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A kind of mechanochemical extraction method for preparing naphthalene pyrone crude extract from iron-clad gold

A naphthopyrone and mechanochemical technology, which is applied in the field of mechanochemical extraction for the preparation of naphthalene pyrone crude extract, can solve the problems of reducing the extraction rate, and achieve the effects of improving the extraction yield, low cost, and rapid extraction process

Active Publication Date: 2020-12-01
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

During mechanochemical assisted extraction, the physical and chemical properties of the target compound can also be used to selectively add solid reagents. Different additives will cause different physical and chemical conditions during ball milling, thereby changing the dissolution rate of the target compound in the extraction solvent; Alkaline conditions may also change the structure of the target compound, thereby reducing the extraction rate. Therefore, it is necessary to optimize the additives during ball milling extraction (Wu Feifei, Zhao Liangzhong, Xu Yongping. Study on the extraction of citrus peel essential oil assisted by shear-auxiliary interaction technology[J]. food safety Journal of All Quality Inspection , 2016(8): 3246-3252.)

Method used

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  • A kind of mechanochemical extraction method for preparing naphthalene pyrone crude extract from iron-clad gold
  • A kind of mechanochemical extraction method for preparing naphthalene pyrone crude extract from iron-clad gold

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] The iron-clad gold produced in Guangzhou, Guangdong is crushed and passed through an 80-mesh sieve to obtain iron-clad gold powder with a mesh size greater than 80 mesh. Add 0.30 g of the iron-clad gold powder into the stainless steel ball milling tank, add 10 stainless steel balls with a diameter of 8 mm (the filling rate of the ball mill is 5.4%), the ball milling time is 15 min, and the ball milling speed is 200 rpm.

[0039] Weigh 0.10 g of the ball-milled powder and mix it with ethanol aqueous solution (V ethanol: V water = 60 / 40) according to the ratio of solid to liquid at 1:50 (the unit of solid to liquid ratio is g / mL), and then place it in a water bath at 40°C for ultrasonication Extracted for 45 min (ultrasonic frequency 100HZ), filtered, and the filtrate was removed by rotary evaporation to obtain 11 mg of naphthalene pyrone crude extract.

[0040] Take 10.59 mg of the crude naphthalene pyrone extract obtained above and dissolve it in 1 mL of methanol, then ...

Embodiment 2

[0043] The iron-clad gold produced in Guangzhou, Guangdong is crushed and passed through an 80-mesh sieve to obtain iron-clad gold powder with a mesh size greater than 80 mesh. Add 0.31 g of the iron-clad gold powder into the stainless steel ball mill tank, add 15 stainless steel ball milling beads with a diameter of 8 mm (the ball milling filling rate is 8.0%), the ball milling time is 15 min, and the ball milling speed is 200 rpm.

[0044] Weighed 0.10 g of the ball-milled powder, and the rest of the subsequent ultrasonic extraction conditions and ultra-high performance liquid chromatography conditions were the same as in Example 1 to obtain 11 mg of crude naphthalene pyrone extract. Calculation of the yield of rhodofusarmycin-6-O-α-L-rhamnosyl-(1-6)-O-β-D-glucopyranoside in the crude extract was 141.9% (mg / g) .

[0045] Comparing Example 2 and Example 1, it can be seen that when 15 stainless steel ball milling beads are added (the filling rate of the ball mill reaches 8.0%...

Embodiment 3

[0047] The iron-clad gold produced in Guangzhou, Guangdong is crushed and passed through an 80-mesh sieve to obtain iron-clad gold powder with a mesh size greater than 80 mesh. Add 0.30 g of the iron-clad gold powder into the stainless steel ball mill tank, add 20 stainless steel ball milling beads with a diameter of 8 mm (the filling rate of the ball mill is 10.7%), the ball milling time is 15 min, and the ball milling speed is 200 rpm.

[0048] Weigh 0.10 g of the ball-milled powder, and the rest of the subsequent ultrasonic extraction conditions and ultra-high performance liquid chromatography conditions are the same as in Example 1 to obtain 10 mg of crude naphthalene pyrone extract. Calculate the yield of rhodofusarmycin-6-O-α-L-rhamnosyl-(1-6)-O-β-D-glucopyranoside in the crude extract as 138.5% (mg / g) .

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Abstract

The invention discloses a mechanochemical extraction method for preparing a naphthopyranone crude extract from berchemia lineata, which comprises the following steps: drying, crushing and sieving a berchemia lineata raw material, putting the obtained powder into a ball mill for ball milling, mixing the ball-milled powder with an extraction solvent, then putting the mixture into a water bath at a temperature between 20 and 50 DEG C for ultrasonic extraction for 15 to 60 minutes, then cooling to room temperature, filtering, and obtaining a yellow brown naphthopyranone crude extract after the solvent is removed through rotating evaporation of filtrate; dissolving the crude extract with methanol, standing, collecting supernatant, sieving by using a PTFE membrane of 0.22 micrometer; and analyzing by using an UPLC method, the yield of the crude extract is obtained by using the content of the main component of the naphthopyranone crude extract which is naphthopyranone-6-O-alpha-L-rhamnosyl-(1-6)-O-beta-D glucopyranoside. According to the invention, the method is low in cost; the process for preparing and extracting the crude extract of the naphthopyranone is rapid and efficient; and technical basis can be provided for the comprehensive utilization of the medicinal resources of the berchemia lineata.

Description

technical field [0001] The invention relates to the technical field of extraction of active ingredients of botanical medicines, in particular to a mechanochemical extraction method for preparing naphthalene pyrone crude extract from iron-clad gold. Background technique [0002] Iron clad gold ( Berchemia lineate(L.)DC. ) for Rhamnaceae ( Rhamnaceae ) The dried roots or stems of the genus Goucatecha. Because the peg hairs on the root of the plant are brown like iron, and the xylem is yellow like gold, so it is called iron clad gold. Iron-clad Jinyuan plants are mainly distributed in Guangdong, Guangxi, Fujian and other provinces in my country, and are also found in South Korea, Vietnam, India, Japan and other countries. [0003] Iron-coated gold is an important folk medicinal resource in our country. It can be used as a prescription to treat patients' diseases (CN102166275A), and can also be used together with bee pollen and honey to make health food to improve human immu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/04C07H1/08
CPCC07H1/08C07H17/04
Inventor 梁现蕊蒋秀丽
Owner ZHEJIANG UNIV OF TECH
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