Method for refining capsanthin by enzyme catalysis, esterification and molecular distillation

A technology of capsanthin and molecular distillation, which is applied in the field of natural organic chemistry, can solve the problems of by-products that cannot be directly used, difficult degassing, high distillation temperature, etc., and achieves the effects of low production cost, simple process and high product content

Active Publication Date: 2012-08-01
SOUTH CHINA UNIV OF TECH
2 Cites 8 Cited by

AI-Extracted Technical Summary

Problems solved by technology

This process: (1) After degumming with low-carbon alcohol, it does not need to carry out solvent recovery, but directly participates in the esterification reaction; (2...
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Abstract

The invention discloses a method for refining capsanthin by enzyme catalysis, esterification and molecular distillation. The method comprises the following steps of: mixing chili red oil resin and a degumming agent in a mass ratio of 1:1-1:10, stirring uniformly at the temperature of between 20 and 60 DEG C and at the speed of 100 to 800 revolutions per minute, and standing or intermittently stirring and settling at the temperature of between 0 and 5 DEG C; after settling for 5 to 20 hours, filtering under a vacuum condition to obtain filtrate, and separating the filtrate to obtain a degummedpigment solution; adding lipase and water into the degummed pigment solution, mixing uniformly, and reacting at the temperature of between 30 and 60 DEG C under stirring at the speed of 50 to 300 revolutions per minute; after reacting for 2 to 10 hours, dehydrating for 1 to 3 hours; filtering out the lipase, and reclaiming a solvent from the pigment solution under reduced pressure to obtain a fatty acid ester solution containing the capsanthin; and performing two-stage molecular distillation on the fatty acid ester solution to obtain the capsanthin with high color value. The method has the advantages of simple process, high product content, few insoluble acetone substances and low production cost, and is suitable for industrialized production.

Application Domain

Technology Topic

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  • Method for refining capsanthin by enzyme catalysis, esterification and molecular distillation
  • Method for refining capsanthin by enzyme catalysis, esterification and molecular distillation

Examples

  • Experimental program(5)

Example Embodiment

[0031] Example 1
[0032] The present invention is an enzyme-catalyzed esterification molecular distillation method for refining capsanthin (such as figure 1 Shown), including the following steps:
[0033] Step 1: Degumming
[0034] (1) Put 10 kg of capsicum red oleoresin and 10 kg of degumming agent (absolute ethanol) into a jacketed reactor, and stir at 60°C at a speed of 100 revolutions per minute.
[0035] (2) After stirring evenly, pump the mixed solution into the freezing tank, control the temperature of the freezing tank to 5°C, and let it settle down.
[0036] (3) After 5 hours of sedimentation, the vacuum degree of the freezing liquid is 3×10 4 Under Pa conditions, the upper part of the freezing tank is sucked into the vacuum filter to obtain the filtrate, and the filtrate is separated by the tubular centrifuge to obtain the degummed pigment solution.
[0037] Step 2: Esterification
[0038] (1) Add the degummed pigment solution to the enzyme reactor, and add 50 g of lipase (Novozym 435) and 100 g of water, mix well, control the reaction temperature at 60° C., and control the stirring speed at 50 rpm. Among them, the mass ratio of degumming agent, lipase and water is 100:0.5:1.
[0039] (2) After 2 hours of reaction and dehydration under reduced pressure for 1 hour, the conversion rate of fatty acids is 90%.
[0040] (3) After the dehydration, the lipase is filtered and the pigment solution is decompressed to recover the solvent to obtain the capsaicin-containing fatty acid ethyl ester solution. The temperature of the decompression recovery solvent is 30°C and the vacuum degree is 8×10 4 Pa.
[0041] Step 3: Molecular distillation
[0042] The fatty acid ester solution containing capsanthin is subjected to two-stage molecular distillation to obtain 4.8Kg of fatty acid esters and 4.8Kg of high-quality capsanthin with a color value of 291 and a fat-acetone insoluble matter of 0.21%. Air temperature is 80℃, vacuum degree is 2×10 4 Pa, secondary distillation temperature 120℃, vacuum degree 15Pa.

Example Embodiment

[0043] Example 2
[0044] In this embodiment, an enzyme-catalyzed esterification molecular distillation method for refining capsanthin, except for the following differences, other steps and process conditions are the same as in embodiment 1:
[0045] (1) Add capsicum red oleoresin and methanol with masses of 10Kg and 50Kg, respectively, and stir evenly at a speed of 500 revolutions/min at 20°C.
[0046] (2) The temperature of the freezing tank is 3°C, and it is allowed to settle for 10 hours.
[0047] (3) The esterification reaction temperature is 45° C., the reaction is 5 hours, and the stirring speed is 150 rpm.
[0048] (4) Dehydration under reduced pressure for 2 hours.
[0049] (5) Decompression recovery solvent temperature is 40℃, vacuum degree is 6×10 4 Pa.
[0050] (6) The mass ratio of degumming agent, lipase and water is 100:3:3.
[0051] (7) Lipase is Lipozyme RM IM.
[0052] (8) The first-stage degassing temperature is 100℃, and the vacuum degree is 8×10 3 Pa, secondary distillation temperature 160℃, vacuum degree 20Pa.
[0053] (9) The conversion rate of fatty acids is 92%.
[0054] (10) Obtain 4.2Kg of fatty acid ester and 4.9Kg of high-quality capsanthin with a color value of 282 and a fatty acetone insoluble matter of 0.25%.

Example Embodiment

[0055] Example 3
[0056] In this embodiment, an enzyme-catalyzed esterification molecular distillation method for refining capsanthin, except for the following differences, other steps and process conditions are the same as in embodiment 1:
[0057] (1) Add capsicum red oleoresin and the mass fraction of 95% ethanol aqueous solution with masses of 10Kg and 100Kg, respectively, and stir uniformly at a speed of 800 rpm at 35°C.
[0058] (2) The temperature of the freezing tank is 0°C, and it is allowed to stand and settle for 20 hours.
[0059] (3) The esterification reaction temperature is 30°C, the reaction is for 10 hours, and the stirring speed is 300 rpm.
[0060] (4) Dehydration under reduced pressure for 3 hours.
[0061] (5) Decompression recovery solvent temperature is 50℃, vacuum degree is 4×10 4 Pa.
[0062] (6) The mass ratio of degumming agent, lipase and water is 100:10:5.
[0063] (7) Lipase is Lipozyme RM IM.
[0064] (8) The first-stage degassing temperature is 50℃, and the vacuum degree is 6×10 4 Pa, secondary distillation temperature 100℃, vacuum degree 0.1Pa.
[0065] (9) The conversion rate of fatty acids is 91%.
[0066] (10) Obtained 4.5Kg of fatty acid ester and 4.5Kg of high-quality capsicum red pigment with a color value of 286 and a fat acetone insoluble matter of 0.28%.
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