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Mechanochemical extraction method for preparing hydrolysable-tannin crude extract from trapa Sp. pericarps

A technology of hydrolyzing tannins and mechanochemistry, which is applied in chemical instruments and methods, organic chemistry, preparation of sugar derivatives, etc., can solve the problems of long extraction time, noise pollution, long heating time, etc., to improve extraction yield and reduce Waste of resources, fast and efficient results

Active Publication Date: 2019-07-12
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The heating and reflux method solvent can be recycled, but this method takes a long time to heat and is not suitable for the extraction of components that are easily damaged by heat
The enzymatic hydrolysis method adds a specific pH buffer and enzyme to it for enzymatic hydrolysis, and then lyophilizes the product to obtain the product, but this method also has problems such as long extraction time and high cost
The ultrasonic method can quickly release the active ingredients through the means of breaking the wall, so as to achieve the purpose of increasing the yield, but there are problems of high energy consumption and noise pollution.

Method used

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  • Mechanochemical extraction method for preparing hydrolysable-tannin crude extract from trapa Sp. pericarps
  • Mechanochemical extraction method for preparing hydrolysable-tannin crude extract from trapa Sp. pericarps
  • Mechanochemical extraction method for preparing hydrolysable-tannin crude extract from trapa Sp. pericarps

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] The water chestnut shell produced in Shantou, Guangdong is crushed and passed through an 80-mesh sieve to obtain water chestnut shell powder with a mesh size greater than 80 mesh. Add 1.01 g of the water chestnut shell powder in the stainless steel ball mill tank, add 20 stainless steel ball mill beads with a diameter of 10 mm (ball milling filling rate 20.9%) and 0.15 g auxiliary agent (the auxiliary agent is sodium bicarbonate), and the ball milling time is 5 min , the milling speed is 100 rpm.

[0039] Weigh 0.51 g of the ball-milled powder, mix the ball-milled powder with ethanol aqueous solution (V ethanol: V water = 60 / 40) according to the material-liquid ratio of 1:40 (solid-liquid ratio unit g / mL), and then place Ultrasonic extraction was performed in a water bath at 40°C for 30 min, and the ultrasonic dispersion was cooled to room temperature, adjusted to pH = 3 with 1 mol / L hydrochloric acid solution, and left to stand for 4 h.

[0040] Then, the pH-adjusted ...

Embodiment 2

[0043] The water chestnut shell produced in Suqian, Jiangsu is crushed and passed through an 80-mesh sieve to obtain water chestnut shell powder with a mesh size greater than 80 mesh. Add 1.03 g of the water chestnut shell powder in the stainless steel ball mill tank, add 20 stainless steel ball mill beads with a diameter of 10 mm (ball mill filling rate 20.9%) and 0.15 g auxiliary agent (the auxiliary agent is sodium bicarbonate), and the ball mill time is 5 min , the milling speed is 100 rpm.

[0044] Weigh 0.53 g of the powder after ball milling, and the remaining follow-up operating conditions are the same as in Example 1 to obtain 0.12 g of the crude extract of the ethyl acetate layer, and calculate 1,2,3,6-tetra-O-galloyl-β-D-glucose The yield was 1.9%.

Embodiment 3

[0046] The water chestnut shell produced in Jiaxing, Zhejiang is crushed and passed through an 80-mesh sieve to obtain water chestnut shell powder with a mesh size greater than 80 mesh. Add 1.04 g of the water chestnut shell powder in the stainless steel ball mill tank, add 20 stainless steel ball mill beads with a diameter of 10 mm (ball mill filling rate 20.9%) and 0.15 g auxiliary agent (the auxiliary agent is sodium bicarbonate), and the ball mill time is 5 min , the milling speed is 100 rpm.

[0047] Weigh 0.51 g of the powder after ball milling, and the remaining follow-up operating conditions are the same as in Example 1 to obtain 0.11 g of the crude extract of the ethyl acetate layer, and calculate 1,2,3,6-tetra-O-galloyl-β-D-glucose The yield was 1.8%.

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Abstract

The invention discloses a mechanochemical extraction method for preparing a hydrolysable-tannin crude extract from trapa Sp. pericarps. The method comprises the steps of drying, smashing and sieving the trapa Sp. pericarps to obtain trapa Sp. pericarps powder, putting the trapa Sp. pericarps powder into a ball mill for ball milling treatment, mixing an extraction solvent with the trapa Sp. pericarps powder which is subjected to ball milling treatment, carrying out ultrasonic extraction, and adjusting the pH value of a dispersion solution which is subjected to ultrasonic extraction to be 2-4; performing standing for 3-5 hours, putting the dispersion solution into a centrifuge for centrifugal separation, conducting filtering, carrying out reduced-pressure distillation on a filtrate to removethe solvent in order to obtain a crude extract, and dissolving the crude extract in water again; performing extraction through petroleum ether, using ethyl acetate for extracting a raffinate phase, making the ethyl acetate phase subjected to rotary evaporation to remove the solvent, and then obtaining a hydrolysable-tannin crude extract product. According to the method, a mechanochemical auxiliary ultrasonic extraction technology is adopted for extracting the hydrolysable-tannin crude extract in the trapa Sp. pericarps, correspondingly the resource waste of the trapa Sp. pericarps is reducedon the premise of not causing further environmental pollution, the waste is turned into treasure, and the application field of the method is expanded.

Description

technical field [0001] The invention relates to a mechanochemical extraction method for preparing hydrolyzable tannin crude extract from water chestnut shells. Background technique [0002] Water chestnut shell ( Trapa Sp. Pericarps) for Lingke ( Trapaceae ) The dry shell of the rhomboid plant. Water chestnut is an annual aquatic plant, which can be seen in rivers, lakes, and ponds. It is widely distributed in provinces such as Zhejiang, Shandong, Jiangsu, Hubei, and Taiwan in my country. On a global scale, it is more distributed in Asia, Europe, and Africa. widely. There are many kinds of water chestnuts, such as two-cornered water chestnut, four-cornered water chestnut, no-cornered water chestnut, and hill-cornered water chestnut in terms of shape, and two colors of cyan and red in terms of color. [0003] According to the records of "Chinese Medicine Sea", the water chestnut shell is slightly bitter, astringent, cool in nature, enters the lung, spleen, and intestine, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H13/08C07H1/08
CPCC07H1/08C07H13/08
Inventor 梁现蕊江燕
Owner ZHEJIANG UNIV OF TECH
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