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Separation of cis- and trans-Asarone from Acorus tatarinowii by Preparative Gas Chromatography.

Zuo HL, Yang FQ, Zhang XM, Xia ZN - J Anal Methods Chem (2012)

Bottom Line: 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.Two isomers were collected after 90 single injections (5 uL) with the yield of 178 mg and 82 mg, respectively.

View Article: PubMed Central - PubMed

Affiliation: College of Chemistry and Chemical Engineering, Chongqing University, Chongqing 400030, China.

ABSTRACT
A preparative gas chromatography (pGC) method was developed for the separation of isomers (cis- and trans-asarone) from essential oil of Acorus 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 as cis- and trans-asarone by (1)H- and (13)C-NMR spectra, respectively.

No MeSH data available.


Related in: MedlinePlus

TLC of collected fractions (F1 and F2). Developing solvent: PE : EA = 3 : 1. Colorizing agent: vanillin in concentrated sulfuric acid, 5% w/v.
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fig3: TLC of collected fractions (F1 and F2). Developing solvent: PE : EA = 3 : 1. Colorizing agent: vanillin in concentrated sulfuric acid, 5% w/v.

Mentions: Capillary GC chromatograms as well as mass spectra of peaks of every collected fraction are given in Figure 2. It is indicated that the two isomers can be well separated by pGC and result in high purity products (Figure 2). Actually, the isomers are difficult to be separated by conventional method such as silica gel chromatography. As shown in Figure 3, the two separated isomers (F1 and F2) have the same retention factor (Rf) values and similar color (claret-colored). Therefore, pGC shows advantages over the conventional silica gel chromatography in the separation and preparation of volatile isomers.


Separation of cis- and trans-Asarone from Acorus tatarinowii by Preparative Gas Chromatography.

Zuo HL, Yang FQ, Zhang XM, Xia ZN - J Anal Methods Chem (2012)

TLC of collected fractions (F1 and F2). Developing solvent: PE : EA = 3 : 1. Colorizing agent: vanillin in concentrated sulfuric acid, 5% w/v.
© Copyright Policy - open-access
Related In: Results  -  Collection

Show All Figures
getmorefigures.php?uid=PMC3303141&req=5

fig3: TLC of collected fractions (F1 and F2). Developing solvent: PE : EA = 3 : 1. Colorizing agent: vanillin in concentrated sulfuric acid, 5% w/v.
Mentions: Capillary GC chromatograms as well as mass spectra of peaks of every collected fraction are given in Figure 2. It is indicated that the two isomers can be well separated by pGC and result in high purity products (Figure 2). Actually, the isomers are difficult to be separated by conventional method such as silica gel chromatography. As shown in Figure 3, the two separated isomers (F1 and F2) have the same retention factor (Rf) values and similar color (claret-colored). Therefore, pGC shows advantages over the conventional silica gel chromatography in the separation and preparation of volatile isomers.

Bottom Line: 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.Two isomers were collected after 90 single injections (5 uL) with the yield of 178 mg and 82 mg, respectively.

View Article: PubMed Central - PubMed

Affiliation: College of Chemistry and Chemical Engineering, Chongqing University, Chongqing 400030, China.

ABSTRACT
A preparative gas chromatography (pGC) method was developed for the separation of isomers (cis- and trans-asarone) from essential oil of Acorus 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 as cis- and trans-asarone by (1)H- and (13)C-NMR spectra, respectively.

No MeSH data available.


Related in: MedlinePlus