Diphenol compound in tobacco rhizome and preparation method and application thereof
A compound, biphenol technology, applied in the field of tobacco chemistry, can solve problems such as unreported
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Embodiment 1
[0027] ---The preparation method of the compound includes extract extraction, silica gel column chromatography, and high pressure liquid chromatography separation steps, specifically including the following steps:
[0028] 1. Extraction of extract: take tobacco sample, crush it to 30 mesh, extract it with 95% methanol ultrasonically for 4 times, each time for 45 minutes, combine the extracts, filter, and concentrate under reduced pressure to form extract;
[0029] 2. Silica gel column chromatography: the extract is dry-packed with 180 mesh silica gel column with a weight ratio of 2.5 times for silica gel column chromatography; the volume ratio is 1:0, 20:1, 9:1, 8:2, 7:3, 6:4, 1:1, and 1:2 chloroform-acetone solutions were used for gradient elution, the same fractions were combined, and the eluents of each fraction were collected and concentrated;
[0030] 3. High-pressure liquid chromatography separation: the 7:3 part of the eluent in step 2 is further separated and purified ...
Embodiment 2
[0036] The tobacco samples were from Yuxi, Yunnan, and the variety was Yunyan 87. Sampling 2.0 kg of tobacco rhizomes was crushed to 30 mesh, extracted 3 times with 95% methanol by ultrasonic, each time for 30 min, the extracts were combined, filtered, concentrated under reduced pressure to obtain extract, 72.6 g of extract was obtained. After dissolving the extract with 2.5 times the amount of pure methanol by weight, mix the sample with 120g of 100-mesh silica gel, pack 1.5kg of 160-mesh silica gel into a column for silica gel column chromatography, and use 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 and merging the same parts to obtain 8 parts, wherein the volume ratio is 7: The chloroform-acetone eluted part of 3 was separated by Agilent 1100 semi-preparative high-performance liquid chromatography, with 45% methanol as mobile phase, Zorbax SB-C18 (21.2×250mm, 5 μm) preparative column as stationary phase, and...
Embodiment 3
[0038]Tobacco samples are from Dali, Yunnan, and the variety is Yunyan 87. 3.2 kg of tobacco rhizomes are sampled and crushed to 40 meshes, extracted 5 times with 90% methanol by ultrasonic, each time for 45 minutes, the extracts are combined, filtered, and concentrated under reduced pressure to form an extract. Ointment, get extractum 126g. The extract is dissolved in pure methanol with a weight ratio of 2.0 times, and then mixed with 300 g of 80-mesh silica gel, and 1.5 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 7: The chloroform-acetone eluted part of 3 was separated by Agilent 1100 semi-preparative high-performance liquid chromatography, with 45% methanol as mobile phase, Zorbax SB-C18 (21.2×250mm, 5 μm) preparative column as stationary phase, an...
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