scholarly journals Development of a Novel Microwave Distillation Technique for the Isolation of Cannabis sativa L. Essential Oil and Gas Chromatography Analyses for the Comprehensive Characterization of Terpenes and Terpenoids, Including Their Enantio-Distribution

Molecules ◽  
2021 ◽  
Vol 26 (6) ◽  
pp. 1588
Author(s):  
Giuseppe Micalizzi ◽  
Filippo Alibrando ◽  
Federica Vento ◽  
Emanuela Trovato ◽  
Mariosimone Zoccali ◽  
...  
Keyword(s):  
Essential Oil ◽  
Oil And Gas ◽  
Cannabis Sativa ◽  
Internal Standard ◽  
Absolute Quantification ◽  
Internal Standard Method ◽  
Response Factors ◽  
Chiral Compounds ◽  
Flame Ionization ◽  
Microwave Distillation

A microwave distillation method was optimized for the extraction and isolation of cannabis essential oil from fresh and dried hemp inflorescences. The developed method enabled us to obtain a distilled product rich in terpenes and terpenoid compounds, responsible of the typical and unique smell of the cannabis plant. The distillate from different hemp cultivars, including Kompolti, Futura 75, Carmagnola, Felina 32 and Finola were characterized by using a gas chromatograph equipped with both mass spectrometer and flame ionization detectors. In a single chromatographic run, the identity and absolute amounts of distilled compounds were determined. Peak assignment was established using a reliable approach based on the usage of two identification parameters, named reverse match, and linear retention index filter. Absolute quantification (mg g−1) of the analytes was performed using an internal standard method applying the flame ionization detector (FID) response factors according to each chemical family. An enantio-GC-MS method was also developed in order to evaluate the enantiomeric distribution of chiral compounds, an analytical approach commonly utilized for establishing the authenticity of suspicious samples.

scholarly journals Reliable Identification and Quantification of Volatile Components of Sage Essential Oil Using Ultra HRGC

2011 ◽  
Vol 6 (3) ◽  
pp. 1934578X1100600 ◽  
Author(s):  
Laura Tedone ◽  
Ivana Bonaccorsi ◽  
Paola Dugo ◽  
Antonella Cotroneo ◽  
Giovanni Dugo ◽  
...  
Keyword(s):  
Essential Oil ◽  
Stationary Phases ◽  
Internal Standard ◽  
Volatile Components ◽  
Internal Standard Method ◽  
Response Factors ◽  
Reliable Identification ◽  
Relative Response ◽  
Linear Retention Index ◽  
Chemical Class

Salvia officinalis (common sage) essential oil was chemically characterized by means of GC-MS, using 100 meter capillary columns with two different stationary phases. Identification of the analytes was carried out by means of the FFNSC mass spectrum library and the use of the Linear Retention Index (LRI) as an extra criterion of library searching. Quantitative analysis was also carried out by means of GC-FID with the internal standard method and the use of relative response factors determined for each chemical class of components. A total of 45 compounds were identified and quantified and reported with their experimental LRI values.

Development and Validation of Analytical Method for Simultaneous Estimation of Active Constituents in a Polyherbal Ointment by Gas Chromatography

2019 ◽  
Vol 102 (4) ◽  
pp. 1027-1032
Author(s):  
Vishal R Patel ◽  
Hardik K Soni ◽  
Vikram B Trivedi ◽  
Jigna B Patel ◽  
Suresh Jain
Keyword(s):  
Methyl Salicylate ◽  
Internal Standard ◽  
Correlation Coefficients ◽  
Simultaneous Estimation ◽  
Internal Standard Method ◽  
Active Constituents ◽  
Flame Ionization ◽  
Quality Control Testing ◽  
Marker Compounds ◽  
Development And Validation

Abstract Background: The simultaneous, quantitative determination of all active ingredients present in the analgesic formulation (Dazzle ointment) requires an ideal and novel method by which these phytoconstituents can be separated with the highest resolution without any interference from one another. Objective: The present work was conducted to develop and validate a quantitative method for the simultaneous estimation of all five phytoconstituents present in a polyherbal analgesic ointment by GC. Methods: α-Pinene, 1,8-cineole, camphor, menthol, and methyl salicylate present in the ingredients of the ointment were analyzed and quantified by GC using a crosslinked 5% phenyl polydimethylsiloxane capillary column, nitrogen as a carrier gas, and a flame-ionization detector. Aniline was used as the internal standard. Method validation was also performed in order to demonstrate its selectivity, linearity, accuracy, precision, LOD, LOQ, and robustness. Results: The calibration curves of all five marker compounds showed good linear correlation coefficients (r2 >0.998) within the tested ranges. The precision of the method was tested by carrying out intra- and interday analyses of the same sample. RSD values were observed to be <1.00%. The accuracy of the method, determined by performing recovery studies, was found to be between 99.25 and 101.39%. The developed method was also demonstrated to be robust (RSD <1.29%) by making small but deliberate variations in method parameters. Conclusions: The developed GC method is simple, precise, and accurate, it and can be used for the rapid quality control testing of the polyherbal formulation. Highlights: The developed GC method will assist in the standardization of polyherbal analgesic formulation consists of α-pinene, 1,8-cineole, camphor, menthol, and methyl salicylate as active constituents.

scholarly journals Chemical, Enantioselective, and Sensory Analysis of a Cholinesterase Inhibitor Essential Oil from Coreopsis triloba S.F. Blake (Asteraceae)

Plants ◽  
2019 ◽  
Vol 8 (11) ◽  
pp. 448 ◽  
Author(s):  
Sandra Espinosa ◽  
Nicole Bec ◽  
Christian Larroque ◽  
Jorge Ramírez ◽  
Barbara Sgorbini ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Essential Oil ◽  
Enthalpy Of Combustion ◽  
Response Factors ◽  
Flame Ionization ◽  
Gas Chromatography Olfactometry ◽  
Germacrene D ◽  
Biological Tests ◽  
Main Components ◽  
Main Component

The fresh leaves of Coreopsis triloba S.F. Blake, collected at Cerro Villonaco in Loja, Ecuador, were investigated with respect to their essential oil (EO). The chemical composition was determined qualitatively through gas chromatography coupled with mass spectrometry (GC-MS) and quantitatively by gas chromatography coupled with flame ionization (GC-FID), using relative response factors (RRF) based on the enthalpy of combustion. The essential oil contained between 92.5% and 93.4% of monoterpene hydrocarbons, with (E)-β-ocimene being the main component (35.2–35.9%), followed by β-phellandrene (24.6–25.0%), α-pinene (15.3–15.9%), myrcene (10.9–11.0%), sabinene (2.2–2.4%), (Z)-β-ocimene (1.5%), and germacrene D (1.2–1.3%). The enantiomeric distribution of α-pinene, β-pinene, limonene, and germacrene D was also determined. The main components responsible for the aroma were identified through aroma extract dilution analysis (AEDA), a gas chromatography-olfactometry (GC-O) based technique, being α-pinene, β-pinene (0.6%), terpinolene (0.1%), α-copaene (0.1–0.3%), β-phellandrene, and (E)-4,8-dimethyl-1,3,7-nonatriene (0.1–0.2%) the main olfactory constituents according to the decreasing factor of dilution (FD) order. The biological tests showed IC50 inhibition values of 42.2 and 6.8 µg/mL for acetylcholinesterase (AChE) and butyrylcholinesterase (BChE), respectively.

scholarly journals Metabolomic Analysis of Cannabinoid and Essential Oil Profiles in Different Hemp (Cannabis sativa L.) Phenotypes

Plants ◽  
2021 ◽  
Vol 10 (5) ◽  
pp. 966
Author(s):  
Marjeta Eržen ◽  
Iztok J. Košir ◽  
Miha Ocvirk ◽  
Samo Kreft ◽  
Andreja Čerenak
Keyword(s):  
Essential Oil ◽  
High Performance ◽  
Cannabis Sativa ◽  
Animal Health ◽  
Principal Component ◽  
Total Content ◽  
Therapeutic Effects ◽  
Flame Ionization Detection ◽  
Flame Ionization ◽  
Chemical Profiles

Hemp (Cannabis sativa L.) cannabinoids and terpenoids have therapeutic effects on human and animal health. Cannabis plants can often have a relatively high heterogeneity, which leads to different phenotypes that have different chemical profiles despite being from the same variety. Little information exists about cannabinoid and terpenoid profiles in different hemp phenotypes within the same variety. For this study, 11 phenotypes from three different varieties (“Carmagnola” selected (CS), “Tiborszallasi” (TS), and “Finola” selection (FS)) were analyzed. The components of essential oil (29) were analyzed using gas chromatography with flame ionization detection (GC/FID), and 10 different cannabinoids of each phenotype were determined using high-performance liquid chromatography (HPLC). Principal component analysis (PCA) and analysis of variance (ANOVA) showed that according to the components of essential oil, FS and TS plants were more uniform than CS plants, where there were great differences between CI and CII phenotypes. The content of cannabinoid CBD-A was the highest in all four FS phenotypes. By comparing cannabinoid profiles, FS was clearly separated from TS and CS, while these two varieties were not clearly distinguishable. Phenotypes TV and CI had the highest total content of Δ-9-THC, while all phenotypes of FS had the highest total content of CBD. The highest total content of CBG was determined in phenotype CI. Obtained results are useful for the development of new supplementary ingredients, for different pharmacy treatments, and for further breeding purposes.

Flame ionization detector response to coeluting hydrocarbons and carbon disulphide and its application to the determination of the sum of C6-C11 alkanes and cycloalkanes in air

1983 ◽  
Vol 48 (3) ◽  
pp. 722-734
Author(s):  
Martin Koval
Keyword(s):  
Carbon Disulphide ◽  
Internal Standard ◽  
Calibration Procedure ◽  
Detector Response ◽  
Column Temperature ◽  
Flame Ionization ◽  
Other Substances ◽  
Flame Ionisation Detector ◽  
Ionisation Detector

The flame ionisation detector response to C6-C11 aliphatic hydrocarbon solutions in carbon disulphide in the concentration range between 1.3-9.5 mg ml-1 retained lineary despite the excess of solvent entering the detector simultaneously with the analyte. Pure carbon disulphide exhibited a small positive detector response which did not interfere in calibration procedure and which, under certain GC conditions, inverted to negative values. This response was not proportional to the injected volume and was strongly influenced by the column temperature and/or bleed. On the basis of these findings, a method compatible with the widely used charcoal tube carbon disulphide desorption procedure was developed and evaluated. It consists of static desorption of the sum of aliphatic alkanes and cycloalkanes from the activated charcoal after which an internal standard is added to the supernatant eluate. The resulting carbon disulphide solution is analysed on a highly polar stationary phase 1,2,3-tris(2-cyanoethoxy)propane where the solvent and the analyte coelute in a single peak, the height of which is practically proportional to the sum of alkanes and cycloalkanes present. This also makes determinations of other substances present in the sample more simple. The field test of the proposed method yielded values comparable in precision and accuracy with a control infrared spectrophotometric method.

Determination of alcohols in mixtures by 19F NMR spectroscopy using hexefluoroacetone reagent

1982 ◽  
Vol 47 (7) ◽  
pp. 1973-1978 ◽  
Author(s):  
Jiří Karhan ◽  
Zbyněk Ksandr ◽  
Jiřina Vlková ◽  
Věra Špatná
Keyword(s):  
Standard Deviation ◽  
Nmr Spectroscopy ◽  
Standard Method ◽  
Internal Standard ◽  
Internal Standard Method ◽  
Concentration Region ◽  
Experimental Conditions ◽  
Curve Method ◽  
Sample Preparation Procedure

The determination of alcohols by 19F NMR spectroscopy making use of their reaction with hexafluoroacetone giving rise to hemiacetals was studied on butanols. The calibration curve method and the internal standard method were used and the results were mutually compared. The effects of some experimental conditions, viz. the sample preparation procedure, concentration, spectrometer setting, and electronic integration, were investigated; the conditions, particularly the concentrations, proved to have a statistically significant effect on the results of determination. For the internal standard method, the standard deviation was 0.061 in the concentration region 0.032-0.74 mol l-1. The method was applied to a determination of alcohols in the distillation residue from an oxo synthesis.

scholarly journals Chemical Constituents of the Essential Oil from Ecuadorian Endemic Species Croton ferrugineus and Its Antimicrobial, Antioxidant and α-Glucosidase Inhibitory Activity

Molecules ◽  
2021 ◽  
Vol 26 (15) ◽  
pp. 4608
Author(s):  
Eduardo Valarezo ◽  
Génesis Gaona-Granda ◽  
Vladimir Morocho ◽  
Luis Cartuche ◽  
James Calva ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Essential Oil ◽  
Endemic Species ◽  
Chemical Constituents ◽  
Radical Scavenging ◽  
Moderate Activity ◽  
Gram Positive Bacteria ◽  
Flame Ionization ◽  
Total Composition ◽  
Radical Scavenging Properties

Croton ferrugineus Kunth is an endemic species of Ecuador used in traditional medicine both for wound healing and as an antiseptic. In this study, fresh Croton ferrugineus leaves were collected and subjected to hydrodistillation for extraction of the essential oil. The chemical composition of the essential oil was determined by gas chromatography equipped with a flame ionization detector and gas chromatography coupled to a mass spectrometer using a non-polar and a polar chromatographic column. The antibacterial activity was assayed against three Gram-positive bacteria, one Gram-negative bacterium and one dermatophyte fungus. The radical scavenging properties of the essential oil was evaluated by means of DPPH and ABTS assays. The chemical analysis allowed us to identify thirty-five compounds representing more than 99.95% of the total composition. Aliphatic sesquiterpene hydrocarbon trans-caryophyllene was the main constituent with 20.47 ± 1.25%. Other main compounds were myrcene (11.47 ± 1.56%), β-phellandrene (10.55 ± 0.02%), germacrene D (7.60 ± 0.60%), and α-humulene (5.49 ± 0.38%). The essential oil from Croton ferrugineus presented moderate activity against Candida albicans (ATCC 10231) with an MIC of 1000 μg/mL, a scavenging capacity SC50 of 901 ± 20 µg/mL with the ABTS method, and very strong antiglucosidase activity with an IC50 of 146 ± 20 µg/mL.

scholarly journals Chemical Composition and Antimicrobial Activities of the Essential Oil From the Leaves of Pterocephalus hookeri

2020 ◽  
Vol 15 (12) ◽  
pp. 1934578X2098123
Author(s):  
Peng-fei Yang ◽  
Hui Lu ◽  
Qiong-bo Wang ◽  
Zhi-wei Zhao ◽  
Qiang Liu ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Chemical Composition ◽  
Essential Oil ◽  
Chemical Constituents ◽  
Antimicrobial Activities ◽  
Gas Chromatography Mass Spectrometry ◽  
Flame Ionization ◽  
And Staphylococcus Aureus ◽  
Antimicrobial Assay ◽  
Detailed Chemical

Detailed chemical constituents of essential oil from the Pterocephalus hookeri leaves and its antimicrobial activities were investigated in this study. The essential oil, obtained by hydrodistillation, was characterized by gas chromatography-flame ionization detection and gas chromatography-mass spectrometry analyses. Among the 90 identified compounds, hexadecanoic acid (21.27%), phytol (8.03%), furfural (7.08%), oleic acid (5.25%), and phytone (4.56%) were the major components. In the antimicrobial assay, the essential oil showed strong inhibitory activities against Escherichia coli, Candida albicans, and Staphylococcus aureus with minimum inhibitory concentration values of 31.3, 62.5, and 125 µg/mL, respectively. To our knowledge, this is the first report concerning chemical composition and antimicrobial activities of the essential oil from Pterocephalus hookeri.

scholarly journals Minerals, Essential Oils, and Biological Properties of Melissa officinalis L.

Plants ◽  
2021 ◽  
Vol 10 (6) ◽  
pp. 1066
Author(s):  
Fahima Abdellatif ◽  
Muhammad Akram ◽  
Samir Begaa ◽  
Mohammed Messaoudi ◽  
Adel Benarfa ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Essential Oil ◽  
Pathogenic Bacteria ◽  
Antimicrobial Activities ◽  
Biological Properties ◽  
Phytopathogenic Fungi ◽  
Melissa Officinalis ◽  
Flame Ionization ◽  
Analysis Technique ◽  
Total Oil

This study describes the minerals elements, chemical composition, antioxidant and antimicrobial activities of Algerian Melissa officinalis plant. The essential oil (EO) was extracted by hydrodistillation (HD) using a Clevenger-type apparatus of dry leaves of M. officinalis and was analyzed by two techniques, gas chromatography coupled with flame ionization (GC-FID) and gas chromatography coupled with mass spectrometry (GC-MS). Eighteen minerals comprising both macro- and microelements (As, Br, K, La, Na, Sb, Sm, Ba, Ca, Ce, Co, Cr, Cs, Fe, Rb, Sc, Th, and Zn) were determined using neutron activation analysis technique for the first time from Algerian Melissa officinalis plant. Seventy-eight compounds were identified in the essential oil, representing 94.090% of the total oil and the yields were 0.470%. The major component was geranial (45.060%). Other predominant components were neral (31.720%) and citronellal (6.420%). The essential oil presented high antimicrobial activity against microorganisms, mainly five human pathogenic bacteria, one yeast, Candida albicans, and two phytopathogenic fungi. The results can be used as a source of information for the pharmaceutical industry and medical research.

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