Chromone compound as well as preparation method and application thereof
A technology of chromone compounds and compounds, applied in the field of tobacco chemistry
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[0023] The chromone compound C of the present invention 14 h 13 o 4 The preparation method comprises extract extraction, silica gel column chromatography, high-pressure liquid chromatography separation steps, specifically comprises:
[0024] A. Extraction of extract: Take tobacco rhizomes, grind them to 20-40 mesh, use 90-99% ethanol to ultrasonically extract 3-5 times, each time for 30-60 min, combine the extracts, filter, and concentrate under reduced pressure to form extract;
[0025] B. Silica gel column chromatography: use 4~5 times the amount of 160~200 mesh silica gel dry method to pack the extract for silica gel column chromatography; carry out gradient with chloroform-acetone solution with a volume ratio of 1:0~1:2 elute, pool identical fractions, collect eluate from each fraction and concentrate;
[0026] C. High-pressure liquid chromatography separation: the 8:2 part of the eluent in step B is further separated and purified by high-pressure liquid chromatography ...
Embodiment 1
[0035] The tobacco rhizome samples were from Yuxi, Yunnan, and the variety was Yunyan-85. Sampling 2.2 kg of tobacco rhizomes was crushed to 30 mesh, extracted 3 times with 95% ethanol and ultrasonically for 30 min each time, the extracts were combined, filtered, concentrated under reduced pressure to obtain an extract, and 105.4 g of extract was obtained. The extract was dissolved in pure methanol with a weight ratio of 1.5 times, and then mixed with 160 g of 100-mesh crude silica gel, and 1.0 kg of 160-mesh silica gel was packed into a column for silica gel column chromatography, and the volume ratio was 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 8 The chloroform-acetone elution part of :2 was separated by Agilent 1100 semi-preparative high-performance liquid chromatography, with 50% methanol as mobile phase, Zorbax SB-C18 (21.2 × 250 mm, 5 μm) preparat...
Embodiment 2
[0037] The tobacco rhizome samples were from Yuxi, Yunnan, and the variety was Yunyan-85. Sampling 3.5 kg of tobacco rhizomes was crushed to 40 mesh, extracted 5 times with 90% ethanol by ultrasonic, each extraction was 45 min, the extracts were combined, filtered, concentrated under reduced pressure to obtain an extract, and 215 g of extract was obtained. The extract was dissolved with 3 times the amount of pure methanol by weight, and then mixed with 350 g of 80-mesh crude silica gel, and 1.5 kg of 200-mesh silica gel was packed into a column for silica gel column chromatography, and the volume ratio was 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 8 The chloroform-acetone elution part of :2 was separated by Agilent 1100 semi-preparative high-performance liquid chromatography, with 50% methanol as mobile phase, Zorbax SB-C18 (21.2 × 250 mm, 5 μm) prepara...
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