Preparation method and application of a kind of benzolactone compound in tobacco
A technology of benzolides and compounds, applied in the fields of tobacco, application, and treatment of tobacco, etc., to achieve the effect of improving oral moisturization, simple structure, and increasing fineness
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Embodiment 1
[0030] Preparation of benzolide compound C 12 h 12 o 4 , including extracting extract, silica gel column chromatography, and high-pressure liquid chromatography separation, specifically adopting the following steps:
[0031] Step (1), extraction of extract: take tobacco leaves and pulverize them, use high-concentration methanol (w%: 90%) or high-concentration ethanol (w%: 95%) or high-concentration acetone (w%: 75%) as the extraction solvent, Extraction solvent: Tobacco (weight ratio) = 3:1, soak for 54 hours, extract 4 times, combine extracts, filter and concentrate to obtain extract.
[0032] Step (2), silica gel column chromatography: after dissolving the extract obtained in step (1) with 3 times the amount of pure methanol, pure ethanol or pure acetone, use 80-100 mesh silica gel with 2.5 times the weight of the extract Mix the sample, and at the same time, carry out silica gel column chromatography with a 250-mesh silica gel dry-packed column whose weight is 2.5 times ...
Embodiment 2
[0037] The tobacco samples were from Yuxi, Yunnan, and the variety was Yuxi K326. Sampling 2.0 kg of tobacco and pulverizing it with 95% methanol soaking and extracting for 5 times, each extraction for 24 hours, the weight ratio of extraction solvent:tobacco leaves=2:1, the extracts were combined, filtered, and concentrated under reduced pressure to obtain extractum 105g . After dissolving the extract with 2.0 times the amount of pure methanol, mix the sample with 120 g of 100 mesh thick silica gel, pack 0.6 kg of 160 mesh silica gel into a column, and perform silica gel column chromatography, using a volume ratio of 1:0, 20:1, 9:1, 8:2, 7:3, 6:4, 1:1, 1:2 chloroform-acetone gradient elution, TLC monitoring The same parts were combined and concentrated to obtain 8 parts, of which The part obtained by elution and concentration with chloroform-acetone with a volume ratio of 7:3 was separated by Agilent 1100 semi-preparative high-performance liquid chromatography, with 35% metha...
Embodiment 3
[0040] The tobacco sample comes from Dali, Yunnan, and the variety is Yunyan 200. The tobacco sample 3.5kg is cut into small pieces, soaked and extracted with 95% ethanol for 4 times, each extraction is 48h, the extraction solvent:tobacco leaf weight ratio=4:1, the extract Combined, filtered, and concentrated under reduced pressure to form an extract, 250 g of extract was obtained. After dissolving the extract with 2.0 times its weight of pure methanol, mix the sample with 250g of 80-mesh silica gel, pack 1kg of 200-mesh silica gel into a column, and perform silica gel column chromatography. The volume ratio is 1:0, 20 :1, 9:1, 8:27:3, 6:4, 1:1, 1:2 chloroform-acetone gradient elution, TLC monitoring The same fractions were combined and concentrated to obtain 8 fractions, of which the volume The part obtained by elution and concentration with chloroform-acetone with a ratio of 7:3 was separated by Agilent 1100 semi-preparative high-performance liquid chromatography, with 35% m...
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