CN103058906A - Production process of phytoxanthin feed additive - Google Patents
Production process of phytoxanthin feed additive Download PDFInfo
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- CN103058906A CN103058906A CN2013100380735A CN201310038073A CN103058906A CN 103058906 A CN103058906 A CN 103058906A CN 2013100380735 A CN2013100380735 A CN 2013100380735A CN 201310038073 A CN201310038073 A CN 201310038073A CN 103058906 A CN103058906 A CN 103058906A
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Abstract
The invention provides a production process of phytoxanthin feed additive. The process comprises the following steps: preparing potassium hydroxide liquid; adding the potassium hydroxide liquid to cymbopogon citrat extract with a certain temperature according to proportion; adding propylene glycol and ethoxyquin in turn while stirring; raising the temperature and saponifying to obtain the saponification liquid; adding silica powder to the saponification liquid, and then stirring; finally screening to obtain the phytoxanthin feed additive. The production process has the advantages of high yield of products, low industrial production toxicity and high safety, and is convenient to industrial production on large scales; at the same time, the products prepared according to the method has little residual methanol and good quality, and meets the regulations of national standard GB/T212517-2008.
Description
Technical field
The invention belongs to technological field of biochemistry, relate to the technique that a kind of xenthophylls with extracting in the mary bush is produced bird feed additive, particularly a kind of xenthophylls feed additive production technique.
Background technology
Xenthophylls is a kind of natural carotenoid, extensively is present in vegetables, flowers, fruit and some algae.Contained natural carotenol is a kind of good antioxidant in the plant, can prevent that cell is oxidized.A certain amount of xenthophylls is added to a series of diseases that can prevent in the food that human body from causing because of organ senescence.Xenthophylls can also add the color that improves yolk and cock skin in the chicken feed to as a kind of natural pigment.Free lutein can directly be absorbed by human body and bird, and is difficult for being absorbed by human body and animal with the xenthophylls that the lutein ester form exists.Therefore, extraction and separated free xenthophylls have become one of research focus.Mary bush is that known all plant Lutein content are the highest at present, but free lutein content is very low in the mary bush, major part is combined into lutein ester with saturated fatty acids such as lauric acid, tetradecanoic acid, palmitinic acids, need to add metal overbase and make the saponification of xenthophylls straight-chain fatty acid ester and form lutein crystal, thereby extract free lutein.Preparation technology's required time of xenthophylls class material is long at present, causes xenthophylls degraded and isomer to occur, has reduced the product yield, is not easy to large-scale industrialization production; And suitability for industrialized production toxicity is high, security is low.
Summary of the invention
The purpose of this invention is to provide a kind of product yield height, low, the safe xenthophylls feed additive production technique of suitability for industrialized production toxicity, energy consumption is little, and is with short production cycle, is convenient to large-scale industrialization production.
For achieving the above object, the technical solution adopted in the present invention is: a kind of xenthophylls feed additive production technique, the product yield is high, suitability for industrialized production toxicity is low, safe, is convenient to large-scale industrialization production, and this production technique is specifically carried out according to the following steps:
Step 1: be made into potassium hydroxide solution with potassium hydroxide and water;
Step 2: add 27 kilograms of propylene glycol by 270 kilograms of mary bush medicinal extract, the ratio of the potassium hydroxide solution of 10 kilograms of ethoxyquinolines and 150～160 kilograms of step 1 preparations, get respectively mary bush medicinal extract, the potassium hydroxide solution of ethoxyquinoline and step 1 preparation, then potassium hydroxide solution is added temperature and be in 40～50 ℃ the mary bush medicinal extract, form reaction solution, the temperature of control reaction solution is below 80 ℃, in situation about stirring, propylene glycol and ethoxyquinoline are added in this reaction solution successively, be warming up to 75～85 ℃, saponification 50～65 minutes obtains temperature and is 75～85 ℃ saponification liquor;
Add the ratio of 280 kilograms of SiO 2 powders in 270 kilograms of mary bush medicinal extract, get SiO 2 powder, and the SiO 2 powder of getting is added temperature that step 2 obtains is in 75～85 ℃ the saponification liquor, stirred 20～30 minutes, get the saponification powder;
Step 3: the saponification powder is crossed 40 mesh sieves, make the xenthophylls fodder additives.
Production technique of the present invention adopts potassium hydroxide-propylene glycol system, the KOH aqueous solution take 55% is as saponifying agent, add propylene glycol and can obviously accelerate the saponification speed of medicinal extract, and can reduce the viscosity of saponification liquor, 80 ℃ of saponification 60min both can be fully saponified, compare potassium hydroxide-methanol system and potassium hydroxide-ethanol system, suitability for industrialized production toxicity of the present invention is low, safe, saponification time is short, saponification degree is high, methyl alcohol is residual low, superior product quality meets GB GB/T 212517-2008(fodder additives xenthophylls).
Description of drawings
Fig. 1 is the schema of production technique of the present invention.
Embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.
In order to take full advantage of the xenthophylls in the mary bush, it is long to overcome the temperature height, the time that exist when existing technique is extracted free lutein, causes xenthophylls degraded and isomer to occur, and the product yield is low, is not easy to the problem that large-scale industrialization is produced.The invention provides that a kind of yield is high, energy consumption is little, with short production cycle, be convenient to the xenthophylls feed additive production technique that large-scale industrialization is produced.Its technical process is specifically carried out as shown in Figure 1 according to the following steps:
Step 1: get the potassium hydroxide of feed grade, be dissolved in the water, be made into concentration and be 50～60% potassium hydroxide solution;
Step 2: add 27 kilogram of feed grade propylene glycols by 270 kilograms of mary bush medicinal extract, the ratio of the potassium hydroxide solution of 10 kilogram of feed level ethoxyquinolines and 150～160 kilograms of step 1 preparations, get respectively mary bush medicinal extract, the potassium hydroxide solution of ethoxyquinoline and step 1 preparation, then potassium hydroxide solution is added temperature and be in 40～50 ℃ the mary bush medicinal extract, form reaction solution, the temperature of control reaction solution is below 80 ℃, in situation about stirring, propylene glycol and ethoxyquinoline are added in this reaction solution successively, be warming up to 75～85 ℃, saponification 55～65 minutes obtains temperature and is 75～85 ℃ saponification liquor;
Add the ratio of 280 kilogram of feed grade silicon dioxide powder in 270 kilograms of mary bush medicinal extract, get SiO 2 powder, and the SiO 2 powder of getting is added temperature is in 75～85 ℃ the saponification liquor, stirred 20～30 minutes, get the saponification powder;
Step 3: the saponification powder is sieved, make the xenthophylls fodder additives.
The weight of the xenthophylls fodder additives that makes is about 2.6 times of mary bush medicinal extract weight.
Because xenthophylls is to exist with the form with lauric acid, tetradecanoic acid, oleic acid and linolenic acid formation ester in mary bush, through behind the organic solvent extraction, this existence form does not change; Thereby before being further purified, must process through saponification, xenthophylls is reduced to monomeric form.The simplest method for saponification of at present widespread use is that hydrocarbon solution with lutein extract is with the saturated methyl alcohol jolting of potassium hydroxide.Saponification is processed can remove chlorophyll, and hydrolysis from the form of the ester of formation is out removed lipid acid parent molecule is discharged with most of xenthophylls molecule and zeaxanthin molecule.
The saponification mode of using in the industrial production at present generally has two kinds
A) cold saponification: take by weighing the lutein extract of certain mass, add alkaline solution according to predetermined ratio, stir and place and spent the night in 15 hours.
B) hot saponification: take by weighing the lutein extract of certain mass, add alkaline solution according to predetermined proportion, then with mixture heating up to certain temperature afterreaction for some time, until react complete till.
Although the thermooxidizing that cold saponification can be avoided causing because of high temperature is lost, its reaction times is long; Although and hot saponification mode adopts high temperature, but the reaction times can shorten greatly, and fractional yield is also higher, also can avoid the loss that causes because of the Long contact time air simultaneously, thereby present except minority has the technique of particular requirement, what mostly adopt is hot saponification mode.So production technique of the present invention also adopts the mode of hot saponification.
The factor that affects the saponification of mary bush medicinal extract mainly contains saponifying agent concentration, saponifying agent consumption, saponification temperature and four factors of saponification time.The saponifying agent that often uses is potassium hydroxide and sodium hydroxide, and the solvent of saponifying agent is generally water and lower boiling alcohol such as methyl alcohol, ethanol etc.Saponification temperature is larger to the saponification influential effect, and suitable saponification temperature can improve the extracted amount of xenthophylls, and the temperature influence of xenthophylls own is also larger.Mainly exist with transconfiguration under the lutein ester normal temperature, be heated, under illumination and the chemical action, 7% xenthophylls arranged approximately by the trans cis-structure that is converted into, and what play active function mainly is transconfiguration.The too short reaction times can cause the saponification of xenthophylls grease not thorough, and saponification degree is low, is unfavorable for the separation and purification of back.If but saponification under comparatively high temps, overlong time has more xenthophylls and is converted into cis-structure by transconfiguration, thereby affects the quality of saponification xenthophylls, reduces its anti-oxidant activity and anticancer effect.Even the pigment grease is fully by saponification like this, but because the xenthophylls that of dissociating after the saponification is a kind ofly to be easy to carotenoid oxidized, inactivation, and lose utility value.Saponification system commonly used is potassium hydroxide-methanol system and potassium hydroxide-ethanol system at present, and suitability for industrialized production toxicity is high, security is low, saponification time is long, saponification degree is low, and product quality is relatively poor.
This production technique adopts evenly (UD) method of design, and on saponifying agent concentration, saponifying agent consumption, saponification temperature and four factors of saponification time of affecting saponification reaction, every factor is established six levels, selects U under four factors, six levels
6(6
4) uniform designs table, by testing the relatively saponification effect of each factor, saponifying agent concentration, saponifying agent consumption, saponification temperature and four factors of saponification time that affect saponification reaction are optimized selection, processing parameter when having proposed production technique saponification mary bush medicinal extract of the present invention, saponification degree can reach 93.6%.When producing tinting material class (xenthophylls) fodder additives with propylene glycol saponification mary bush medicinal extract, in reaction system, add the saponification speed that propylene glycol can obviously be accelerated ointment, this be because propylene glycol can with water, ethanol and multiple immiscible organic solvent, in the saponification process, add in right amount, can increase the dissolving of grease in the middle of buck, be beneficial to saponification reaction and occur, saponification time has shortened 3 times, and can reduce the viscosity of saponification liquor, and the xenthophylls loss is little, and saponification degree is high.The propylene glycol add-on can be controlled in 1/10,80 ℃ of saponification 60min of mary bush medicinal extract weight both can be fully saponified; The xenthophylls fodder additives that makes meets GB GB/T 212517-2008(fodder additives xenthophylls) regulation, can be added directly in the bird feed.
Embodiment 1
Get the potassium hydroxide of feed grade, be dissolved in the water, be made into concentration and be 50% potassium hydroxide solution;
The ratio that adds 27 kilogram of feed grade propylene glycols, 10 kilogram of feed level ethoxyquinolines and 160 kg of hydrogen potassium oxide solutions in 270 kilograms of mary bush medicinal extract, get respectively mary bush medicinal extract, ethoxyquinoline and potassium hydroxide solution, then potassium hydroxide solution is added temperature and be in 40 ℃ the mary bush medicinal extract, form reaction solution, the temperature of control reaction solution is below 80 ℃, in situation about stirring, propylene glycol and ethoxyquinoline are added in this reaction solution successively, be warming up to 85 ℃, saponification 55 minutes obtains temperature and is 85 ℃ saponification liquor; Add the ratio of 280 kilogram of feed grade silicon dioxide powder in 270 kilograms of mary bush medicinal extract, get SiO 2 powder, and the SiO 2 powder of getting is added temperature is in 85 ℃ the saponification liquor, stirred 20 minutes, get the saponification powder; This saponification powder is crossed 40 mesh sieves, make the xenthophylls fodder additives.
Comparative Examples
Get the potassium hydroxide of feed grade, be dissolved in the methyl alcohol, be made into concentration and be 50% potassium hydroxide methanol solution; The ratio that adds 25 kilograms of potassium hydroxide methanol solutions in 50 kilograms of mary bush medicinal extract, get respectively mary bush medicinal extract and potassium hydroxide methanol solution, then potassium hydroxide methanol solution is added in the mary bush medicinal extract, form reaction solution, control the temperature of reaction solution at 55 ~ 60 ℃, saponification 180 minutes; Add the ratio of 50 kilogram of feed grade silicon dioxide powder in 50 kilograms of mary bush medicinal extract, get SiO 2 powder, and the SiO 2 powder of getting is added temperature is in 60 ℃ the saponification liquor, stirred 30 minutes, get the saponification powder; This saponification powder is crossed 40 mesh sieves, make the xenthophylls fodder additives.
Can be found out that by embodiment 1 and Comparative Examples the saponification time of production technique of the present invention is far smaller than the saponification time of existing technique, energy consumption is little, with short production cycle.
Embodiment 2
Get the potassium hydroxide of feed grade, be dissolved in the water, be made into concentration and be 55% potassium hydroxide solution;
The ratio that adds 27 kilogram of feed grade propylene glycols, 10 kilogram of feed level ethoxyquinolines and 150 kg of hydrogen potassium oxide solutions in 270 kilograms of mary bush medicinal extract, get respectively mary bush medicinal extract, ethoxyquinoline and potassium hydroxide solution, then potassium hydroxide solution is added temperature and be in 50 ℃ the mary bush medicinal extract, form reaction solution, the temperature of control reaction solution is below 80 ℃, in situation about stirring, propylene glycol and ethoxyquinoline are added in this reaction solution successively, be warming up to 75 ℃, saponification 65 minutes obtains temperature and is 75 ℃ saponification liquor; Add the ratio of 280 kilogram of feed grade silicon dioxide powder in 270 kilograms of mary bush medicinal extract, get SiO 2 powder, and the SiO 2 powder of getting is added temperature is in 75 ℃ the saponification liquor, stirred 30 minutes, get the saponification powder; This saponification powder is crossed 40 mesh sieves, make the xenthophylls fodder additives.
Embodiment 3
Get the potassium hydroxide of feed grade, be dissolved in the water, be made into concentration and be 60% potassium hydroxide solution;
The ratio that adds 27 kilogram of feed grade propylene glycols, 10 kilogram of feed level ethoxyquinolines and 155 kg of hydrogen potassium oxide solutions in 270 kilograms of mary bush medicinal extract, get respectively mary bush medicinal extract, ethoxyquinoline and potassium hydroxide solution, then potassium hydroxide solution is added temperature and be in 45 ℃ the mary bush medicinal extract, form reaction solution, the temperature of control reaction solution is below 80 ℃, in situation about stirring, propylene glycol and ethoxyquinoline are added in this reaction solution successively, be warming up to 80 ℃, saponification 60 minutes obtains temperature and is 80 ℃ saponification liquor; Add the ratio of 280 kilogram of feed grade silicon dioxide powder in 270 kilograms of mary bush medicinal extract, get SiO 2 powder, and the SiO 2 powder of getting is added temperature is in 80 ℃ the saponification liquor, stirred 25 minutes, get the saponification powder; This saponification powder is crossed 40 mesh sieves, make the xenthophylls fodder additives.
Claims (3)
1. xenthophylls feed additive production technique, the product yield is high, suitability for industrialized production toxicity is low, safe, is convenient to large-scale industrialization production, it is characterized in that this production technique is specifically carried out according to the following steps:
Step 1: be made into potassium hydroxide solution with potassium hydroxide and water;
Step 2: add 27 kilograms of propylene glycol by 270 kilograms of mary bush medicinal extract, the ratio of the potassium hydroxide solution of 10 kilograms of ethoxyquinolines and 150～160 kilograms of step 1 preparations, get respectively mary bush medicinal extract, the potassium hydroxide solution of ethoxyquinoline and step 1 preparation, then potassium hydroxide solution is added temperature and be in 40～50 ℃ the mary bush medicinal extract, form reaction solution, the temperature of control reaction solution is below 80 ℃, in situation about stirring, propylene glycol and ethoxyquinoline are added in this reaction solution successively, be warming up to 75～85 ℃, saponification 55～65 minutes obtains temperature and is 75～85 ℃ saponification liquor;
Add the ratio of 280 kilograms of SiO 2 powders in 270 kilograms of mary bush medicinal extract, get SiO 2 powder, and the SiO 2 powder of getting is added temperature that step 2 obtains is in 75～85 ℃ the saponification liquor, stirred 20～30 minutes, get the saponification powder;
Step 3: the saponification powder is crossed 40 mesh sieves, make the xenthophylls fodder additives.
2. according to xenthophylls feed additive production technique claimed in claim 1, it is characterized in that the concentration of the potassium hydroxide solution in the described step 1 is 50～60%.
3. according to xenthophylls feed additive production technique claimed in claim 1, it is characterized in that, in the described step 3.The saponification powder is crossed 40 mesh sieves.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104171390A (en) * | 2014-07-22 | 2014-12-03 | 河北中进生物科技有限公司 | Making method of high-density xanthophylls powder as feed additive |
| CN104982735A (en) * | 2015-07-16 | 2015-10-21 | 周玉珍 | Xanthophyll egg feed additive and preparation method thereof |
| CN109452576A (en) * | 2018-11-23 | 2019-03-12 | 江苏省徐州医药高等职业学校 | A kind of Tilapia mossambica dried fish floss and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1997023436A1 (en) * | 1995-12-21 | 1997-07-03 | Kemin Foods, L.C. | A process for the formation, isolation and purification of comestible xanthophyll crystals from plants |
| CN1463966A (en) * | 2002-06-07 | 2003-12-31 | 青岛大学 | Process for preparing lutein |
| CN1603308A (en) * | 2004-06-03 | 2005-04-06 | 成都枫澜科技有限公司 | Method for preparing lutein crystal from marigold extractive |
| CN101434568A (en) * | 2008-11-19 | 2009-05-20 | 黑龙江省嘉宝生物技术开发有限公司 | Method for preparing high-content xanthophyll crystal from Calendula officinalis extract |
| CN101473893A (en) * | 2008-11-19 | 2009-07-08 | 黑龙江省嘉宝生物技术开发有限公司 | Feed addictive containing xanthophyll and zeaxanthol as well as preparation method |
| CN101693681A (en) * | 2009-09-26 | 2010-04-14 | 美科尔(河北)生物科技有限公司 | Method for preparing lutein crystal from lutein extract |
-
2013
- 2013-01-31 CN CN2013100380735A patent/CN103058906A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1997023436A1 (en) * | 1995-12-21 | 1997-07-03 | Kemin Foods, L.C. | A process for the formation, isolation and purification of comestible xanthophyll crystals from plants |
| CN1463966A (en) * | 2002-06-07 | 2003-12-31 | 青岛大学 | Process for preparing lutein |
| CN1603308A (en) * | 2004-06-03 | 2005-04-06 | 成都枫澜科技有限公司 | Method for preparing lutein crystal from marigold extractive |
| CN101434568A (en) * | 2008-11-19 | 2009-05-20 | 黑龙江省嘉宝生物技术开发有限公司 | Method for preparing high-content xanthophyll crystal from Calendula officinalis extract |
| CN101473893A (en) * | 2008-11-19 | 2009-07-08 | 黑龙江省嘉宝生物技术开发有限公司 | Feed addictive containing xanthophyll and zeaxanthol as well as preparation method |
| CN101693681A (en) * | 2009-09-26 | 2010-04-14 | 美科尔(河北)生物科技有限公司 | Method for preparing lutein crystal from lutein extract |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104171390A (en) * | 2014-07-22 | 2014-12-03 | 河北中进生物科技有限公司 | Making method of high-density xanthophylls powder as feed additive |
| CN104982735A (en) * | 2015-07-16 | 2015-10-21 | 周玉珍 | Xanthophyll egg feed additive and preparation method thereof |
| CN109452576A (en) * | 2018-11-23 | 2019-03-12 | 江苏省徐州医药高等职业学校 | A kind of Tilapia mossambica dried fish floss and preparation method thereof |
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Application publication date: 20130424 |