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A method for isolating and preparing anthocyanin monomer from Lycium barbarum fruit

A technology for medlar and anthocyanin is applied in the field of separation and preparation of anthocyanin monomers, which can solve the problems of volatile chemical reagents, harm to operators, long separation time and the like, and achieves the advantages of short separation time, safe operation and improved separation effect. Effect

Active Publication Date: 2015-09-30
CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, high-speed countercurrent chromatography (HSCCC) is mainly used for the separation of anthocyanins. The limitation is that there are fewer chromatographic peaks, poor separation effect, and long separation time; while high-speed countercurrent chromatography is used to separate anthocyanins. Due to the high polarity of anthocyanins, it is necessary to add methyl tert-butyl ether and n-butanol in the separation system. These two highly polar reagents are difficult to remove in the subsequent concentration process, and even if they can be removed, high temperatures are required. will cause loss of anthocyanins
Furthermore, high-speed countercurrent chromatography is an open separation system, and the chemical reagents, especially methyl tert-butyl ether, are easy to volatilize, causing harm to operators and easy to pollute the environment.

Method used

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  • A method for isolating and preparing anthocyanin monomer from Lycium barbarum fruit
  • A method for isolating and preparing anthocyanin monomer from Lycium barbarum fruit
  • A method for isolating and preparing anthocyanin monomer from Lycium barbarum fruit

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Example 1 A method for isolating and preparing anthocyanin monomer from Lycium barbarum fruit, comprising the following steps:

[0030] (1) Raw material pretreatment: select the black fruit wolfberry fruit to remove impurities, wash it with water, and wash away the floating soil on the surface to obtain the processed black fruit wolfberry fruit.

[0031] (2) Prepare a methanol solution with a volume concentration of 2% formic acid: mix 200 mL of formic acid and 9800 mL of methanol evenly.

[0032] (3) Add the formic acid methanol solution obtained in step (2) to the fruit of Lycium ruthenicum fruit, and carry out normal temperature leaching at a ratio of 1 g: 1 mL at room temperature in the dark, and the extraction frequency is 1 time, 12 h each time, and combined to obtain the extract.

[0033] (4) Remove insoluble matter, protein, and polysaccharides from the extract with filter paper to obtain a filtrate, which is vacuum-evaporated on a rotary evaporator at 40...

Embodiment 2

[0042] Example 2 A method for isolating and preparing anthocyanin monomer from Lycium barbarum fruit, comprising the following steps:

[0043] ⑴Raw material pretreatment is the same as Example 1 .

[0044] ⑵Preparation volume concentration is 2% methanol solution of formic acid Example 1 .

[0045] (3) Add the formic acid methanol solution obtained in step (2) to the fruit of Lycium ruthenicum fruit, carry out normal temperature leaching at a ratio of 1 g: 5mL at room temperature in the dark, the extraction times are 3 times, each time for 24 h, combined to obtain extract.

[0046] (4) Remove insoluble matter, protein, and polysaccharides from the extract with filter paper to obtain a filtrate. The filtrate is vacuum evaporated and concentrated to a paste on a rotary evaporator at 50° C. to obtain anthocyanin extract from Lycium barbarum, and methanol is recovered.

[0047] ⑸The treatment of macroporous adsorption resin is the same as Example 1 .

[0048] (6) Re...

Embodiment 3

[0055] Example 3 A method for isolating and preparing anthocyanin monomer from Lycium barbarum fruit, comprising the following steps:

[0056] ⑴Raw material pretreatment is the same as Example 1 .

[0057] ⑵Preparation volume concentration is 2% methanol solution of formic acid Example 1 .

[0058] (3) Add the formic acid methanol solution obtained in step (2) to the fruit of Lycium ruthenicum fruit, and carry out normal temperature leaching at a ratio of 1 g: 3 mL at room temperature in the dark, and the extraction times are 2 times, each time for 18 h, and combined to obtain extract.

[0059] (4) Remove insoluble matter, protein, and polysaccharides from the extract with filter paper to obtain a filtrate, which is vacuum-evaporated on a rotary evaporator at 45°C and concentrated to a paste to obtain anthocyanin extract from Lycium ruthenicum, and recover methanol.

[0060] ⑸The treatment of macroporous adsorption resin is the same as Example 1 .

[0061] (6) R...

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Abstract

The invention relates to a method for separating an anthocyanins monomer from lycium ruthenicum fruits. The method comprises the following steps: (1) pretreating raw materials: removing impurities from lycium ruthenicum fruits, washing the lycium ruthenicum fruits with water to obtain the treated lycium ruthenicum fruits; (2) preparing a formic acid-methanol solution at a volume concentration of 2%; (3) adding the formic acid-methanol solution into the lycium ruthenicum fruits for extraction at room temperature to obtain an extract; (4) filtering, and concentrating the extract by evaporating to obtain an lycium ruthenicum anthocyanins extract; (5) treating macroporous adsorption resin; (6) redissolving the lycium ruthenicum anthocyanins extract, applying the redissolved lycium ruthenicum anthocyanins extract to the treated macroporous adsorption resin, and collecting effluent; (7) concentrating the effluent under reduced pressure to obtain crude anthocyanins; (8) injecting the crude anthocyanins into a high-performance semipreparative chromatographic column, and separating to obtain the anthocyanins monomer with the purity of higher than or equal to 90%; concentrating the anthocyanins monomer under reduced pressure, and performing freeze drying in vacuum to constant weight to obtain finished anthocyanins monomer. The method is good in separating effect, short in time consumption and low in cost.

Description

technical field [0001] The invention relates to a method for separating and preparing anthocyanin monomers, in particular to a method for separating and preparing anthocyanin monomers from black wolfberry fruit. Background technique [0002] Black Goji Berry ( Lycium ruthenicum Murray) is a perennial shrub belonging to the family Solanaceae (Solanaceae) and has significant physiological activity. Tibetan medicine classics "Jingzhu Materia Medica" and "Four Medical Classics" all record: black fruit wolfberry is sweet, calm in nature, clears heart heat, and is used to treat heart fever, heart disease, irregular menstruation, and menopause. "Uyghur Medicine Chronicle" records: black fruit wolfberry fruit can treat diseases such as urethral calculus, ringworm and scabies, bleeding gums, etc., and it is used as nourishing and strong, improving eyesight and antihypertensive medicine among the people. Lycium barbarum is rich in anthocyanins (Anthocyanins) natural pigments, anthoc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/065C07H1/08C09B61/00
Inventor 索有瑞胡娜丁晨旭张秋龙
Owner CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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