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Method for simultaneously extracting tricin, eoixol and vanillic acid from imperata cylindrical by subcritical water

A technology of subcritical water and alfalfa, applied in the separation/purification of carboxylic acid compounds, organic chemistry, etc., can solve the problems of low extraction rate, low content of active ingredients, viscous leachate, etc., and achieve high extraction rate and low price , the effect of easy separation

Inactive Publication Date: 2016-12-21
SHANDONG ANALYSIS & TEST CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the methods for extracting active ingredients in Imperatae mainly include solvent extraction and water decoction. Among them, the solvent extraction method is more toxic, pollutes, and easily leaves organic solvents, which takes a long time and has a low extraction rate; Solubility is limited, so the water decoction method extracts less active ingredients and complex ingredients. In addition to active ingredients, some fat-soluble substances and impurities are also leached out, which is not conducive to refining, and the leachate is viscous and difficult to filter. It is effective in post-processing It is difficult to separate the components

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] The method for simultaneously extracting alfalfalin, coixin and vanillic acid in Imperatae imperina with subcritical water comprises the following steps:

[0051] ① Pulverize the Imperata imperata sample and pass it through a 20-90 mesh sieve to obtain Imperata imperata powder;

[0052] ②Put 150kg of deionized water and 10kg of the impermanae powder obtained in step ① into a subcritical water extraction device for extraction for 90 minutes to obtain an extract; the extraction pressure is 1MPa, and the extraction temperature is 120°C;

[0053] ③ Add ethanol to the extract obtained in step ② to obtain a mixed solution, put the mixed solution in a centrifuge tube of a centrifuge, centrifuge at a speed of 3000 rpm for 5 minutes, remove the centrifuge tube, and obtain a supernatant and sediment ; The volume ratio of the extract and ethanol obtained in step ② is 1:1;

[0054] ④ The supernatant obtained in step ③ was distilled under reduced pressure to obtain alfalfalin, coix...

Embodiment 2

[0056] A method for simultaneously extracting alfalfalin, coixin and vanillic acid in Imperata coixa with subcritical water, comprising the following steps:

[0057] ① Pulverize the Imperata imperata sample and pass through a 90-mesh sieve to obtain the Imperata imperata powder;

[0058] ②Put 250kg of deionized water and 10kg of the impermanae powder obtained in step ① into a subcritical water extraction device for extraction for 30 minutes to obtain an extract; the extraction pressure is 3MPa, and the extraction temperature is 200°C;

[0059] ③ Add ethanol to the extract obtained in step ② to obtain a mixed solution, put the mixed solution in a centrifuge tube of a centrifuge, centrifuge at a speed of 5000 rpm for 15 minutes, remove the centrifuge tube, and obtain a supernatant and sediment ; The volume ratio of the extract and ethanol obtained in step ② is 1:2;

[0060] ④ The supernatant obtained in step ③ was distilled under reduced pressure to obtain alfalfalin, coixin an...

Embodiment 3

[0062] A method for simultaneously extracting alfalfalin, coixin and vanillic acid in Imperata coixa with subcritical water, comprising the following steps:

[0063] ① Pulverize the Imperata imperata sample and pass through a 40-mesh sieve to obtain the Imperata imperata powder;

[0064] ②Put 180kg of deionized water and 10kg of the impermanae powder obtained in step ① into a subcritical water extraction device for extraction for 50 minutes to obtain an extract; the extraction pressure is 2.5MPa, and the extraction temperature is 140°C;

[0065] ③ Add ethanol to the extract obtained in step ② to obtain a mixed solution, put the mixed solution in a centrifuge tube of a centrifuge, centrifuge at a speed of 3500 rpm for 8 minutes, remove the centrifuge tube, and obtain a supernatant and sediment ; The volume ratio of the extract obtained in step ② to ethanol is 1:1.5;

[0066] ④ The supernatant obtained in step ③ was distilled under reduced pressure to obtain alfalfalin, coixin ...

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Abstract

The invention discloses a method for simultaneously extracting tricin, eoixol and vanillic acid from imperata cylindrical by subcritical water, comprising the following steps: crushing an imperata cylindrical sample to obtain imperata cylindrical powder of 20-90 meshes; putting deionized water and the imperata cylindrical powder into a subcritical water extraction apparatus and extracting for 30-90 min so as to obtain an extracting solution; adding ethanol into the extracting solution to obtain mixed liquor, and centrifuging to obtain a supernatant and sediment; and carrying out reduced pressure distillation on the supernatant to obtain tricin, eoixol and vanillic acid products. The extraction solvent subcritical water is a typical green solvent, is nontoxic and harmless, and is low-cost and environment friendly. The active components tricin, eoixol and vanillic acid extracted from imperata cylindrical by the use of subcritical water have few impurity, are nontoxic and pollution-free, have no residue, and are low-cost and environment friendly. According to the method for simultaneously extracting tricin, eoixol and vanillic acid from imperata cylindrical by subcritical water, extraction efficiency is high, and other impurity components are easy to separate.

Description

technical field [0001] The invention relates to the technical field, in particular to a method for simultaneously extracting alfalfalin, coixin and vanillic acid from impermanae imperata with subcritical water. Background technique [0002] The active ingredients of Imperatae mainly include triterpenoids, sugars, lactones, organic acids, coumarins, etc., and contain various elements such as potassium, iron, and calcium. It is often used as a single ingredient or a compound to treat stranguria hematuria and chyle. Urine, acute and chronic glomerulonephritis, edema, icteric and anicteric hepatitis, etc. In recent years, it has been found that the rhizome of Imperatae has the functions of lowering blood pressure, enhancing immunity and anti-tumor. What play these roles is the effective medicinal ingredients in Imperatae Rhizoma Imperatae. How to obtain these medicinal ingredients in Imperata Rhizoma Imperatae more scientifically and accurately is an important development direc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/30C07D311/40C07D263/58C07C51/42C07C65/21
CPCC07C51/42C07D263/58C07D311/30C07D311/40C07C65/21
Inventor 程燕王晓赵汝松王英鹏吴丹
Owner SHANDONG ANALYSIS & TEST CENT
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