scholarly journals Separation ofcis- andtrans-Asarone fromAcorus tatarinowiiby Preparative Gas Chromatography

2012 ◽  
Vol 2012 ◽  
pp. 1-5 ◽  
Author(s):  
H. L. Zuo ◽  
F. Q. Yang ◽  
X. M. Zhang ◽  
Z. N. Xia

A preparative gas chromatography (pGC) method was developed for the separation of isomers (cis- andtrans-asarone) from essential oil ofAcorus tatarinowii. The oil was primarily fractionated by silica gel chromatography using different ratios of petroleum ether and ethyl acetate as gradient elution solvents. And then the fraction that contains mixture of the isomers was further separated by pGC. The compounds were separated on a stainless steel column packed with 10% OV-101 (3 m × 6 mm, i.d.), and then the effluent was split into two gas flows. One percent of the effluent passed to the flame ionization detector (FID) for detection and the remaining 99% was directed to the fraction collector. Two isomers were collected after 90 single injections (5 uL) with the yield of 178 mg and 82 mg, respectively. Furthermore, the structures of the obtained compounds were identified ascis- andtrans-asarone by1H- and13C-NMR spectra, respectively.

2011 ◽  
Vol 2011 ◽  
pp. 1-6 ◽  
Author(s):  
F. Q. Yang ◽  
H. K. Wang ◽  
H. Chen ◽  
J. D. Chen ◽  
Z. N. Xia

A preparative gas chromatography (pGC) method was developed for the separation of volatile components from the methanol extract ofCurcumarhizome. The compounds were separated on a stainless steel column packed with 10% OV-101 (3 m × 6 mm, i.d.), and then, the effluent was split into two gas flows. One percent of the effluent passed to the flame ionization detector (FID) for detection and the remaining 99% were directed to the fraction collector. Five volatile compounds were collected from the methanol extract ofCurcumarhizome (5 g/mL) after 83 single injections (20 uL) with the yield of 5.1–46.2 mg. Furthermore, the structures of the obtained compounds were identified asβ-elemene, curzerene, curzerenone, curcumenol, and curcumenone by MS and NMR spectra, respectively.


1978 ◽  
Vol 61 (3) ◽  
pp. 500-503
Author(s):  
Leonard R Schronk ◽  
Billy M Colvin ◽  
Alan R Hanks

Abstract Flame ionization gas-liquid chromatography (GLC) with a 10% DC-200 on 80-100 mesh Gas-Chrom Q column is used for the rapid determination of oxydemeton-methyl in commercial formulations. The detector response is linear for 1.0–10.0 μg oxydemeton-methyl, with a sensitivity of 4 ng. The column was stabilized before analysis by injection of a lecithin solution. Samples were diluted with chloroform and injected; peak height ratios were used for quantitation with fluoranthrene as the internal standard. Carbaryl was removed from mixed formulations by silica gel chromatography, oxydemeton- methyl was eluted with methanolchloroform (2+98), and the eluate was collected for infrared (IR) and GLC analyses. Methoxychlor and Karathane were removed by chromatography on Florisil before IR analysis. GLC results compare favorably with those for IR, with recoveries ranging from 98.44 to 102.88% for spiked formulations.


1996 ◽  
Vol 79 (6) ◽  
pp. 1423-1427 ◽  
Author(s):  
Rosario Garcia-Repetto ◽  
Isabel Garrtoo ◽  
Manuel Repetto

Abstract A multiresidue analytical method is described for determining 6 pesticides in wine: chlorpyrifos, dimethoate, quinalphos, simazine, tetradifon, and endosulfan. Wine (200 mL) is extracted with dichloromethane (50 mL, 3 times), and the evaporated extracts are purified by silica gel chromatography. Pesticide residues are eluted with n-hexane, n-hexane-benzene (1 + 1), benzene, benzene–acetone (1 + 1), and acetone. Residues are determined by gas chromatography with nitrogen–phosphorus and electron capture detection, using CPSH-5CB, Carbo wax-20M, and CPSH-19CB columns. Recoveries of pesticides added at 0.025 μg/L were 83–97%, with standard deviations of 0.01–0.05%. Detection limits were 0.13–8.9 ng/L, except for simazine (36.7 μg/L). Results are compared with those obtained with a solid-phase extraction (C18) purification and with different eluant series.


2018 ◽  
Vol 16 (1) ◽  
pp. 453-467 ◽  
Author(s):  
Gülmira Özek ◽  
Erdal Bedir ◽  
Nurhayat Tabanca ◽  
Abbas Ali ◽  
Ikhlas A. Khan ◽  
...  

AbstractIn the present work, an endemic species Prangos heyniae collected in four locations from Turkey was subjected to hydrodistillation in Clevenger type apparatus to obtain the essential oils (EO1-4). The gas-chromatography/mass spectrometry (GC/MS) and gas-chromatography-flame ionization detector (GC/FID) analyses showed that the EOs were rich in sesquiterpenes, germacrene D (10.3-12.1%), β-bisabolene (14.4%), kessane (26.9%), germacrene B (8.2%), elemol (3.4-46.9%), β-bisabolenal (1.4-70.7%), β-bisabolenol (8.4%) and an eudesmane type sesquiterpene (1) (16.1%) with [M+218]. This unidentified compound (1) was isolated in a rapid one-step manner with >95.0% purity using Preparative Capillary Gas Chromatography (PCGC) with an HP Innowax column connected to a Preparative Fraction Collector (PFC) system. Structure determination was accomplished from 1D- and 2D-NMR spectroscopic data which determined a new eudesmane type sesquiterpene, 3,7(11)-eudesmadien-2-one (1). Using a biting deterrent bioassay, the mean proportion not biting (PNB) values of the P. heyniae EO1-4 were 0.88 for EO1 and 0.80 for EO2 which were similar to the positive control DEET (N,N-diethyl-3-methylbenzamide). The EO3 and EO4 had lower PNB values of 0.64 and 0.44, respectively. P. heyniae EO1-4 showed good larvicidal activity at 125 and 62.5 ppm whereas EO1-3 were slightly less effective at the dose of 31.25 ppm and EO4 was not active at 31.25 ppm against 1st instar Aedes aegypti.


1972 ◽  
Vol 55 (6) ◽  
pp. 1280-1287
Author(s):  
W A Steller ◽  
N R Pasarela

Abstract Residues of both dimethoate and dimethoxon are extracted from finely chopped plant or animal tissues with methylene chloride. The resulting extract is concentrated and cleaned up by silica gel chromatography, if necessary. The concentrate is injected into a gas chromatograph equipped with either a flame photometric or an alkali flame ionization detector and a column containing 11% DC-200 on 60–80 mesh Gas-Chrom Q/0.01% Versamid 900. Recovery values for dimethoate and dimethoxon added a t 0.002–1.0 p pm ranged from 56 to 112% with an overall average of 89.2% for dimethoate and from 60 to 127% with an overall average of 81.9% for dimethoxon. The lower limit at which recovery values were obtained for both compounds was 0.05 p pm for plant tissues, 0.02 for animal tissues and eggs, and 0.002 for milk. Residue values obtained for animal tissues involving both exposure and feeding studies a n d for field-treated plant samples are also presented.


Molecules ◽  
2021 ◽  
Vol 26 (15) ◽  
pp. 4608
Author(s):  
Eduardo Valarezo ◽  
Génesis Gaona-Granda ◽  
Vladimir Morocho ◽  
Luis Cartuche ◽  
James Calva ◽  
...  

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.


2020 ◽  
Vol 15 (12) ◽  
pp. 1934578X2098123
Author(s):  
Peng-fei Yang ◽  
Hui Lu ◽  
Qiong-bo Wang ◽  
Zhi-wei Zhao ◽  
Qiang Liu ◽  
...  

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.


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