the isolation of alkaloids and volatile oil fractions (F1-F5) was performed by column chromatography. The alkaloids, such as 3-O-methoxyglycocitrine II, noracronycine, 1-hydroxy-3-methoxy-10-methyl-9-acridone and kokusaginine, were first isolated from the fruits of G. pentaphylla. Additionally, GC-MS analysis identified 78 metabolites. The isolated compounds and identified volatile oil fractions were explored for their anti-cancer activity by cell viability assay. Results demonstrated that isolated compounds were found inactive, while the volatile fraction F1 was found active in CAL 27 cell line. Fraction F1 impeded wound healing in CAL 27 cells by scratch assay, and significantly inhibited colony formation in colony formation assay. In cell cycle analysis, treatment with fraction F1 redistributed cells to the S and G2 phases of the cell cycle. α-elemol (2) is the major metabolite identified from the F1 fraction by GC-MS, which could be responsible for the anti-cancer activity. There is potential for future work to further isolate volatile oil metabolites and evaluate their anti-cancer activity through in-vivo techniques.

Multiple-matrix metabolomics analysis for the distinct detection of colorectal cancer and adenoma.

OBJECTIVES: Although colorectal cancer (CRC) is the leading cause of cancer-related morbidity and mortality, current diagnostic tests for early-stage CRC and colorectal adenoma (CRA) are suboptimal. Therefore, there is an urgent need to explore less invasive screening procedures for CRC and CRA diagnosis. METHODS: Untargeted gas chromatography-mass spectrometry (GC-MS) metabolic profiling approach was applied to identify candidate metabolites. We performed metabolomics profiling on plasma samples from 412 subjects including 200 CRC patients, 160 CRA patients and 52 normal controls (NC). Among these patients, 45 CRC patients, 152 CRA patients and 50 normal controls had their fecal samples tested simultaneously. RESULTS: Differential metabolites were screened in the adenoma-carcinoma sequence. Three diagnostic models were further developed to identify cancer group, cancer stage, and cancer microsatellite status using those significant metabolites. The three-metabolite-only classifiers used to distinguish the cancer group always keeps the area under the receiver operating characteristic curve (AUC) greater than 0.7. The AUC performance of the classifiers applied to discriminate CRC stage is generally greater than 0.8, and the classifiers used to distinguish microsatellite status of CRC is greater than 0.9. CONCLUSION: This finding highlights potential early-driver metabolites in CRA and early-stage CRC. We also find potential metabolic markers for discriminating the microsatellite state of CRC. Our study and diagnostic model have potential applications for non-invasive CRC and CRA detection.

Foraging animal origin food samples as passive indicators of dioxin-like POPs contamination in industry sites: Method development, characterisation and risk assessment.

Titanium dioxide (TiO2) is an important industrial chemical, and studies suggest its major production route - the chloride process could lead to the generation of unintentional dl-POPs. However, no relevant studies assessed the occurrence of dl-POPs associated with TiO2 production in the industrial zones, which is mostly due to the ultra-trace level distribution of these compounds in environmental compartments. The present study explored the novel possibility of utilising foraging animal-origin foods as sensitive indicators for addressing this challenge and generated a globally beneficial dataset by assessing the background levels of dl-POPs in the vicinity of a TiO2 production house in Southern India. Systematic sampling of foraging cow's milk and free-ranging hen's eggs was carried out from the study site, and the dl-POPs assessments were conducted utilising an in-house developed cost-effective GC-MS/MS-based analytical methodology. The median dl-POPs levels in milk and egg samples were about 3 times higher than the control samples collected from farm-fed animals and retail markets. The contaminant loads in the foraging animal-origin food samples were further traced to their presence in environmental compartments of soil and sediment and admissible degree of correlations were observed in congener fingerprints. Elevated health risks were inferred for the population in the industrial zones with weekly intakes weighing about 0.15 to 17 times the European Food Safety Authority-assigned levels. The consumption of foraging cow's milk was observed to have a higher contribution towards the hazard indices and cancer risk estimates and were significantly higher (p < 0.05) for children. The study also presents a critical validation of the GC-MS/MS-based method for the purpose of regulatory monitoring of dl-POPs, which could be of practical significance in economies in transition.

Phytochemical potential and GC-MS analysis of propolis from Punjab region of India.

Propolis is a beehive product produced from honeybees by mixing ß-glycosidase enzyme and beeswax with exudate collected from plant resins. The main goal of this study was to investigate the phytochemical potential and GC-MS profiling of the main constituents of propolis. The antioxidant activity was assessed by using 2,2-diphenyl-1-picrylhydrazyl (DPPH) free radical scavenging assay, total phenolic content and total flavonoid content were analysed by Folin-Ciocalteu reagent method and aluminium chloride method respectively. Methanolic extract exhibited highest antioxidant activities, ethanolic extract had the highest total phenolic content, and maximum amount of flavonoid was observed in the chloroform extract. GC-MS analysis revealed the presence of flavonoids, fatty acids and phenolic compounds. Results revealed that propolis from Derra Bassi can be used as natural antioxidant, also extracting solvents had a significant impact on the phytochemical activities and with its standardisation can be used for prevention of diseases related with free radicals.

Sensory Impact of Novel Dihydrocoumarins in Native Lime Oils.

Citrus fruits have been known and valued for their aroma in food and perfume ever since humans have maintained written records. Often described as the "champagne" of citrus oils, especially cold pressed lime peel oils have raised attention. Particularly peel oils of Citrus latifolia exhibit a pleasant coumarinic, sweet, and balsamic aroma in comparison to its close relative, the Citrus aurantifolia. Those coumarinic notes have not been completely understood until today. Thus, this study aimed to identify the responsible substances and elucidate their contribution and impact on the aroma of cold-pressed lime oil. By combining distillation, fractionation, olfactory detection, and structure elucidation, the responsible key aroma components were identified. A combination of coumarins and their corresponding saturated analogs have been identified to significantly contribute to the typical coumarinic-like aroma, including three new flavor compounds that have not yet been described in the literature as lime oil constituents: 7-methoxy-2-chromanone (3,4-dihydro-7-methoxy-2H-1-benzopyran-2-one; CAS 20921-02-2), 5,7-dimethoxy-2-chromanone (3,4-dihydro-5,7-dimethoxy-2H-1-benzopyran-2-one; CAS 82243-01-4) and 5,6-dihydrobergaptene (5,6-dihydro-4-methoxy-7H-furo[3,2-g][1]benzopyran-7-one; CAS 29050-61-1). The sensorial evaluation of the impact of these components on the lime aroma profile has shown flavor-modulating effects and the ability to enhance aldehydic-peely, juicy, and fruity notes as well as their importance in reproducing the authentic, typical coumarin-like notes.

Characterization of industrial TNT in ammunition shells: An in-depth study of artificial aging effects using Fourier-Transform infrared spectroscopy and gas chromatography-mass spectrometry.

In this study, we comprehensively investigated the degradation of industrial trinitrotoluene (TNT), focusing on the effects of aging and direct contact with steel surfaces, mirroring real-world usage conditions. While practical knowledge exists regarding this degradation, the existing literature lacks in-depth insights into the underlying processes. To address this gap, we conducted experiments using small steel samples, representative of military ammunition casings, which were coated with TNT and subjected to 30 days of heating at 75 °C under vacuum conditions. A subset of these samples was coated with a protective red alkyd paint. After the aging process, the TNT was carefully removed from the metal surfaces and subjected to a comprehensive analysis encompassing scanning electron microscopy, Fourier-transform infrared spectroscopy, and gas chromatography-mass spectrometry. Our results reveal a remarkable preservation of the chemical integrity of industrial TNT, even in the presence of thermal stress and direct steel contact. Although superficial changes were observed in the TNT's appearance, all analytical data consistently demonstrated the maintenance of its chemical composition. Notably, the sole change in composition was attributed to the presence of degradation products associated with the alkyd paint coating, rather than intrinsic TNT degradation. These findings underscore the negligible impact of degradation processes on TNT in scenarios involving the solid-phase thermal stress of TNT in direct contact with metal, significantly enhancing our understanding of TNT safety when packaged within steel artifacts-a common context in military ammunition.