A kind of biphenol compound contained in tobacco rhizome and its preparation method and application
A compound, biphenol technology, applied in the field of tobacco chemistry, can solve the problems that have not been reported, and achieve the effect of good activity, good anti-tobacco mosaic virus activity, and simple structure
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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 elution part of 3 was separated by Agilent 1100 semi-preparative high-performance liquid chromatography, with 45% methanol as mobile phase, ZorbaxSB-C18 (21.2×250mm, 5 μm) preparative column as stationary phase, flo...
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 extraction takes 45 minutes, the extracts are combined, filtered, and concentrated under reduced pressure to obtain a 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 elution part of 3 was separated by Agilent 1100 semi-preparative high-performance liquid chromatography, with 45% methanol as mobile phase, ZorbaxSB-C18 (21.2×250mm, 5 μm) preparative column as stationary phase, fl...
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