Gas Chromatography Coupled To Mass Spectrometry Research Articles

Anticancer and antiproliferative activities of Algerian Origanum majorana L.’s essential oil on PC-3 and SKBR3 cells

Cancer is a prominent cause of death globally, with breast cancer and prostate cancer being among the most devastating types. Therefore, the available anticancer treatments have some drawbacks, like higher toxicity and limited bioavailability. Thus, this study aimed to investigate for the first time the anticancer activity of Algerian Origanum majorana L.’s essential oil (OMEO). This research assessed the chemical profile of Algerian OMEO by gas chromatography coupled with mass spectrometry (GC-MS). The analysis revealed 29 compounds, which represent 98.08% of total volatile oil. The major compounds identified in OMEO were terpinen-4-ol (21.37%), γ-terpinene (15.78%), α-terpinene (10.43%), and trans-sabinene hydrate (9.27%). Additionally, MTT (3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyl tetrazolium bromide) was also used to test the cytotoxicity on prostate cancer (PC-3), breast cancer (SKBR3), and normal retinal pigment epithelium (ARPE-19) cell lines. The results showed a selective cytotoxicity effect by decreasing cell viability of PC-3 cancer cells with half inhibitory concentration (IC50) of 608.57 μg/mL and 672.5 μg/mL after 48h and 72h, respectively. Regarding SKBR3 cancer cells, the IC50 was 991.5 μg/mL. OMEO exhibited no significant cytotoxicity against normal (ARPE-19) cells. Furthermore, we conducted a cell apoptosis assay using Hochest 33342 dye to explore the potential mechanism pathway of OMEO. The findings verified that OMEO could trigger apoptosis in PC-3 and SBKR3 cancer cells. The ability of OMEO to inhibit cell migration assessed via wound healing assay revealed a significant decrease in cell migration. Our results imply that OMEO decreases cell viability by inducing cell apoptosis. Moreover, the oil suppresses cell migration in prostate cancer and breast cancer cells.

Pharmacognostic Standardization and Chemical Study of Euphorbia nutans Lag. Euphorbiaceae

Aims: This study was designed to set macro/micro morphological standards, phytochemical and physicochemical parameters for the identification of E. nutans, a traditional remedy for the management of many disesases. Study Design: To establish pharmacognostic standards for proper identification of E. nutans and also study its phytochemicals using Gas Chromatography coupled to Mass Spectrometry (GC-MS). Place and Duration: This work was undertaken at the Department of Pharmacognosy and Natural Medicine, Faculty of Pharmacy, University of Uyo, Uyo, Nigeria for three month spanning from April through June, 2022. Methodology: Examination of microscopic characters, venation, chemomicroscopy, micromeritic properties, fluorescence analysis and phytochemical profiling using Gas Chromatography-Mass Spectrometry (GC-MS) were carried out. Results: Epidermal cell shapes were irregular with undulate-sinuous anticlinal walls. Stomatal distribution was amphistomatic with anisocytic and anomocytic stomata on both surfaces. Areolation was quadrangular, linear and biforked vein termination. The fluorescence characteristics showed the presence of different colours supporting the presence of various phytoconstituents for both leaf and stem. The flow properties for both leaf and stem were poor while GC-MS analysis of the dichloromethane extracts revealed lupeol (64.05%), 2-methylhexacosane (9.37%), stigmasterol (4.16%) and campesterol (1.29%) as major components in the leaf while campesterol (0.67%), stigmasterol (2.15 %), beta.-sitosterol (6.22%), lupeol (9.85%) and vitamin E (1.05%) for the stem extract. Conclusion: The results of the study could be useful for correct identification, standardization and preparation of monograph.

Salivary Metabolic Pathway Alterations in Brazilian E-Cigarette Users.

In recent years, the use of electronic cigarettes (e-cigs) has increased. However, their long-term effects on oral health and saliva remain poorly understood. Therefore, this study aimed to evaluate the saliva of e-cig users and investigate possible biomarkers. Participants were divided into two groups: the Electronic Cigarette Group (EG)-25 regular and exclusive e-cig users-and Control Group (CG)-25 non-smokers and non-e-cig users, matched in sex and age to the EG. The clinical analysis included the following parameters: age, sex, heart rate, oximetry, capillary blood glucose, carbon monoxide (CO) concentration in exhaled air, and alcohol use disorder identification test (AUDIT). Qualitative and quantitative analyses of saliva included sialometry, viscosity, pH, and cotinine concentrations. Furthermore, the EG and CG salivary metabolomes were compared using gas chromatography coupled with mass spectrometry (GC-MS). Data were analyzed using the Mann-Whitney test. The MetaboAnalyst 6.0 software was used for statistical analysis and biomarker evaluation. The EG showed high means for exhaled CO concentration and AUDIT but lower means for oximetry and salivary viscosity. Furthermore, 10 metabolites (isoleucine, 2-hydroxyglutaric acid, 3-phenyl-lactic acid, linoleic acid, 3-hydroxybutyric acid, 1,6-anhydroglucose, glucuronic acid, valine, stearic acid, and elaidic acid) were abundant in EG but absent in CG. It was concluded that e-cig users had high rates of alcohol consumption and experienced significant impacts on their general health, including increased cotinine and CO concentration in exhaled air, decreased oximetry, and low salivary viscosity. Furthermore, they showed a notable increase in salivary metabolites, especially those related to inflammation, xenobiotic metabolism, and biomass-burning pathways.

Improvement of Properties of Bio-Oil from Biomass Pyrolysis in Auger Reactor Coupled to Fluidized Catalytic Bed Reactor

The goal of this research work was to investigate the improvement of bio-oil issued from beechwood biomass through catalytic de-oxygenation. Pyrolysis was conducted in an auger reactor and the catalytic treatment was performed in a fluidized catalytic bed reactor. Lab-synthesized Fe-HZSM-5 catalysts with different iron concentrations were tested. BET specific surface area, BJH pore size distribution, and FT-IR technologies were used to characterize the catalysts. Thermogravimetric analysis was used to measure the amount of coke deposited on the catalysts after use. Gas chromatography coupled to mass spectrometry (GC-MS), flame ionization detection (GC-FID), and thermal conductivity detection (GC-TCD) were used to identify and quantify the liquid and gaseous products. The pyrolysis temperature proved to be the most influential factor on the final products. It was observed that a pyrolysis temperature of 500 °C, vapor residence time of 18 s, and solid residence time of 2 min resulted in a maximum bio-oil yield of 53 wt%. A high percentage of oxygenated compounds, such as phenolic compounds, guaiacols, and the carboxylic acid group, was present in this bio-oil. Catalytic treatment with the Fe-HZSM-5 catalysts promoted gas production at the expense of the bio-oil yield, however, the composition of the bio-oil was strongly modified. These properties of the treated bio-oil changed as a function of the Fe loading on the catalyst, with 5%Fe-HZSM-5 giving the best performance. A higher iron loading of 5%Fe-HZSM-5 could have a negative impact on the catalyst performance due to increased coke formation.

Chemical Composition, Antibacterial and Antibiotic-Modifying Activity of Croton grewioides Baill Essential Oil

Background: Croton grewioides Baill., a species native to the Caatinga, popularly known as canela de cunhã, is used in traditional medicine to treat gastrointestinal diseases such as diarrhea, gastritis and stomach ulcers. The combination of essential oils with antibiotics reveals several beneficial effects associated with the increased efficacy of these drugs against pathogenic agents. Through this perspective, this study aimed to identify the chemical composition of the essential oil of C. grewioides (OECG) and evaluate its antibacterial and antibiotic-modifying activities against standard and multiresistant bacteria. Methods: To analyze the compounds present in the oil, the techniques of gas chromatography coupled with mass spectrometry (GC/MS) and gas chromatography with a flame ionization detector (GC/FID) were used. In the bacteriological tests, the Minimum Inhibitory Concentration (MIC) was obtained by the broth microdilution technique. The modulating effect of the essential oil was determined by calculating the subinhibitory concentration, followed by a serial microdilution of the antibiotics. The MIC reduction factor (CRF) was calculated, and its data were expressed as a percentage. Results: The analysis of the chemical composition identified the presence of the major compound estragole with a relative abundance of 50.34%. The MIC values obtained demonstrated efficacy in K. pneumoniae isolated from urine with MIC values of 512 µg/mL. OECG potentiated the effects of all antibiotics tested on the strains S. aureus ATCC 29213, K. pneumoniae Carbapnemase, E. coli ATCC 25922 and S. aureus ATCC 29213 with their CRF of 97.65%, 99.80%, 99.85% and 99.88%, respectively. Conclusions: Thus, the essential oil of C. grewioides presents synergistic effects when combined with the antibiotics tested, in addition to acting in the fight against bacterial resistance to antibiotics.

GC/MS Screening of Substances Released from Post-Consumer Recycled HDPE Pellets into 95% Ethanol: Reproducibility and Variation between Production Batches

The use of post-consumer recycled (PCR) plastic materials in sensitive packaging applications, such as for cosmetic products and detergents, requires a clear understanding of the identities and quantities of chemical substances, which they may release into packed products. With many potential sources of and thus different types of potentially releasable substances, a reliable non-targeted screening method is required to assess these materials. Such a method should be readily applicable in industrial practice and provide a realistic estimation of substance release. This investigation focused on the use of gas chromatography/coupled mass spectrometry (GC/MS) to analyze substances, which recycled HDPE (rHDPE) plastic pellets release into 95% ethanol under accelerated testing conditions. The results of the repeated testing of reference samples clearly demonstrated the good reproducibility of the described methodology, with standard deviations of repeated determinations of the total released substance amounts of 6.8–8.1%. The application to several production batches of three commercial rHDPE grades additionally demonstrated that the batch-to-batch variation of substances which rHDPE materials release can be confined to less than 10% of variation of the total detectable substance amount. The described methodology is therefore seen as a pragmatic, repeatable assessment of recycled HDPE plastic batches with a view to substance release.

Exploring the antimicrobial efficacy of tea tree essential oil and chitosan against oral pathogens to overcome antimicrobial resistance

BackgroundConsidering that antimicrobial resistance among oral pathogens is a significant concern in dental practice, with broader implications for overall health due to the oral microbiota serving as a reservoir for antibiotic resistance genes (ARGs), research into natural products is crucial for addressing this issue. ObjectiveThis study aimed to evaluate tea tree oil (TTO) and chitosan (CH) performance against oral pathogens, including mixed-species biofilm, and its effects on bacteria growth, in addition to chemical characterization and cytotoxicity of TTO. MethodsTea Tree Oil and low molecular weight chitosan were used in this study. The chemical composition of TTO was analyzed using gas chromatography coupled with mass spectrometry (GC-MS). To evaluate TTO's antimicrobial properties, time-kill and cell viability assays were conducted. Additionally, minimum inhibitory concentration (MIC), minimum microbiocidal concentration (MMC), checkerboard, and biofilm assays were performed using TTO and CH alone and in combination. ResultsTTO chromatography peaks found consistent with the standard ISO4730:2017 and literature. TTO and CH exhibited inhibitory activity against all tested microorganisms. The predominantly microbiostatic activity of TTO is probably related to terpinen-4-ol associated with terpinene. The oil at MIC value was able to delay the log phase of Aggregatibacter actinomycetemcomitans growth. Fibroblasts (L929) viability remained above 70 % during 24 h for TTO concentrations ranging from 0.5 to 0.0625 mg/ml. TTO-CH combination showed a synergistic activity (FIC = 0.5) against A. actinomycetemcomitans and Streptococcus sanguinis, at a concentration of 0,25MIC for both species. The compounds at MIC concentration inhibited both monospecies and mixed-species biofilms studied bacteria to the same extent as the azithromycin control. ConclusionTTO and CH demonstrated efficacy in combating oral pathogens and TTO-CH combination offers a promising approach to confront microbial resistance in the oral environment.

In vitro antibacterial activity of essential oils from Cymbopogon flexuosus and Cymbopogon winterianus

The objective of the study was to identify and quantify chemical compounds present in the essential oils of C. flexuosus and C. winterianus and evaluate their antibacterial action on Escherichia coli, Pseudomonas aeruginosa and Staphylococcus aureus. This is an in vitro experimental study using essential oils of Cymbopogon flexuosus and Cymbopogon winterianus. The gram-negative strains E. coli (ATCC 25922) and P. aeruginosa (ATCC 27853) and Staphylococcus aureus (ATCC 25923) were used as a Gram-positive strain for the analysis of the antibacterial properties of essential oil. Oil analyzes were carried out using gas chromatography coupled to mass spectrometry (GC/MS). The antibacterial activity of lemongrass (Cymbopogon flexuosus) and citronella (Cymbopogom winterianus) essential oils against bacteria of pathological relevance was confirmed, denoting the potential of using plant essential oils as antibacterial agents, an important alternative considering the emergence of antibiotic resistance.

Behavioural responses of Sitophilus granarius (L.) and Rhyzoperta dominica (F.) to odours of old and modern wheat genotypes

Sitophilus granarius (L.) and Rhyzopertha dominica (F.) are among the major stored-product pests worldwide. The identification of low or un-attractive wheat genotypes toward storage pests and their Volatile Organic Compounds (VOCs) profile is useful in breeding programs and in characterization of behaviourally active compounds suitable in developing semiochemical-based control means. Old wheat cultivars are genetic resources useful for breeding purposes. In this study, the VOC profiles of old genotypes, Senatore Cappelli, old Saragolla, Dauno III, and modern wheat varieties, Mec, Ofanto, Svevo, and Faridur, were characterized by headspace - solid phase microextraction (HD-SPME) and gaschromatography coupled with mass spectrometry (GC-MS) and their attractiveness towards S. granarius and R. dominica adults was evaluated in two-choice pitfall bioassays and Y-tube olfactometer, respectively. Sitophilus granarius adults were significantly attracted to odours of all varieties, with females being significantly more attracted by Faridur, Ofanto, Mec, and old Saragolla compared to Svevo. Rhyzopertha dominica males and females exhibited a significant olfactory preference for the odours of Faridur, Mec, and old Saragolla. The olfactory preferences of both species could be related to differences emerged in varietal VOC profiles. The most attractive variety for both species, Faridur, was rich in alcohols, alkanes, and terpenes. Old Saragolla, Ofanto, and Mec were rich in alcohols and organic acids. Dauno III was the richest variety in alcohols and lactones, and the poorest in aldehydes and terpenes compared to other varieties. Svevo showed the lowest amounts of alcohols and the highest value of aldehydes; Senatore Cappelli was rich in aldehydes, organic acids, and alkanes. The possible effects of the differences in VOC profiles on the olfactory preferences of insects are discussed. The study offers new knowledge for further investigation testing VOCs of the most and the lowest attractive varieties to identify effective attractants or strong repellents towards S. granarius and R. dominica.

Acute oral toxicity and genotoxicity assessment of the essential oil from Croton pulegiodorus Baill (Euphorbiaceae) leaves in mice

Essential oils obtained from Croton pulegiodorus leaf are renowned for their biological activities; however, data on their toxicity are limited. Therefore, this study aimed to evaluate the acute oral toxicity and genotoxicity of a C. pulegiodorus leaf essential oil (CPLEO). Chemical characterization of CPLEO was conducted by gas chromatography coupled to mass spectrometry (GC-MS). In vitro assay was performed to verify the hemolytic capacity of the oil in mice erythrocytes. Next, an acute oral toxicity study was conducted on female mice at CPLEO doses of 2000, 1000, 500, 250, 100, and 50 mg/kg. Hematological, biochemical, and histopathological markers were assessed in mice from groups were no death occurred. Relative consumption of water and food and the weight of animals and their organs were also recorded. Finally, a genotoxicity analysis was performed using the micronucleus and comet assays. The extraction yield of CPLEO was 1.149% and its major compounds were ascaridole (23.18%), eucalyptol (17.20%), camphor (14.20%), p-cymene (7.91%), α-terpineol (4.69%), and isobornyl acetate (4.57%). CPLEO showed a hemolytic effect only at high concentrations (185.5–1000 mg/mL). It showed acute oral toxicity in mice with a LD50 of 460.42 mg/kg. CPLEO (50–250 mg/kg) caused some significant changes in hematological and biochemical parameters. Histopathological evaluation indicated alterations in liver and kidneys but transaminases, urea and creatinine levels remained like the negative control. CPLEO administration impaired weight gain and reduced water and food consumption. Finally, it was not genotoxic by both comet and micronucleus tests. The results highlight the need for attention when choosing doses to evaluate the bioactivities of CPLEO.

Chemical composition, mutagenicity, and cytotoxicity of urban submicron particulate matter (PM1) in Agra, India

This study, conducted in Agra, India, examined the mass concentrations, chemical compositions, and seasonal variations of submicron particles (PM1). The concentrations of metals, water-soluble inorganic ions (WSIs) including anions (F−, Cl−, NO₃−, SO₄2−) and cations (Ca2+, K+, Mg2+, NH₄+, Na+), organic carbon (OC) and elemental carbon (EC) and polycyclic aromatic hydrocarbons (PAHs) in PM1 extract were determined using Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES), Ion Chromatography, Thermogravimetric Analysis and Gas Chromatography-Mass Spectrometry (GC–MS) respectively. For morphological observation of PM1 particles, Field Emission Scanning Electron Microscopy-Energy Dispersive X-ray spectrometry (FESEM-EDS) was used. The annual average concentration of PM1 was 82.9 ± 33.4 μg/m3, which exceeds the World Health Organisation's (WHO) safe limit for PM2.5 of 5 μg/m3 by a factor of 17. The PM1 mass composition included metals (31 %), WSIs (28 %), OC and EC (9.8 %), and PAHs (0.4 %). Winter recorded the highest PM1 concentration (96.1 ± 25.8 μg/m3), followed by post-monsoon, summer, and monsoon seasons. The average concentration of PAHs was 364.6 ± 226.6 ng/m3. Positive Matrix Factorization (PMF) identified traffic, emissions from biomass/coal and wood combustion, industrial/stationary sources, and secondary aerosols as potential contributors. The Ames test revealed the presence of frameshift mutations and base pair substitutions, especially in winter and post-monsoon. Additionally, PM1 exhibited cytotoxic effects on V-79 cells, with heightened toxicity during winter and prolonged exposure in other seasons. This study underscores the urgent need to address local emission sources and establish regulatory standards for PM1 in urban areas.

Effect of zinc oxide-eugenol endodontic paste on planktonic aggregates and biofilm of Enterococcus faecalis - An atomic force microscopy evaluation

ObjectiveThis work aimed to evaluate the in vitro effect of zinc oxide-eugenol paste (ZOE) on planktonic aggregates (EfPA) and biofilm (EfBio) of Enterococcus faecalis, focusing on their morphological aspects observed and analyzed using atomic force microscopy (AFM). DesignThe eugenol and paste were characterized by Gas Chromatography coupled with Mass Spectrometry (GC-MS) and Fourier Transform Infrared Spectroscopy (FTIR), respectively. The effect of ZOE on EfPA and EfBio was evaluated by a direct-contact test through colony counting and crystal violet staining protocol. AFM images of untreated and treated EfPA and EfBio growth on bovine dentin were obtained to analyze the morphological damage caused by the treatments. ResultsThe characterization showed high purity in the eugenol composition and chemical interaction between the components of the paste. A bactericidal effect on aggregates was observed after 6 h of exposure, and on biofilm after 24 h of treatment (p < 0.001). A disruptive effect on the biofilm was also evident. AFM images revealed the formation of EfPA, with a notable presence of an exopolysaccharide matrix. After 6 h of ZOE treatment, there was a significant increase in the size and surface roughness profile of treated cells (p < 0.05). Loss of typical cell morphology was observed after 24 h. The effect on the biofilm showed a tendency towards a less condensed biofilm pattern in the treated group, with no differences in surface roughness. ConclusionZOE presents bactericidal action on EfPA and EfBio, promoting significant morphological changes after treatment, especially in the aggregates.

Chemical Mechanism of Exogenous Jasmonic Acid-Induced Resistance in Rose Against Spodoptera exigua (Lepidoptera: Noctuidae)1

Abstract Jasmonic acid (JA) plays an important role in the indirect plant-mediated interactions between rose powdery mildew (Podosphaera pannosa [Wallr.: Fr.] de Bary) and Spodoptera exigua (Hübner) (Lepidoptera: Noctuidae) on their shared host Rosa chinensis Jacquin. Bioassays showed that the total number of eggs laid by S. exigua on rose twigs decreased significantly after the twigs were treated with exogenous JA. Gas chromatography coupled with mass spectrometry (GC-MS) showed that the volatile organic chemicals (VOCs) from roses, including alkanes, terpenes, aldehydes, ketones, alcohols, and esters, were significantly changed following treatment with JA. Based on gas chromatography-electroantennographic detection (GC-EAD) and GC-MS analysis, the electrophysiological responses of S. exigua moths could be elicited by 8 compounds from the JA-induced roses, including 3-carene, 1-dodecanol, methyl stearate, 1-tetradecanol, hexadecane, eucalyptol, β-myrcene, and 1-iodododecane. Among these chemicals, the first 6 exhibited significant repellent activity to ovipositional behaviors of the gravid moths, while the latter 2 were attractive. The inhibition index of methyl stearate at a concentration of 15 mg/ml reached 65.12%. On the other hand, the quantity of the first 6 chemicals increased significantly and the latter two decreased due to the JA induction. These results reveal a new mechanism for resistance in rose plants against S. exigua. After JA induction, the rose plants appear to up-regulate the biosynthesis of the chemicals with repellent activities against S. exigua and, in the meantime, down-regulate the attractant chemicals.

Chemical constituents and larvicidal activity of the microencapsulated essential oil of Citrus aurantium L. against Aedes aegypti

This study aimed to evaluate the chemical profile and larvicidal activity of the microencapsulated essential oil (EO) of Citrus aurantium L. against Aedes aegypti. The barks of C. aurantium were collected in São Luís-MA. The EO was extracted by hydrodistillation at 100°C for 3h, with chemical characterization through Gas Chromatography coupled with mass spectrometry (GC-MS). Encapsulation of the EO was performed by ionic gelling. To quantify the total phenolic content of the EO, the Folin-Ciocalteu spectrophotometric method was applied. Then, the lethality of the EO against Aedes aegypti was evaluated, and the LC50 for the action of the EO was calculated using the Probit method. The major constituents found in the EO of C. aurantium were: (-)-Terpinen-4-ol (32, 56%) and Caryophyllene oxide (23.52%). The larvicidal activity of the EO showed a LC50 of 3.589 mg L-1. The results indicate that the evaluated EO is composed of substances that provide a good larvicidal effect, revealing its efficiency in combating and controlling Aedes aegypti.

Effect of stationary factors on the yield and chemical composition of essential oils of Tetraclinis articulata (Vahl) Masters from Sdama Chergui massif’s (Tiaret, North-West Algeria)

This paper aims to study the influence of exposure, altitude, and soil pH on the yield and chemical composition of essential oils (EOs) from the leaves of Tetraclinis articulata (Vahl) Masters, developed in the Sdama Chergui massif in northwestern Algeria. These EOs were obtained by hydrodistillation, resulting in average yields of 0.33±0.13 %, 0.29±0.07 %, 0.24±0.07 %, and 0.2±0.03 %, recorded at the south, west, north, and east exposures, respectively. Upon analyzing the obtained EOs by gas chromatography coupled with mass spectrometry (GC/MS), a total of chemical molecules grouped into 22 families were identified. The predominant compounds were Bornyl acetate (9.14 %, 7.95 %, 11.20 %, and 9.78 %), Limonene (5.03 %, 7.18 %, 5.76 %, and 5.41 %), α-Pinene (4.97 %, 5.26 %, 5.09 %, and 4.79 %), Camphor (7.53 %, 3.69 %, 3.01 %, and 5.91 %), and Borneol (5.20 %, 6.26 %, 4.93 %, and 5.11 %). Additionally, the analysis of these molecules by Factorial Analysis of Mixed Data (PCAmix) revealed that exposure, altitude, and soil pH have little effect on the yield and chemical composition of the essential oils of Tetraclinis articulata. Finally, careful attention to stationary parameters is crucial for obtaining essential oils of high quality and optimal quantity.

1H-NMR-based metabolomic profiling and proteomic analysis of soybean (Glycine max L.) in response to dicarboxylic acids (photon) application as a stress priming agent

Soybean (Glycinemax L.) serves not only as food for humans, animals, and industrial purposes, but is also a plant that can be used to comprehend molecular mechanisms occurring in stress response to various development techniques. To reveal the effect of applying dicarboxylic acids as stress priming agents on a metabolic level in soybean leaf extracts, the chemical profile of methanolic extracts were collected at different time points (1 h, 2 h, 12 h, 24 h, 1 week, 2 weeks and 3 weeks) after spraying were analyzed using 1H-NMR based metabolomics by way of PCA and OPLS-DA. The OPLS-DA revealed several metabolites, including organic acids (fumarate, citrate and malate) and amino acids (asparagine, alanine and GABA), which accumulated in higher amounts, with fumarate accumulating the highest in Glycinemax L. leaf extracts compared to untreated leaves. Denaturing 1DE gels were prepared for MS-based protein analysis and the presence of fatty acids (linolenic, oleic and α-linolenic acid) were confirmed by gas chromatography coupled with mass spectrometry (GC-MS), which served as jasmonic acid precursors. The MS-based profiling of proteins on the denaturing 1DE gels revealed several proteins that were differentiated between the treated and untreated leaf extracts. These proteins included ferritins, CaM, ferredoxin-thioredoxin reductase and chalcone-flavanone isomerase 1A. Following the treatment, fumarate was significantly elevated at 12 h to 3 weeks, compared to other compounds. It is, therefore, proposed that elevated quantities of fumarate could be related to the KEAP1-NRF2 metabolic pathway. This study represents the initial investigation of the effect of dicarboxylic acid application as a stress priming agent on Glycinemax L. using 1H-NMR metabolomic analysis, GC-MS and proteomic analysis.

Essential Oils from Phlomis longifolia Boiss. &amp; C.I. Blanche. Aerial Parts (Flowers, Calyxes, Leaves): GC-MS Analyzes and Biological Properties

Objective/Background: Phlomis longifolia Boiss. &amp; C.I. Blanche. is one of the significant medicinal plants extensively utilized in folk medicine in Syria. So, this study aimed to identify the chemical components with potential pharmacological properties of essential oils extracted from the aerial parts of the Syrian P. longifolia plant for the first time. Methods: The aerial parts of the plant were collected from a mountainous area in Latakia Province, Syria. Subsequently, the essential oils were obtained using hydrodistillation with a yield of (0.14% for flowers, 0.075% for calyxes, and 0.19% for leaves) using a Clevenger-type apparatus and analyzed by gas chromatography coupled with mass spectrometry (GC-MS). Results: A total of 63, 61, and 48 compounds, which represent (98.0%, 97.1%, and 97.9%) of the total oils, were identified for flowers, calyxes, and leaves, respectively. The major compounds identified in the flower's essential oil were: widdrol (29.8%), β-caryophyllene (9.7%), and (E)-nerolidyl acetate (5.8%). While in the calyx's essential oil were: (E)-nerolidyl acetate (8.6%), α-humulene (8.1%), and β-caryophyllene (7.7%). As for the leave's essential oil were: (E)-nerolidyl acetate (11.4%), β-caryophyllene (9.5%), α-amorphene (8.8%), caryophyllene oxide (6.7%), α-humulene (5.3%), and 3,5-dihydroxy-6-methyl-2,3-dihydro-4H-pyran-4-one (5.2%). Additionally, the majority of the identified compounds have various biological activities, according to the published literature. Conclusion: In this work, the chemical composition of essential oils extracted from the aerial parts of P. longifolia was determined for the first time by GC-MS. Terpenes were the dominant chemical content of essential oils (83.3% for flowers, 72.7% for calyxes, and 80.9 for leaves), and sesquiterpenes had the highest concentration among them (77.3% for flowers, 65.7% for calyxes, and 77.1% for leaves). These compounds are known for their diverse biological activities and promote the use of such plants in phytopharmaceuticals.

Analysis of Essential Oils Extracted from Algerian Medicinal Plants and Their Aphicidal Effect Against the Melon Aphid Aphis Gossypii Glover (Homoptera: Aphididae)

Chemical insecticides are decisive in controlling insect pests, but they harm the environment. Reducing the use of chemical insecticides has become the main goal for ensuring healthy produce. However, research focusing on plant-based compounds has recently increased. The present study was carried out to analyze essential oils extracted from Algerian medicinal plants by gas chromatography coupled with mass spectrometry (GC-MS) to determine the insecticidal activity of essential oils from Juniperus phoenicea, Rosmarinus officinalis, Lavandula stoechas, Mentha pulegium and Pinus sylvestris, against Aphis gossypii Glover The main components constituting each essential oil were: α-pinene, β-Pinene 1,8- cineol, Linalool, Linalyl acetate, Fenchone, Pulegone, and Camphor. The toxicity of tested essential oils against Aphis gossypii was different and dependent on the concentration used (1000, 10000, and 100000 ppm), the duration of exposure (24, 48, and 72 h), and the chemical composition of the oil. The highest toxicity was for J. phoenicea, M. pulegium, and L. stoechas which were toxic as Actara® insecticide.

Analysis of the Volatile and Enantiomeric Compounds Emitted by Plumeria rubra L. Flowers Using HS-SPME-GC.

The volatile components emitted by fresh aromatic flowers of Plumeria rubra L., harvested in southern Ecuador during three different months were determined to evaluate the fluctuation of secondary metabolites. The volatile compounds were analyzed using headspace solid-phase microextraction (HS-SPME) followed by gas chromatography coupled to mass spectrometry (GC-MS) and a flame ionization detector (GC-FID) using two types of columns: a non-polar (DB-5ms) and polar column (HP-INNOWax). The principal chemical groups were hydrocarbon sesquiterpenes (43.5%; 40.0%), oxygenated sesquiterpenes (23.4%; 26.4%), oxygenated monoterpenes (14.0%; 11.2%), and hydrocarbon monoterpenes (12.7%; 9.3%). The most representative constituents were (E,E)-α-Farnesene (40.9-41.2%; 38.5-50.6%), (E)-nerolidol (21.4-32.6%; 23.2-33.0%), (E)-β-ocimene (4.2-12.5%; 4.5-9.1%), (Z)-dihydro-apofarnesol (6.5-9.9%; 7.6-8.6%), linalool (5.6-8.3%; 3.3-7.8%), and perillene (3.1-5.9%; 3.0-3.2%) in DB-5ms and HP-INNOWax, respectively. Finally, we reported for the first time the enantiomeric distribution of P. rubra flowers, where the enantiomers (1R,5R)-(+)-α-pinene, (S)-(-)-limonene, (S)-(+)-Linalool, and (1S,2R,6R,7R,8R)-(+)-α-copaene were present as enantiomerically pure substances, whereas (S)-(+)-(E)-Nerolidol and (R)-(+)-(E)-Nerolidol were observed as scalemic mixtures. This study provides the first comprehensive and comparative aroma profile of Plumeria rubra cultivated in southern Ecuador and gave us a clue to the variability of P. rubra chemotypes depending on the harvesting time, which could be used for future quality control or applications in phytopharmaceutical and food industries.

Genotoxic and antiproliferative effect of Alpinia zerumbet (Zingiberaceae) essential oil in Allium cepa biotest

The species Alpinia zerumbet popularly known as colony is quite abundant in northeastern Brazil and is widely used for medicinal purposes, due to its hypotensive and cardiovascular effect, without, however, due scientific evidence. Therefore, the objective of this study was to evaluate the genotoxic and antiproliferative effect of A. zerumbet essential oil, in test systems with Allium cepa. The chemical composition of the essential oil was determined by gas chromatography coupled with mass spectrometry (GC-MS). The antiproliferative and genotoxic effect was tested in seven treatments with three replications, and five concentrations of essential oil (0.01 to 1.0%) using onion bulbs. Two roots were analyzed from each bulb, with a count of 500 cells per slide/root, totaling 3,000 cells per treatment. The results showed that the main chemical constituents of the essential oil were 1.8 cineole (60.50%) and terpinen-4-ol (23.80%). In the assays with A. cepa, both the mitotic index (MI) and the cellular alteration percentages differed significantly in relation to the control, through the appearance of chromosomal and nuclear aberrations at the concentrations tested, revealing possible harmful effects to human health.