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Method for extracting 1-deoxynojirimycin and resveratrol from mulberry leaf

A technology of resveratrol and mulberry leaves, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problem of easy loss of 1-deoxynojirimycin and resveratrol, high production conditions, Problems such as long flocculation and sedimentation time are achieved to alleviate the large demand, ensure follow-up resources, and make planting easy

Inactive Publication Date: 2012-02-15
广州湘喜生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since 1-deoxynojirimycin and resveratrol are mainly used in the pharmaceutical and food industries, the 1-deoxynojirimycin and resveratrol products extracted by these patented methods are harmful to human health; in addition, although in Chinese patent 200910192542.2 There is no introduction of toxic reagents for separation and purification, and the use of flocculants for flocculation and precipitation takes a long time, and 1-deoxynojirimycin and resveratrol are easily lost during this process, which is not conducive to improving their yields. Furthermore, the process used Complicated, demanding production conditions, low yield, not conducive to reducing production costs

Method used

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  • Method for extracting 1-deoxynojirimycin and resveratrol from mulberry leaf
  • Method for extracting 1-deoxynojirimycin and resveratrol from mulberry leaf
  • Method for extracting 1-deoxynojirimycin and resveratrol from mulberry leaf

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Crush and dry 100kg of mulberry leaves, add 700L of water, heat and reflux at 86°C for 2 hours, filter the extract twice through three layers of gauze, filter through a ceramic membrane, concentrate under reduced pressure to 100L, add 50kg of granular activated carbon for decolorization for 30min, and the solution after decolorization Use KLFC-150 macroporous adsorption resin for separation, first use pure water to elute impurities, then use 30% ethanol to elute, collect ethanol eluate, concentrate under reduced pressure to 50L, slowly lower the temperature to room temperature for 24h to obtain 205g DNJ samples.

[0037] The residue after water extraction of mulberry leaves was extracted with 500L of 70% ethanol, heated and refluxed at 80°C for 2h, filtered twice with three layers of gauze, filtered with a ceramic membrane, concentrated under reduced pressure to 60L (no ethanol smell), and then the concentrated solution was divided with 150L ethyl acetate. Extract three...

Embodiment 2

[0040] Crush and dry 200kg of mulberry leaves, add 1600L of water, heat and reflux at 86°C for 2 hours, and filter the extract twice through three layers of gauze and ceramic membrane. Use KLFC-150 macroporous adsorption resin for separation, first use pure water to elute impurities, then use 30% ethanol to elute, collect ethanol eluate, concentrate under reduced pressure to 90L, slowly lower the temperature to room temperature for 24 hours to crystallize, and obtain 421g DNJ samples.

[0041] The residue after water extraction of mulberry leaves was extracted with 1150L of 70% ethanol, heated and refluxed at 80°C for 2h, filtered twice with three layers of gauze, filtered with a ceramic membrane, concentrated under reduced pressure to 110L (no ethanol smell), and then the concentrated solution was divided with 170L ethyl acetate. Extract three times, combine the ethyl acetate layer and concentrate to 95L, add 8kg granular activated carbon to decolorize for 30min, after decolo...

Embodiment 3

[0043] Crush and dry 400kg of mulberry leaves, add 3400L of water, heat and reflux at 86°C for extraction for 2 hours, filter the extract twice through three layers of gauze and ceramic membrane, concentrate under reduced pressure to 350L, add 80kg of granular activated carbon for decolorization for 30min, and the solution after decolorization Use KLFC-150 macroporous adsorption resin for separation, first use pure water to elute impurities, then use 30% ethanol to elute, collect ethanol eluate, concentrate under reduced pressure to 160L, slowly lower the temperature to room temperature for 24 hours to obtain 830g DNJ samples.

[0044] The residue after water extraction of mulberry leaves was extracted with 2500L of 70% ethanol, heated and refluxed at 80°C for 2h, filtered twice with three layers of gauze, filtered with a ceramic membrane, concentrated under reduced pressure to 60L (no ethanol smell), and then the concentrated solution was divided with 150L ethyl acetate. Extr...

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Abstract

The invention mainly relates to a method for extracting 1-deoxynojirimycin and resveratrol from mulberry leaf, and provides a whole set of method for separating and extracting high-purity 1-deoxynojirimycin and resveratrol from mulberry leaf. By the method, the yield and purity of 1-deoxynojirimycin and resveratrol are greatly increased. The method comprises the following steps of: carrying out alcohol reflux extraction, film filtration, concentration, extraction and activated carbon decolorizing, and then controlling crystallization and recrystallization conditions to separately obtain 1-deoxynojirimycin and resveratrol pure products. The method has the advantages that: in the whole separation process, the requirements on the ambient conditions and equipments are low, the separation timeis shortest, the product purity is highest, and the comprehensive utilization rate of raw materials is highest; and moreover, the separation materials are obtained easily and inexpensive, the separation operation process is simple and easy to control, crystallization and recrystallization are adopted, the purification efficiency is high, used reagents are nontoxic and safe, and the cost is low.

Description

Technical field: [0001] The invention relates to a technology for rapidly extracting and separating 1-deoxynojirimycin and resveratrol from mulberry leaves, belonging to the technical field of biological separation engineering. Background technique [0002] my country's mulberry resources and output rank first in the world, and are cultivated all over the country. At present, mulberry is cultivated as forage in most areas. After winter, the breeding of winter silkworms decreases, and a large amount of mulberry leaves are discarded. Mulberry leaves taste bitter, sweet, cold in nature, and return to the lung and liver meridian. 1-deoxynojirimycin (DNJ), resveratrol and other components in leaves, so it is of great significance to study the extraction technology of these two components in mulberry leaves. [0003] DNJ is a piperidine alkaloid, the chemical name is 3,4,5-trihydroxy-2-hydroxymethyltetrahydropyridine, and its molecular formula is C 6 h 13 NO 4 (see structural...

Claims

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Application Information

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IPC IPC(8): C07D211/46C07C39/21C07C37/84C07C37/70
Inventor 向华
Owner 广州湘喜生物科技有限公司
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