Coumarin compound and preparation method and application thereof
A technology of coumarins and compounds, applied in the field of tobacco chemistry
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
preparation example Construction
[0023] Preparation method C of coumarin compounds of the present invention 17 h 14 o 5 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 rhizome, crush it to 20-40 mesh, use 90-99% ethanol to ultrasonically extract 3-5 times, each time for 30-60min, combine the extracts, filter, and concentrate under reduced pressure to form extract;
[0025] B. Silica gel column chromatography: the extract is packed with 160~200 mesh silica gel dry method with a weight ratio of 2~3 times for silica gel column chromatography; chloroform-acetone solution with a volume ratio of 1:0~1:2 Perform gradient elution, pool the same fractions, collect and concentrate the eluate from each fraction;
[0026] C. High-pressure liquid chromatography separation: the 7:3 part of the eluent in step B is further separated and purified by high-pressu...
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 minutes each time, the extracts were combined, filtered, and concentrated under reduced pressure to obtain an extract, 105.4 g of extract was obtained. The extract was dissolved in pure methanol with a weight ratio of 2.5 times, and then mixed with 150 g of 100-mesh crude silica gel, and 1.5 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 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, Zorbax SB-C18 (21.2 × 250 mm, 5 μm) prepa...
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 time for 45 minutes, the extracts were combined, filtered, concentrated under reduced pressure to obtain an extract, and 215 g of extract was obtained. The extract was dissolved in pure methanol with a weight ratio of 2.0 times, and then mixed with 300 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 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, Zorbax SB-C18 (21.2 × 250 mm, 5 μm) preparative...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More