A compound with antibacterial effect, its preparation method and its use in cigarettes
A compound, tobacco technology, applied in the field of phytochemistry to achieve the effects of good durability, easy availability of raw materials and large biological yield
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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 the benzopyran lactone compound of the present invention comprises the following steps:
[0047] 20kg of tobacco stem bark was sampled and pulverized and extracted with 95wt% methanol aqueous solution for 5 times, each extraction was 24h, the extracts were combined, filtered, and concentrated under reduced pressure to obtain an extract of 1.2kg. The weight ratio of the methanol aqueous solution to the tobacco stem bark was 3.
[0048] The obtained extract was subjected to molecular distillation and separation, and the 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, mixed with 120g of 100-mesh thick silica gel, and 0.6kg of 160-mesh silica gel was packed into a column for silica gel column chroma...
Embodiment 2
[0053] The tobacco sample comes from Dali, Yunnan, the variety is Yunyan-300, 35kg of tobacco stem bark is sampled and chopped, extracted with 95wt% ethanol aqueous solution for 4 times, each extraction is 48h, the extracts are combined, filtered, and concentrated under reduced pressure to form an extract. Got extract 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 the fractions at 170-210° C. were collected to obtain 234 g of distillation products.
[0055] After dissolving the distillation product obtained by molecular distillation with 2.0 times of pure methanol by weight, mix the sample with 250g of 80-mesh thick silica gel, and pack 1.2kg of 200-mesh silica gel column to carry out 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 solution for gradient elution, TLC monitoring to com...
Embodiment 3
[0059] Tobacco samples come from Kunming, Yunnan, the variety is Yunyan-300, 50kg of tobacco stem bark was sampled and pulverized, extracted 3 times with 75wt% acetone aqueous solution by ultrasonic, each extraction was 72h, the extracts were combined, filtered, and concentrated under reduced pressure into extract , get the extract 3.92kg. The weight ratio of the acetone aqueous solution to the tobacco stem bark was 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 chromatography was performed on silica gel column 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 and combining the same polar fractions to ...
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