Nicotianasesterpene-F prepared through supercritical fluid chromatography and application of nicotianasesterpene-F
A supercritical fluid, sesquiterpene technology, applied in the field of tobacco chemistry, can solve the problem that the components have not been identified yet, etc.
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Embodiment 1
[0024] The tobacco samples were from Yuxi, Yunnan, and the variety was Yuxi K326. Sampling 2.0 kg of tobacco was pulverized and extracted 5 times with 95% methanol for 24 hours each time. The extracts were combined, filtered, and concentrated under reduced pressure to form an extract to obtain 105 g of extract. After dissolving the extract with 2.0 times the amount of pure methanol by weight, mix the sample with 120 g of 100-mesh silica gel, pack 0.4 kg of 160-mesh silica gel into a column for silica gel column chromatography, and use a volume ratio of 1:0, 20:1, Chloroform-acetone gradient elution of 9:1, 8:2, 7:3, 6:4, 1:1, 1:2, monitored by thin layer chromatography (TLC) Merge the same parts to obtain 8 parts, of which the volume Proportioning ratio is 8:2 Chloroform-acetone elution part uses Waters SFC80Q supercritical fluid preparative chromatographic separation, with carbon dioxide / methanol as mobile phase (90 / 10%, mass ratio), Silica2-EP (10mm * 150mm, 5μm) preparativ...
Embodiment 2
[0026]The tobacco sample comes from Dali, Yunnan, and the variety is Yunyan 200. The tobacco sample is 3.5kg and chopped, and extracted 4 times with 95% ethanol, each extraction is 48h, the extracts are combined, filtered, and concentrated under reduced pressure to obtain an extract. 250g. The extract is dissolved in pure methanol with a weight ratio of 2.0 times, and then mixed with 250 g of 80-mesh silica gel, and 0.5 kg of 200-mesh silica gel is packed into a column for silica gel column chromatography. The volume ratio is 1:0, 20:1, 9:1, 8:2, 7:3, 6:4, 1:1, 1:2 chloroform-acetone gradient elution, TLC monitoring and merging the same parts to obtain 8 parts, wherein the volume ratio is 8: The chloroform-acetone eluting part of 2 uses Waters SFC80Q supercritical fluid preparative chromatographic separation, is mobile phase (90 / 10%, mass ratio) with carbon dioxide / methanol, Silica2-EP (10mm * 150mm, 5 μ m) preparative column is Stationary phase, the mobile phase flow rate is...
Embodiment 3
[0028] The tobacco sample comes from Kunming, Yunnan, and the variety is Honghua Dajinyuan. The tobacco sample is 5kg and pulverized, and extracted 3 times with 75% acetone by ultrasound, each extraction is 72h, the extracts are combined, filtered, and concentrated under reduced pressure to form an extract. Obtain extractum 380g. The extract is dissolved in pure methanol with a weight ratio of 1.6 times, and then mixed with 400 g of 90 mesh thick silica gel, and 2.4 kg of 180 mesh silica gel is packed into a column for silica gel column chromatography, and the volume ratio is 1:0, 20:1, 9:1, 8:2, 7:3, 6:4, 1:1, 1:2 chloroform-acetone gradient elution, TLC monitoring and merging the same parts to obtain 8 parts, wherein the volume ratio is 8: The chloroform-acetone eluting part of 2 uses Waters SFC80Q supercritical fluid preparative chromatographic separation, is mobile phase (90 / 10%, mass ratio) with carbon dioxide / methanol, Silica2-EP (10mm * 150mm, 5 μ m) preparative column ...
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