Compound with antibacterial effect, preparation method thereof and application thereof in cigarettes
A compound, tobacco technology, applied in the field of phytochemistry, achieves good antibacterial activity, simple preparation and operation process, and high purity
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Embodiment 1
[0045] The tobacco samples were from Yuxi, Yunnan, and the variety was Yunyan-300.
[0046] The preparation method of benzopyranolactone compound of the present invention comprises the following steps:
[0047] Sampling 20 kg of tobacco stem bark, crushing and extracting 5 times with 95 wt% methanol aqueous solution for 24 hours each time, combining the extracts, filtering, and concentrating under reduced pressure to obtain 1.2 kg of extract. The weight ratio of the aqueous methanol solution to the tobacco stem bark is 3.
[0048] The obtained extract was subjected to molecular distillation and separation, and fractions at 170-210°C were collected to obtain 112 g of distillation products.
[0049] The distillation product obtained by molecular distillation was dissolved in pure methanol with a weight ratio of 2.0 times, and then mixed with 120 g of 100-mesh crude silica gel, and 0.6 kg of 160-mesh silica gel was packed into a column for silica gel column chromatography. The v...
Embodiment 2
[0053] The tobacco sample comes from Dali, Yunnan, and the variety is Yunyan-300. The tobacco stem bark is sampled 35kg and chopped, extracted 4 times with 95wt% ethanol aqueous solution, each extraction is 48h, the extracts are combined, filtered, and concentrated under reduced pressure to form an extract. Obtain extractum 2.63kg. The weight ratio of the ethanol aqueous solution to the tobacco stem bark is 2.
[0054] The obtained extract was subjected to molecular distillation and separation, and fractions at 170-210°C were collected to obtain 234 g of a distillation product.
[0055] The distillation product obtained by molecular distillation was dissolved in pure methanol with a weight ratio of 2.0 times, and then mixed with 250 g of 80-mesh crude silica gel, and 1.2 kg of 200-mesh silica gel was packed into a column for silica gel column chromatography. The volume ratio was 1:0, 20:1, 9:1, 8:2, 7:3, 6:4, 1:1, 1:2 chloroform-acetone solution for gradient elution, TLC moni...
Embodiment 3
[0059] The tobacco sample comes from Kunming, Yunnan, and the variety is Yunyan-300. Take 50kg of tobacco stem bark and grind it, and use 75wt% acetone aqueous solution to extract 3 times with ultrasound, each time for 72 hours. The extracts are combined, filtered, and concentrated under reduced pressure to form an extract. , to obtain extract 3.92kg. The weight ratio of the acetone aqueous solution to the tobacco stem bark is 4.
[0060] The extract was separated by molecular distillation, and the fractions at 170-210°C were collected to obtain 438g of distillation products. The part obtained by molecular distillation was dissolved in pure methanol with a weight ratio of 1.6 times, and then mixed with 400g of 90-mesh crude silica gel, and 2.4kg of 180-mesh Silica gel column was packed for silica gel column chromatography, using a chloroform-acetone gradient with a volume ratio of 1:0, 20:1, 9:1, 8:2, 7:3, 6:4, 1:1, 1:2 Elution, TLC monitoring Merge the same polar fractions t...
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