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Method for synergistically extracting and preparing active components in ramulus mori (folium mori) by aid of solid acid reinforcement thermal reaction

A technology of hydrothermal reaction and active ingredients, applied in separation methods, chemical instruments and methods, medical preparations containing active ingredients, etc., can solve the problems of large amount of petroleum ether and ethanol, increased safety production costs, and long time consumption. To achieve the effect of simple operation, environmental protection and increased safety

Active Publication Date: 2018-10-09
CHONGQING TECH & BUSINESS UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The existing invention patent CN201610569828.8 published on November 2, 2016 is "a method for extracting tea polysaccharides by hydrothermal method". The solution makes tea polysaccharides quickly and completely dissolved to extract tea polysaccharides, which can effectively extract tea polysaccharides, but there are still the following deficiencies: (1) only relying on the pyrolysis of hydrothermal reaction to destroy the complex and dense network structure of plant cell walls; (2) This invention only extracts one substance, tea polysaccharide; (3) water is used as an extractant, and other substances such as tea polyphenols, amino acids and proteins in tea cannot be fully dissolved, and the maximum utilization of resources cannot be realized
Although the chemical composition and content of the active substance extracted by this method are stable, there are still the following shortcomings: (1) The entire extraction process takes a long time; (2) The amount of petroleum ether and ethanol is relatively large, 6.0L; (3) The flammability, explosiveness and chronic toxicity of petroleum ether pose a threat to human health and the environment, increasing the cost of safety production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Raw material pretreatment

[0023] The picked fresh mulberry leaves were dried in an oven at 60°C for 5 hours, and the dried mulberry leaves were pulverized into powder by a pulverizer, sieved with 80 mesh, put into sealed bags, and set aside.

[0024] (2) Solid acid enhanced hydrothermal reaction treatment of raw materials

[0025] After step (1) is completed, first weigh 2g of pretreated mulberry leaf powder into the hydrothermal reaction kettle, then add 5‰ of the mass of mulberry leaves (g), that is, 0.01g of phosphotungstic heteropolyacid, and finally The ratio of water ethanol volume (ml) to mulberry leaf powder mass (g) is 9:1, measure 18ml of absolute ethanol and pour it into the hydrothermal reaction kettle. Then, the reaction kettle was put into an oven at 180° C. to react for 110 minutes.

[0026] (3) Analysis and detection of active ingredients

[0027] After step (2) is completed, take out the reaction kettle and cool it to room temperature, pour it ...

Embodiment 2

[0031] A method for synergistically extracting active ingredients in mulberry branches (leaves) by solid acid-enhanced hydrothermal reaction, the same as in Example 1, wherein:

[0032] In step (1), the oven temperature is 50°C, the drying time is 6 hours, and the sieve is 60 mesh.

[0033]In step (2), the mass (g) of phosphotungstic heteropolyacid is 4‰ of the mass (g) of mulberry leaf, the ratio of absolute ethanol (ml) to the mass (g) of mulberry leaf powder is 7:1, and the reaction The temperature is 170° C., and the reaction time is 130 minutes.

[0034] In step (3), the rotation speed is 2000r / min, and the centrifugation time is 20min. The ratio of acetonitrile (ml) to water (ml) was 35:65, the temperature was 30°C, the injection volume was 5 μL, the flow rate was 0.8ml / min, and the peak area (mAu*s) was 19738.334.

[0035] In step (4), when the vacuum pressure is 0.4Mpa and the temperature is 80°C, the ratio of the mass (g) of the mulberry leaf extract product to the ...

Embodiment 3

[0037] A method for synergistically extracting active ingredients in mulberry branches (leaves) by solid acid-enhanced hydrothermal reaction, the same as in Example 1, wherein:

[0038] In step (1), the oven temperature is 70°C, the drying time is 4 hours, and the sieve is 100 mesh.

[0039] In step (2), the mass (g) of phosphotungstic heteropolyacid is 6‰ of the mass (g) of mulberry leaf, the ratio of absolute ethanol (ml) to the mass (g) of mulberry leaf powder is 11:1, and the reaction The temperature is 190° C., and the reaction time is 90 minutes.

[0040] In step (3), the rotational speed is 3000r / min, the centrifugation time is 15min; the ratio of acetonitrile (ml) to water (ml) is 50:50, the temperature is 40°C, the injection volume is 20μL, the flow rate is 1ml / min, the peak The area (mAu*s) is 18549.287.

[0041] In step (4), when the vacuum pressure is 0.6Mpa and the temperature is 100°C, the mass (g) of the mulberry leaf extract product: the volume (ml) ratio of ...

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PUM

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Abstract

The invention discloses a method for synergistically extracting and preparing active components in ramulus mori (folium mori) by the aid of solid acid reinforcement thermal reaction, belongs to the technical field of extraction of active components in natural products, and particularly relates to methods for regulating and controlling phosphotungstic heteropoly acid catalysis and hydrothermal reaction. The method has the advantages that efficient pharmacological effects can be realized by the ramulus mori (folium mori), the ramulus mori (folium mori) is already widely applied to the industriesof food, medicines, skincare products and the like, the pharmacological effects realized by the ramulus mori (folium mori) are closely related to the active components in the ramulus mori (folium mori), and accordingly improvement of the extraction efficiency for the active components in the ramulus mori (folium mori) and increase of the recycling value of the active component have research significance and realistic economic values; the shortcomings of existing methods for extracting existing active components in existing ramulus mori (folium mori) can be pertinently overcome by the aid of the method for extracting the active components by means of phosphotungstic heteropoly acid catalysis-hydrothermal reaction regulation and control, plant tissues can be synergistically degraded by phosphotungstic heteropoly acid catalysis and the hydrothermal reaction, hydrogen bonds between celluloses and hemicelluloses and compact structures of cell walls can be destructed, mass transfer barrierbetween the cell walls and intercellular substances can be reduced, the active components can be advantageously sufficiently dissolved out, the method includes few and simple extraction conditions andoperation steps and is little in environmental pollution and low in production energy consumption and cost, and the like.

Description

technical field [0001] The invention belongs to the technical field of extracting active components from natural products, and in particular relates to a method for catalyzing phosphotungstic heteropolyacid and controlling hydrothermal reaction. Background technique [0002] Mulberry leaves are rich in multivitamins (100g mulberry leaf dry product contains 670μg retinol, 7440μg carotene, V B1 0.59 mg, V B2 1.35 mg, V C 31.6mg) and amino acids (contains as many as 18 kinds, accounting for 10.10% of the dry weight, of which the content of essential amino acids accounts for 3.281%, the first limiting amino acid lysine of plant protein accounts for 0.454%, and the semi-essential amino acids account for 1.843%); mulberry leaves The extract has good hypoglycemic, hypolipidemic, anti-inflammatory, anti-aging, anti-filariasis and anti-tumor effects. The mulberry branch contains active ingredients such as polyhydroxyalkaloids, flavonoids, mulberry leaf polysaccharides, phytosterol...

Claims

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Application Information

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IPC IPC(8): A61K36/605B01D11/02A61K127/00
CPCA61K36/605A61K2236/15A61K2236/17A61K2236/33B01D11/02B01D11/028
Inventor 王星敏王露王莹谭双詹力
Owner CHONGQING TECH & BUSINESS UNIV
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