Method for separating high-purity anthocyanin monomers from black rice

Anthocyanin, high-purity technology, applied in the direction of preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of restricting the development and utilization of anthocyanins, small output, and many impurities, so as to be suitable for large-scale production, Large sample loading and good selectivity

Active Publication Date: 2010-06-09
GUANGZHOU TRACE ELEMENTS BIOLOGICAL TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the commonly used anthocyanin separation and preparation method is solvent extraction method, which is usually extracted with acidic alcohol solution. The total anthocyanin content of the obtained crude extract is mostly between 10% and 35%, which often contains more impurities and is difficult to obtain. Its identification also limits the development and utilization of anthocyanins
At present, it has been reported to use high performance liquid chromatography (HPLC) or high-speed countercurrent chromatography to purify the crude extract to prepare anthocyanin monomers, but there are problems such as low yield and high cost.

Method used

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  • Method for separating high-purity anthocyanin monomers from black rice

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Embodiment 1

[0019] Implementation Example 1: Take 5kg of black rice, grind 300g of rice skin, mix with 3L of 60% ethanol (containing 0.1% HCl), extract 2 times at room temperature, each 4-6h; Filtrate, and the filtrate was rotary evaporated at = 42°C until there was no ethanol; degreased with petroleum ether, filtered and passed through a pre-acidified macroporous resin adsorption column at a flow rate of 1-1.5 column volume / h, and washed off with 0.01% HCl after the adsorption was completed Impurities; elute with 80% ethanol solution, the flow rate is 2-3 column volumes / h, collect the eluent and rotate evaporate at 45°C until there is no ethanol to obtain anthocyanin extraction concentrate; connect three 40g medium-pressure chromatographic columns in series, inject Sample loading, 0.1% trifluoroacetic acid aqueous solution (A) and methanol (B) were used as mobile phase gradient elution, and the absorption peaks with corresponding retention times were collected to obtain 228mg Cy-3-G and 3...

Embodiment 2

[0020] Implementation Example 2: Take 25kg of black rice, grind 1500g of rice skin, mix with 15L of 60% ethanol (containing 0.1% HCl), extract 2 times at room temperature, each 4-6h; Filtrate, and the filtrate was rotary evaporated at = 42°C until there was no ethanol; degreased with petroleum ether, filtered and passed through a pre-acidified macroporous resin adsorption column at a flow rate of 1-1.5 column volume / h, and washed off with 0.01% HCl after the adsorption was completed Impurities; elute with 80% ethanol solution, the flow rate is 2-3 column volumes / h, collect the eluent and rotate evaporate at 45°C until there is no ethanol to obtain anthocyanin extraction concentrate; use a guard column (about 12g C18 packing) and glass The separation column (400g C18 filler, 50mm×500mm) was loaded with samples, 0.1% trifluoroacetic acid aqueous solution (A) and methanol (B) were used as mobile phase gradient elution, and the corresponding retention time absorption peaks were col...

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Abstract

The invention provides a method for separating high-purity anthocyanin monomers from black rice. The method comprises the following steps of: grinding 5 to 8 percent of episperm on the outer layer of black rice and brown rice to obtain black rice pericarp, leaching anthocyanin in the black rice pericarp by acidized ethanol, and extracting and defatting petroleum ether; performing primary purification of ethanol extracts of the black rice pericarp by using macroporous resin; separating the anthocyanin in coarse extracts of the anthocyanin of the black rice pericarp by the medium pressure preparation liquid phase chromatographic technique, collecting two leading anthocyanin components, which are cyanidin-3-glucoside and paeonidin-3-glucoside, in the black rice pericarp respectively according to the obtained chromatogram, and performing rotary evaporation of eluent at a temperature of below 45 DEG C until all methanol is gone, and performing freeze-drying to obtain powder of the anthocyanin monomers.

Description

【Technical field】 [0001] The invention belongs to the technical field of deep processing of agricultural products, and relates to a method for separating and preparing high-purity anthocyanin monomers from black rice. 【Background technique】 [0002] Black rice (Oryza sativa L. indica) is an important type of colored special rice. Because of its rich nutrition and certain health effects, it has always been loved by people. It has a long history of planting and cultivation in my country and other countries in East Asia. Edible history. At present, black rice in my country is mainly distributed in provinces such as Yunnan, Guizhou, Guangdong, Guangxi, Hunan and Shaanxi. During the maturation process of black rice, a large amount of anthocyanin pigments will accumulate in the seed coat, so that the brown rice will appear brownish red, purple red, purple black and even black. In addition to black rice, anthocyanins are also widely distributed in other dark grain potatoes, berrie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/065C07H1/08
Inventor 凌文华
Owner GUANGZHOU TRACE ELEMENTS BIOLOGICAL TECH CO LTD
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