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A kind of method for separating chiral eriodictyol in peanut shell and its application

A technology for peanut shells and eriodictyol is applied in the directions of organic chemistry methods, chemical instruments and methods, separation of optically active compounds, etc., which can solve the problems of high price and limited application of chiral columns, and improve the comprehensive utilization rate and dosage. The effect of less and shorter component analysis time

Active Publication Date: 2022-05-06
QIQIHAR UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, studies have reported that many enantiomer separation methods of chiral drugs, such as high performance liquid chromatography (HPLC), gas chromatography (GC), thin layer chromatography (TLC), supercritical fluid chromatography (SFC), etc. respective disadvantages
The chiral columns used in HPLC and GC are expensive, and in most cases, a specific chiral column can only analyze a certain type of substance, and its application is often limited

Method used

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  • A kind of method for separating chiral eriodictyol in peanut shell and its application
  • A kind of method for separating chiral eriodictyol in peanut shell and its application
  • A kind of method for separating chiral eriodictyol in peanut shell and its application

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specific Embodiment approach 1

[0019] Specific implementation mode one: what this implementation mode records is a kind of method for separating chiral eriodictyol in peanut shells, and the described method steps are as follows:

[0020] Step 1: Processing of peanut shells: remove impurities, wash, and dry until the surface is dry or there is no clear water on the surface, then crush and pass through a 40-100 mesh sieve;

[0021] Step 2: Add 10-20 times the weight of 40-90wt.% ethanol to the peanut shell powder for reflux extraction for 1-3 times, 1-2h / time, and combine the extracts;

[0022] Step 3: Concentrate the extract from step 2 and use acetic acid to adjust the pH to be weakly acidic, add deionized water to dilute, pass through a macroporous resin column, quickly elute with water to remove impurities, then add 60~90wt.% ethanol to elute and collect The eluate was concentrated to obtain the purified product;

[0023] Step 4: Prepare ammonium acetate buffer solution with a pH of 8.0~9.0, add MAH-β-CD...

specific Embodiment approach 2

[0025] Specific embodiment two: a method for separating chiral eriodictyol in peanut shells described in specific embodiment one, in step two, 15 times the weight of 60wt.% ethanol is added to the peanut shell powder for reflux extraction twice , 1~2 h / time, combine the extracts; in step 3, concentrate the extract in step 2 to 60% of the original volume, add acetic acid to adjust the pH to 5.5, add deionized water to dilute 2~4 times, pass 0.10 ~0.20 g medicinal material / mL resin column, quickly eluted with water to remove impurities, then added 60~90wt.% ethanol for elution, collected the eluate, concentrated to 20~50% of the original volume, and obtained the purified product.

specific Embodiment approach 3

[0026] Embodiment 3: The method for separating chiral eriodictyol in peanut shells described in Embodiment 1, in step 3, the macroporous resin column is HPD300, HPD500 or D101.

[0027] Embodiment 4: A method for separating chiral eriodictyol in peanut shells described in Embodiment 1. In step 4, the synthesis method of the MAH-β-CD is to weigh maleic anhydride dissolved In dimethylformamide (DMF), add β-CD with stirring at room temperature, and react in a constant temperature water bath at 80°C±2°C for 8-12 hours. After the reaction, the product is cooled to room temperature, and the product is precipitated with chloroform. Wash thoroughly with acetone, drain with a suction filter bottle, dry in vacuum, and set aside.

[0028] Specific embodiment five: a method for separating chiral eriodictyol in peanut shells described in specific embodiment four, the synthetic method of the MAH-β-CD is to take 5.0 g maleic anhydride and dissolve it in 30 Add 5.6 g β-CD to mL DMF with stir...

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Abstract

A method for separating chiral eriodictyol, a flavonoid compound in peanut shells, and its application, which belong to the technical field of plant extraction and separation medicines. The steps of the method are as follows: treatment of peanut shells; reflux extraction of peanut shell powder with ethanol for 1 to 3 times to obtain a concentrated solution; concentrating the extract, adjusting the pH, diluting, passing through a macroporous resin column, and eluting with water, Elute with ethanol and collect the eluent, concentrate to obtain a purified product; prepare ammonium acetate, adjust the pH of the system, add MAH-β-CD to the prepared buffer solution to mix, dissolve, and constant volume to obtain a running buffer; The substance was filtered with a filter membrane, and the capillary electrophoresis method was used to separate the two eriodictyol enantiomers of the R configuration body 2R eriodictyol and the S configuration body 2S eriodictyol. The invention has the advantages of improving the comprehensive utilization rate of peanut shells, simple extraction and separation operation, short analysis time and high efficiency, choosing a suitable chiral selector, high separation efficiency, less chiral selector consumption, and high cost performance , the resolution reached 4.17.

Description

technical field [0001] The invention belongs to the technical field of extracting and separating medicines from plants, and in particular relates to a method for separating chiral eriodictyol, a flavonoid compound in peanut shells, and an application thereof. Background technique [0002] Peanuts are derived from the dried pods of peanuts, an annual herbaceous plant of the family Fabaceae, and the peanut shell is the shell of the pods. my country's peanut shells are rich in resources and low in price, and have broad application prospects in the fields of medicine, industry, agriculture, and health food. Peanut shell is a Chinese herbal medicine in the folk, which can treat asthma, phlegm, high blood pressure and so on. The flavonoids in peanut shells have various pharmacological activities such as lowering blood pressure, lowering blood fat, dilating coronary arteries, anti-oxidation, antitussive, expectorant and asthma, anti-bacterial and anti-inflammatory, enhancing immun...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D311/32C07D311/40C07D311/30A61P9/00A61P11/00
CPCA61P9/00A61P11/00C07B57/00C07D311/30C07D311/32C07D311/40C07B2200/07
Inventor 徐蕾高立娣陈林刘树仁王宁
Owner QIQIHAR UNIVERSITY
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