A kind of naphthalene formaldehyde compound with antibacterial activity, its preparation method and its use in cigarette paper
A compound, naphthalene formaldehyde technology, applied in the field of natural product chemistry
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Embodiment 1
[0037] Embodiment 1: the preparation of compound
[0038] Throat hair samples come from Yulong Snow Mountain in Lijiang, Yunnan. Sampling 2.0 kg of dried trichomes was crushed to 35 mesh, extracted 5 times with 95wt% methanol for 30 hours each time, combined the extracts, filtered, concentrated under reduced pressure to obtain 108 g of extract. The extract is dissolved in pure methanol with a weight ratio of 2.0 times, and then mixed with 130 g of 100-mesh silica gel, and 0.8 kg of 160-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 48wt% methanol as mobile phase, Zorbax SB-C18 (21.2×250mm, 5 μm) preparative column as stationary ph...
Embodiment 2
[0039] Embodiment 2: the preparation of compound
[0040] Throat hair sample comes from Haba Snow Mountain in Lijiang, Yunnan. The dried throat hair sample is crushed to 30 mesh, 3.6kg is sampled, extracted 4 times with 95wt% ethanol, each extraction is 48h, the extracts are combined, filtered, and concentrated under reduced pressure Become extractum, obtain extractum 259g. After dissolving the extract with 2.0 times the amount of pure methanol by weight, mix the sample with 280g of 80-mesh silica gel, pack 1.4kg of 200-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 48wt% methanol as mobile phase, Zorbax SB-C18 (21.2×250mm, 5 μm) pre...
Embodiment 3
[0041] Embodiment 3: the preparation of compound
[0042] The sample of laryngeal hair flower comes from Laojun Mountain in Lijiang. Take 5.5kg of the sample of laryngeal hair flower and crush it, extract it with 75% acetone and ultrasonically extract it for 3 times, and extract for 72 hours each time. Cream 392g. The extract is dissolved in pure methanol with a weight ratio of 1.6 times, and then mixed with 450 g of 90 mesh thick silica gel, and 2.8 kg of 180 mesh silica gel is packed 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 7: The chloroform-acetone elution part of 3 was separated by Agilent 1100 semi-preparative high performance liquid chromatography, with 48wt% methanol as mobile phase, Zorbax SB-C18 (21.2×250mm, 5 μm) preparative column as stationary phase, flow rate was 20ml / min, the ...
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