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Method for extracting DNJ in mulberry leaves through hydrothermal acid control and alcohol extraction

A mulberry leaf and hydrothermal technology, applied in organic chemistry, climate sustainability, chemical industry and other directions, can solve the problem of increasing equipment maintenance costs, hydrochloric acid environmental treatment costs, increasing production equipment purchase costs and production energy consumption, increasing production costs and increasing production costs. Environmental governance costs and other issues, to achieve the effect of realizing the utilization of mulberry leaves, improving the utilization rate of mulberry leaves, and reducing the impact of equipment and environmental pollution

Active Publication Date: 2022-05-27
CHONGQING TECH & BUSINESS UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method of this patent has the following disadvantages: (1) Dilute hydrochloric acid is used to treat mulberry leaves, and hydrochloric acid (pH value = 1) is used in the production process, which is easy to cause corrosion to production equipment, increase equipment maintenance costs and environmental treatment costs for hydrochloric acid
(2) The treatment of mulberry leaves is successively soaked in hydrochloric acid for 1-2 hours, and then treated with an ultrasonic generator for 1-2 hours. The use of an ultrasonic generator requires special equipment, high technical requirements, and high energy consumption, which increases the purchase cost of production equipment and production energy consumption. , thereby increasing production costs
(3) Using 75% ethanol solution as the extraction solution, the purity of the organic solvent used is higher than the actual production, and the use of membrane filtration requires more consumables for production, which increases production costs and environmental governance costs

Method used

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  • Method for extracting DNJ in mulberry leaves through hydrothermal acid control and alcohol extraction
  • Method for extracting DNJ in mulberry leaves through hydrothermal acid control and alcohol extraction
  • Method for extracting DNJ in mulberry leaves through hydrothermal acid control and alcohol extraction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The concrete steps of a kind of hydrothermal acid-controlled alcohol extraction of DNJ in mulberry leaves are as follows:

[0020] (1) Raw material pretreatment

[0021] Using mulberry leaves (including fresh mulberry leaves, waste mulberry leaves, and leftovers from the processing of mulberry leaves) as raw materials. First wash the raw materials with water, then place them in an oven at 100 °C for 60 minutes, then grind them through a pulverizer and pass through a 60-mesh sieve. processed raw material.

[0022] (2) Hydrothermal acid catalytic treatment of mulberry leaves

[0023] After the step (1) is completed, first weigh 2 g of the pretreated raw material obtained in the step (1) and place it in the hydrothermal reaction kettle, and then according to the ratio of the mass (g) of the raw material: the volume (ml) of the acid solution is 1 Add citric acid and ethanol aqueous solution in a ratio of 20:20, seal the reaction kettle after stirring, then put the hydrot...

Embodiment 2

[0027] A kind of DNJ method in mulberry leaf extraction with hydrothermal acid control alcohol, with embodiment 1, wherein:

[0028] In step (1), the oven temperature is 110°C, the oven time is 30 minutes, and the mesh number of mulberry leaves is 80 meshes.

[0029] In step (2), the ratio of the mass (g) of the raw material: the volume (ml) of the acid solution is 1:10, the reaction temperature is 80 °C, the reaction time is 100 min, the centrifugal speed is 2000 r / min, and the yield of DNJ is It is 0.54mg / g, the mass fraction of citric acid is 0.75%, and the volume fraction of ethanol solution is 60%.

[0030] In step (3), the retention time was 10.235 min, the purity of DNJ monomer was 41.0%, the mobile phase: methanol: water (30:70), the injection volume: 8 mL, and the flow rate: 15 mL / min.

Embodiment 3

[0032] A kind of DNJ method in mulberry leaf extraction with hydrothermal acid control alcohol, with embodiment 1, wherein:

[0033] In step (1), the oven temperature is 85°C, the oven time is 90 minutes, and the number of mulberry leaves is 100 meshes.

[0034] In step (2), the ratio of the mass (g) of the raw material: the volume (ml) of the acid solution is 1:15, the reaction temperature is 70 °C, the reaction time is 50 min, the centrifugation time is 10 min, and the DNJ yield is 0.89 mg / g, the mass fraction of citric acid was 0.5%, and the volume fraction of ethanol solution was 70%.

[0035] In step (3), the retention time was 15.893 min, the purity of DNJ monomer was 14.92%, mobile phase: methanol: water (20:80), injection volume: 5 mL, flow rate: 10 mL / min.

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Abstract

The invention discloses a method for extracting DNJ (1-deoxynojirimycin) in mulberry leaves through hydrothermal acid control alcohol extraction, and belongs to the technical field of extraction of active ingredients in natural products. According to the method, mulberry leaves are used as raw materials, and DNJ is obtained through three steps of raw material pretreatment, synchronous treatment of the mulberry leaves through hydrothermal acid catalysis and preparation of a DNJ (1-deoxynojirimycin) product. And a theoretical basis is provided for mulberry leaf medicinal resource development. The method can be widely applied to extraction of DNJ in mulberry leaves, can also be used for extraction of high-value natural products in biomass, and has important practical significance on improvement of the utilization value of mulberry leaves.

Description

technical field [0001] The invention belongs to the technical field of DNJ extraction from mulberry leaves, and in particular relates to a method for leaching DNJ from mulberry leaves with alcohol controlled by citric acid under a hydrothermal reaction. Background technique [0002] Mulberry leaves are rich in mulberry leaf polysaccharides, alkaloids, flavonoids and other natural active substances. Among them, DNJ, namely 1-deoxynojirimycin, is an alkaloid, easily soluble in water, ethanol and methanol, and has hypoglycemic, anti-tumor, anti-tumor properties. It is an important raw material for the synthesis of drugs such as hypoglycemic, tumor metastasis inhibition, and anti-HIV virus. At present, the extraction methods of DNJ mainly include water extraction, ethanol extraction, ultrasonic extraction, and enzyme extraction, which have problems such as low yield, environmental damage by organic solvents, high energy consumption, and long extraction time. Therefore, finding ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/46
CPCC07D211/46Y02P20/10
Inventor 王星敏何孟阳唐付杰张杰陈泓岐
Owner CHONGQING TECH & BUSINESS UNIV
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