Method for extracting and separating 1-deoxynojirimycin from mulberry leaves

A technology of deoxynojirimycin and mulberry leaves, which is applied in the direction of organic chemistry, can solve the problems of difficult separation and recycling of mixed solvents, high production costs, long process, etc., and achieve improved solvent dissolution efficiency, low equipment requirements, and safe operation Effect

Active Publication Date: 2011-09-21
HUNAN HUACHENG BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disclosed method of CN10134586A is to take the initial extract of mulberry leaves as raw material (containing more than 40% of DNJ), after dissolving in water, directly pass through cationic resin, then use eluent to elute and collect step by step, and finally obtain the product with relatively high purity through repeated recrystallization. High product, because the mixed solvent used in recrystallization is not easy to separate and recycle, so the production cost is high
The method disclosed in CN101671294A not only separates and obtains the DNJ prod

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Raw material pretreatment: crush 100 kg of dried mulberry leaves, and more than 80% of them pass through 24 meshes;

[0024] (2) Enzymolysis: Add 1000 kg of water to the crushed mulberry leaf raw material, heat to 55°C, then add 150g of combined enzyme (5:1 cellulose: pectinase, w / w), enzymolysis After 12 h, filter to obtain the raw material for enzymolysis;

[0025] (3) Alkali-alcohol extraction: Add 600 kg of 60% ethanol solution (containing 10 g of calcium hydroxide) to the enzymatic hydrolysis raw material, stir for 30 min, then heat to 80°C for reflux extraction twice, each extraction for 2 h, Cool to about 5°C, filter to obtain the extract;

[0026] (4) Acid dissolution and ultrafiltration: Concentrate the extract under low pressure at 60°C. When the feed liquid is released, the concentrated liquid weighs 52 kg, cool to 7°C, and stand for 12 hours to collect the precipitate, then add 36.5 kg of 1% Sulfuric acid solution (v / v), stirred to make it fully dissol...

Embodiment 2

[0031] The difference between this example and Example 1 is that the weight of the combined enzyme added is 150 g (cellulose: pectinase is 1:1), the amount of acid added is 28 kg, and the final mulberry leaf extract is 38.7 g. The yield was 0.038%, and the content of 1-deoxynojirimycin was 95.7%.

Embodiment 3

[0033] The difference between this example and Example 2 is that the diameter-to-height ratio of the resin column is 20:1, the ratio of methanol to saturated ammonia water in the mixed solution is 5:1 (v / v), and the final mulberry leaf extract obtained is 38.1 g. 0.038%, 1-deoxynojirimycin content is 96.5%.

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Abstract

The invention discloses a method for extracting and separating 1-deoxynojirimycin from mulberry leaves, which comprises the following steps of: pretreating a raw material, namely crushing a mulberry leaf raw material; performing enzymolysis; extracting by using alkali-alcohol, cooling, filtering to obtain extracting solution; concentrating, and performing acid dissolution and ultrafiltration to obtain ultrafiltrate; removing impurities by using cation resin, namely making the obtained ultrafiltrate pass through the cation resin, eluting by using ammonia alcohol solution, collecting eluent; making the eluent pass through macroporous adsorption resin, eluting by using ethanol solution, and collecting eluent; and concentrating the eluent, adding a methanol-saturated ammonia water mixed solvent, regulating temperature, cooling for crystallization to obtain crystals, and drying. A product with the purity of over 95 percent can be extracted and separated from the mulberry leaf raw material,and the 1-deoxynojirimycin is effectively separated; requirements on equipment are low, and the operation is safe; the process is simple, the used solvents can be recycled, and the production cost isreduced; and the used solvents are low in toxicity, environment-friendly and safe.

Description

technical field [0001] The invention relates to the technical field of separation of effective components of traditional Chinese medicines, in particular to a method for extracting and separating 1-deoxynojirimycin from mulberry leaves. Background technique [0002] Mulberry leaves are the dry leaves of the Moraceae plant mulberry, which are sweet in taste and cold in nature. They are mostly planted in my country and can be used as medicine. With the development of science and technology, people are doing more and more research on mulberry leaves. In recent years, scholars have found that there is a special hypoglycemic substance in mulberry leaves, namely 1-deoxynojirimycin (DNJ) , and the number of diabetic patients in my country and the world is increasing day by day, so 1-deoxynojirimycin in mulberry leaves is more and more favored by researchers. [0003] It is generally believed that the mechanism of 1-deoxynojirimycin for lowering blood sugar is: DNJ is an inhibitor o...

Claims

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Application Information

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IPC IPC(8): C07D211/46
Inventor 黄华学唐方华刘永胜
Owner HUNAN HUACHENG BIOTECH
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