A kind of deoxynojirimycin extraction method

A deoxynojirimycin and extraction method technology, applied in the field of biological extraction, can solve the problems of inability to obtain pure product, difficult to handle, low safety, etc., and achieve the effects of easy mastery of production technology, realization of recycling, process energy saving and environmental protection

Inactive Publication Date: 2011-12-14
SOUTHWEST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method requires that the "total alkaloids" of the raw material contain more than 40% of deoxynojirimycin, and the step-by-step eluents are alcohol solutions of different concentrations, and the recrystallization is a mixed solution of methanol and acetone; a large amount of detection work is required during the step-by-step elution And the collection of pure products, the operation is more troublesome, and the mixed solvent of recrystallization is difficult to handle
[0013] Chinese patent technology (200810236144.1) reported a compound extraction process for the co-production of mulberry leaf flavonoids, polysaccharides and alkaloids, but did not separate and obtain pure deoxynojirimycin
This process requires the use of ultrafiltration technology, ethanol distributed elution, and the collection of the target eluent requires continuous detection of the effluent components, etc. The operation is complicated; the energy consumption is high
[0020] So far, from the existing literature and patented technology, the extraction of pure deoxynojirimycin or the use of too much organic solvent, especially the use of chloroform, lead to low safety; or require multiple concentrations and high energy consumption ; or need to use too many steps, or need to detect and collect target components step by step, because deoxynojirimycin has no ultraviolet absorption, detection is more troublesome, complex operation, difficult to control industrial production; or can not get pure products, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] (1) Soak 1 kg of mulberry branches in 10 liters of 0.1% (w / v) sulfuric acid solution at room temperature for 48 hours; filter to obtain an extract (about 9 liters).

[0053] (2) 9 liters of the extract was stirred and adsorbed with 0.9 liters of pretreated 732 cation exchange resin, then, the resin was washed with 0.9 liters of water, and then washed with 0.9 liters of 2mol / L ammonia water. About 0.9 liters of ammonia eluate was obtained.

[0054] (3) After 0.9 liters of ammonia eluate was concentrated twice by reverse osmosis (about 0.45 liters of concentrated solution), ammonia was recovered by distillation to obtain intermediate A (about 10 grams); the recovered ammonia water was used for the elution of (2).

[0055] (4) Intermediate A was dissolved in water and prepared into a 20% solution (about 50 ml), added 0.01% hydrochloric acid (w / v) at 100°C for 1 hour under reflux conversion, and put on a 50 ml Superose gel chromatography column, Elute with water; collect e...

Embodiment 2

[0059] (1) Soak 1Kg of mulberry leaves in 2 liters of 5% (w / v) hydrochloric acid solution at 100°C for 0.1 hour, filter to obtain the extract (about 1 liter); then use 2 liters of 0.5% (w / v) hydrochloric acid solution for the residue Soak in hydrochloric acid solution at 100°C for 0.1 hour, filter to obtain extract (about 1 liter); soak the residue in 2 liters of water at 100°C for 0.1 hour, filter to obtain extract (about 1 liter). The three extracts were combined to obtain about 3 liters of extract.

[0060] (2) 3 liters of extract was stirred and adsorbed with 3 liters of pretreated 001 cation exchange resin, then, the resin was washed with 30 liters of water, and then washed with 30 liters of 0.05mol / L ammonia water. About 30 liters of ammonia eluent was obtained.

[0061] (3) After 30 liters of ammonia water eluate was concentrated 20 times by reverse osmosis (about 1.5 liters of concentrated solution), ammonia was recovered by distillation to obtain intermediate A (abou...

Embodiment 3

[0066] (1) Soak 1Kg of Morus alba cortex with 5 liters of 1% (w / v) sulfuric acid solution at 60°C for 5 hours, filter to obtain the extract (about 3 liters); use 5 liters of 1% (w / v) for the residue The sulfuric acid solution was soaked at 60°C for 5 hours, and filtered to obtain an extract (about 4 liters). The secondary extracts were combined to obtain about 7 liters of extracts.

[0067] (2) 7 liters of extract was stirred and adsorbed with 3.5 liters of pretreated D151 cation exchange resin, then, the resin was washed with 7 liters of water, and then washed with 7 liters of 0.5mol / L ammonia water. About 7 liters of ammonia eluate was obtained.

[0068] (3) After the 7 liters of ammonia water eluate was concentrated by reverse osmosis 10 times (about 0.7 liters of concentrated solution), the ammonia was recovered by distillation to obtain intermediate A (about 30 grams); the recovered ammonia water was used for the elution of (2).

[0069] (4) Intermediate A was dissolved...

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PUM

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Abstract

The invention discloses a method for extracting a deoxynojirimycin monomer. The method comprises the following steps of: soaking a mulberry raw material in acidic aqueous solution, and extracting for 1 to 3 times; adsorbing extracting solution on a cation exchange resin, washing, and eluting by using ammonia water; performing reverse osmosis pre-concentration on eluent, recovering ammonia, dissolving an intermediate in a hydrophilic solvent, performing catalytic conversion, allowing the solution to pass through a gel chromatographic column, and eluting the hydrophilic solvent; recovering the solvent, dissolving in a mixed solvent, allowing the mixed solvent to pass through the chromatographic column, and eluting the mixed solvent; and recovering the mixed solution to obtain pure deoxynojirimycin products. The method is low in energy consumption and environment-friendly, and the pure deoxynojirimycin products with various purity grades of 10 percent, 50 percent, 99 percent and the like.

Description

technical field [0001] The invention relates to biological extraction technology, in particular to a method for extracting deoxynojirimycin monomer. Background technique [0002] 1-deoxynojirimycin (1-deoxynojirimycin, DNJ) is a polar N-containing compound, its chemical name is 3, 4, 5-trihydroxy-2-hydroxymethyltetrahydropyridine, and its molecular formula is C 6 h 13 NO 4 , with a relative molecular mass of 163. DNJ has a strong inhibitory effect on α-glucosidase, and is an effective ingredient for lowering blood sugar and treating diabetes [1~4] , and antiviral [5] , anti-tumor metastasis [6] and other pharmacological effects. In recent years, scholars at home and abroad have conducted a lot of research and exploration on the source of DNJ, the synthesis mechanism in vivo and chemical synthesis methods, hoping to find a stable, efficient and economical way to obtain DNJ [7] . [0003] Li Yuliang [8] reported a method for extracting deoxynojirimycin from mulberry l...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/46
Inventor 李学刚张波叶小利
Owner SOUTHWEST UNIV
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