Method for preparing high-purity norbixin

An annatto, high-purity technology, applied in the field of phytochemistry, can solve the problems of backward technical level, low purity of annatto, limited application scope, etc., and achieves improved clarity and quality, safe technical guarantee, and low extraction cost. Effect

Active Publication Date: 2011-01-19
河北泽华生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are many shortcomings in this method: (1) due to the direct use of alkaline water as the extraction solvent, the extract contains a large amount of sugar, protein and other polar impurities; (2) the extract is not purified by column chromatography, but is directly acidified. Precipitation and crystallization, resulting in low purity of the obtained nor annatto
[0007] The development of annatto pigment in my country is still in its infancy, and the technical

Method used

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  • Method for preparing high-purity norbixin
  • Method for preparing high-purity norbixin

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Experimental program
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Embodiment 1

[0024] Embodiment 1: the annatto seed is added in the aqueous solution of ethanol or acetone of 2~10 times of (v / w) amount, promptly annatto seed takes weight gram or kilogram as unit of measurement, and the aqueous solution of ethanol or acetone takes volume liter or milliliter For the unit of measurement, the present embodiment gets 1000 grams of annatto seeds (annatto content is 2.5%), adds 4000 ml of ethanol with a volume concentration of 60%, and filters after stirring for 1 hour at 40° C., and the gained annatto extract filtrate is diluted with water to When the ethanol concentration is 50%, the capture and enrichment of annatto is carried out through a D312, XAD-16 or X-5 macroporous resin adsorption column with a 400ml loading capacity at a flow rate of 1BV / h with a height-to-diameter ratio of 3:1. , the adsorption flow rate is controlled at 1.5 to 2BV / h. After the adsorption, use a 70% ethanol aqueous solution to purify the saturated resin column. After removing most o...

Embodiment 2

[0025]Embodiment 2: The difference between this embodiment and Example 1 is to get 10 kilograms of annatto seeds (annatto content is 2.5%), add ethanol 50L of volume concentration 65%, filter after stirring at 45 ℃ for 1.5 hours. Gained annatto extract filtrate adds water and is diluted to ethanol concentration when being 50%, with the flow velocity of 1.5BV / h, be 4: 1 by height-to-diameter ratio, and loading capacity is the CAD-40 or LX700 macroporous resin resin adsorption column of 7500ml to carry out For the capture and enrichment of annatto, the adsorption flow rate is controlled at 1.5-2BV / h. After adsorption, use 70% ethanol aqueous solution to perform saturated resin column purification, remove most of the sugar and other polar impurities, and then use 95% ethanol Ethanol water solution (or methanol or acetone) adopts discontinuous gradient desorption method for resin desorption, and the desorption flow rate is controlled at 0.5BV / h. When HPLC detects that annatto flows...

Embodiment 3

[0026] Embodiment 3: The difference between the present embodiment and Example 1 is to get 100 kilograms of annatto seeds (annatto content is 2.5%), add ethanol 600L of volume concentration 70%, filter after stirring 2 hours under 50 ℃. Gained annatto extract filtrate adds water and dilutes to ethanol concentration when being 50%, is 4: 1 with the flow velocity of 2BV / h, the adsorption column that HZ818 or HZ801 or D1300 macroporous resin load is 120L carries out annatto extraction with the flow rate of 2BV / h. For orange capture and enrichment, the adsorption flow rate is controlled at 1.5-2BV / h. After adsorption, use 70% ethanol aqueous solution to perform saturated resin column purification, remove most of the sugar and other polar impurities, and then use 95% ethanol aqueous solution (or methanol or acetone) adopt the discontinuous gradient desorption method to carry out resin desorption, the desorption flow rate is controlled at 0.5BV / h, when HPLC detects that annatto flows...

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Abstract

The invention discloses a method for preparing high-purity norbixin, which comprises the following steps of: adding annatto seeds into aqueous solution of ethanol or acetone, stirring the solution, and performing solid-liquid separation to obtain bixin extract; enriching and desorbing the extract through adsorbent resin; and concentrating the desorption solution, drying the concentrate to obtain bixin crystal, adding aqueous solution of ethanol and alkali into the bixin crystal to dissolve the crystal, adjusting the pH value, separating out norbixin crystal, and performing solid-liquid separation to obtain the high-purity norbixin. Most impurities with high polarity can be removed by adopting macroporous absorption resin enrichment so as to improve the clarity and quality of the extract. Because a discontinuous gradient desorption method is adopted in the desorption process, a low-concentration ethanol flushing resin column can remove polysaccharide and high-polarity impurities; and the adopted high-concentration ethanol desorption greatly improves the quality of the desorption solution and is favorable for subsequent crystallization. By detecting, the HPLC content is more than 95percent, and the yield reaches over 80 percent; and the method provides safer technical guarantee for producing medicinal raw materials, has low extraction cost and is suitable for industrialized production.

Description

technical field [0001] The invention belongs to the technical field of phytochemistry, and in particular relates to a method for preparing high-purity annatto from annatto seeds. Background technique [0002] Annatto (mahogany pigment) is a non-toxic and tasteless natural pigment extracted from the aril of the tropical plant annatto. It has good dyeing properties and can provide three shades of yellow, orange, and orange. Not only It can be widely used as a coloring agent for daily necessities, food, and cosmetics, and it also has certain pharmacological effects. It has been used in Western countries for thousands of years. It is an international functional food coloring. It has passed the review of FAO / WHO and JECFA, and its product marketing is 167 country or region. In our country, it has also been included in the national standard food additive use hygienic standard (GB2760-1996), and many domestic businesses have already been operating and using mahogany pigment. [0...

Claims

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Application Information

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IPC IPC(8): C09B61/00C09B67/54
Inventor 王辉樊书旗杨贵国
Owner 河北泽华生物科技有限公司
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