Method for extracting orientin from bamboo leaf
A technology of orientin and bamboo leaves, which is applied in the field of natural product separation, to achieve the effects of enhanced separation effect, good separation effect and short cycle
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Embodiment 1
[0026] Take 2kg of bamboo leaf crushed material, add 18L lime water (control the pH at 8-9) and 30g borax, mix well, heat to 75℃ for 3 hours, filter, and extract the residue again according to the above conditions, combine the filtrate and the filtrate Add 8% hydrochloric acid solution to adjust the pH to 5, pass the 200 mesh polyamide chromatographic column adsorption, elution with 3BV 65% ethanol solution, concentrate the eluate, and then extract with n-butanol 3 times, evaporate Butanol, mix well with 40g ODS silica gel with a particle size of 50μm, dry it, dry it on a silica gel column, use ethanol-water-acetic acid mixed solution gradient elution, pressure control flow rate 30ml / min, thin layer monitoring, collect The oxaloside fraction was concentrated to recover ethanol, and vacuum dried to obtain 6.8 g of product with a content of 97.1%.
Embodiment 2
[0028] Take 2kg of bamboo leaf crushed material, add 20L lime water (control the pH at 8-9) and 25g borax, mix well, heat to 70℃ for 3 hours, filter, and extract the filter residue again according to the above conditions. Combine the filtrate and the filtrate Add 5% hydrochloric acid solution to adjust the pH to 4.5, pass the 200 mesh polyamide chromatographic column adsorption, elution with 2BV 70% ethanol solution, concentrate the eluate, and then extract twice with n-butanol, evaporate and dry Butanol, mix well with 35g ODS silica gel with a particle size of 50μm, dry, apply dry method to silica gel column, elution with ethanol-water-acetic acid solution gradient, pressure control flow rate 50ml / min, thin layer monitoring, collect Orientia The glycoside fraction was concentrated to recover ethanol, and vacuum dried to obtain 7.4 g of product with a content of 97.5%.
Embodiment 3
[0030] Take 5kg of bamboo leaf crushed material, add 60L lime water (control pH 8-9) and 60g borax, mix well, heat to 65℃ for 3 hours, filter, add 50L lime water (control pH 8-9) and 50g the filter residue After the borax is evenly mixed, heat to 60°C for extraction for 2 hours, filter, combine the filtrate, add 8% hydrochloric acid solution to the filtrate to adjust the pH to 5, pass through a 300 mesh polyamide chromatography column for adsorption, use 2.5BV of 75% ethanol The solution is eluted, the eluate is concentrated, and then extracted 3 times with n-butanol. The n-butanol is evaporated and mixed with 70g of ODS silica gel with a particle size of 50μm, dried, and dried on a silica gel column with ethanol-water- Gradient elution of acetic acid mixed solution, pressure control flow rate 40ml / min, thin layer monitoring, collect orientin fractions, concentrate to recover ethanol, vacuum dry to obtain product 16.2g, content 95.3%.
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