CN108299265A - A method of extracting zeaxanthin and lutein from corn and its by-product - Google Patents

A method of extracting zeaxanthin and lutein from corn and its by-product Download PDF

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Publication number
CN108299265A
CN108299265A CN201810044969.7A CN201810044969A CN108299265A CN 108299265 A CN108299265 A CN 108299265A CN 201810044969 A CN201810044969 A CN 201810044969A CN 108299265 A CN108299265 A CN 108299265A
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China
Prior art keywords
corn
lutein
zeaxanthin
extract
raw material
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CN201810044969.7A
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Chinese (zh)
Inventor
吕美
王云龙
王利涛
胡锦霞
卢尉航
王其宝
王慧云
张敏娜
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JINING MEDICAL COLLEGE
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JINING MEDICAL COLLEGE
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Priority to CN201810044969.7A priority Critical patent/CN108299265A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C403/00Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone
    • C07C403/24Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone having side-chains substituted by six-membered non-aromatic rings, e.g. beta-carotene

Abstract

The method that the invention discloses a kind of to extract zeaxanthin and lutein from corn and its by-product, includes the following steps:Using corn and/or its processing byproduct as raw material, raw material is crushed to powdery;Above-mentioned raw materials are mixed with organic solvent with 5%~20% solid-liquid ratio;At a temperature of 40 DEG C~80 DEG C, mixed liquor is extracted by the method for stirring and/or ultrasound;Extracting solution is collected, concentration obtains natural zeaxanthin and lutein crude extract.The invention has the beneficial effects that:(1) organic solvent extraction and heating, stirring, combination of ultrasound so that zeaxanthin and lutein in raw material can be dissolved out preferably, so recovery rate is big, DNA purity is high;(2) substances such as highly basic are not used, although using organic solvent, dosage is seldom, and safe and non-toxic is environmentally friendly;(3) reaction condition is relatively mild so that the zeaxanthin and lutein that extract are more stable, waste is less.

Description

A method of extracting zeaxanthin and lutein from corn and its by-product
Technical field
The present invention relates to a kind of extracting methods, and in particular to one kind extracting zeaxanthin and leaf from corn and its by-product The method of flavine, belongs to technical field of agricultural product process.
Background technology
China is maize production big country, and the total output whole world is number two, and annual output is up to 600,000,000 tons or more, is had abundant Corn resources.Corn is used for the fields such as production of corn starch, alcoholic fermentation, feed processing more, and will produce many by-products Object, such as:Corn protein powder, corn flour, corn puffing powder, hominy grits, corn skin and grit, corn cake fodder, corn bran material etc.. Corn and its processing byproduct also contain a large amount of carotenoid other than containing protein, starch, fat and fiber --- Zeaxanthin and lutein.Zeaxanthin and lutein have protection eyesight, alleviate eye strain, anti-oxidant, anticancer and prevention The excellent effect such as angiocardiopathy.
China is also that corn consumes big country, but it is alcohol that corn, which mostly directly eats, is processed as starch or fermentation, at present simultaneously, Its by-product is multi-purpose to make animal feed, or directly discarded, and utilization rate is extremely limited, causes the waste of resource.
In order to improve the economic value of corn and its processing byproduct, someone passes through organic solvent extractionprocess or overcritical CO2Extraction method is extracted zeaxanthin and lutein, the zeaxanthin and lutein of extraction from corn and its processing byproduct The fields such as natural food colour, health products, cosmetics and drug are can be applied to, there is huge economic potential.
However, when extracting zeaxanthin and lutein from corn and its by-product using organic solvent extractionprocess at present, The organic solvent amount not being used only is big, and recovery rate is low, and production cost is high, meanwhile, zeaxanthin ester and lutein ester need Highly basic is hydrolyzed into monomer, there is larger pollution to environment.
Invention content
To solve the deficiencies in the prior art, that the purpose of the present invention is to provide a kind of recovery rates is big, DNA purity is high, economical The method that zeaxanthin and lutein are extracted in the slave corn and its processing byproduct of environmental protection.
In order to realize that above-mentioned target, the present invention adopt the following technical scheme that:
A method of extracting zeaxanthin and lutein from corn and its processing byproduct, which is characterized in that including Following steps:
Step1:Using corn and/or its processing byproduct as raw material, raw material is crushed to powdery;
Step2:Above-mentioned raw materials are mixed with organic solvent with 5%~20% solid-liquid ratio;
Step3:At a temperature of 40 DEG C~80 DEG C, mixed liquor is extracted by the method for stirring and/or ultrasound;
Step4:Extracting solution is collected, concentration obtains natural zeaxanthin and lutein crude extract.
Method above-mentioned, which is characterized in that in Step1, aforementioned processing byproduct includes:Corn flour, corn puffing Powder, hominy grits, corn skin and grit, corn protein powder feed, corn cake fodder and corn bran material.
Method above-mentioned, which is characterized in that in Step2, aforementioned organic solvents are ethyl alcohol, ethyl acetate, petroleum ether, third Any one either arbitrary two kinds of mixing or arbitrary three kinds of mixing in ketone and n-hexane.
Method above-mentioned, which is characterized in that in Step3, when being extracted to mixed liquor by the method for ultrasound, ultrasound The power of wave is 25KHz~80KHz.
Method above-mentioned, which is characterized in that in Step3, the time of extraction is 20min~120min, the number of extraction It is 1 time~3 times.
Method above-mentioned, which is characterized in that in Step4, concentrated using Rotary Evaporators.
The invention has the beneficial effects that:
(1) substances such as highly basic are not used, although using organic solvent, dosage is seldom, safe and non-toxic, to environment friend It is good;
(2) organic solvent extraction and heating, stirring, combination of ultrasound so that zeaxanthin and lutein in raw material can Preferably dissolution, so recovery rate is big, DNA purity is high;
(3) reaction condition is relatively mild so that the zeaxanthin and lutein that extract are more stable, waste is less.
Description of the drawings
Fig. 1 is the chromatogram of 1 obtained zeaxanthin and lutein of embodiment;
Fig. 2 is the chromatogram of 2 obtained zeaxanthin and lutein of embodiment;
Fig. 3 is the chromatogram of 3 obtained zeaxanthin and lutein of embodiment;
Fig. 4 is the chromatogram of 4 obtained zeaxanthin and lutein of embodiment;
Fig. 5 is the chromatogram of 5 obtained zeaxanthin and lutein of embodiment;
Fig. 6 is the chromatogram of 6 obtained zeaxanthin and lutein of embodiment;
Fig. 7 is the chromatogram of 7 obtained zeaxanthin and lutein of embodiment;
Fig. 8 is the chromatogram of 8 obtained zeaxanthin and lutein of embodiment.
Specific implementation mode
Specific introduce is made to the present invention below in conjunction with the drawings and specific embodiments.
Embodiment 1
Using corn protein powder as raw material, zeaxanthin and lutein are extracted according to the following steps:
1st step:It crushes
Corn protein powder is crushed, for use.
2nd step:Mixing
Corn protein powder is mixed with ethyl alcohol according to 20% solid-liquid ratio, 100g corn protein powders is taken, is added to 500mL's In ethyl alcohol, mix well.
3rd step:Extraction
40 DEG C of constant temperature, magnetic agitation extract 120min, and filtering is extracted 3 times, and extracting solution is merged.
4th step:Concentration
Combined extracting solution is concentrated with Rotary Evaporators, obtains natural zeaxanthin and lutein crude extract.
Crude extract is freeze-dried by we, through weighing, obtains 10.65g powdered extracts.
Finally, we by high performance liquid chromatography to the content of the content of zeaxanthin in powdered extract and lutein into Measurement is gone.
The condition of high performance liquid chromatography:C18 (4.6mm × 250mm, 5 μm) chromatographic column, mobile phase is second Nitrile:Methanol:Dichloromethane=80:13:7 (v/v/v), flow velocity 1.0mLmin-1, Detection wavelength 450nm, column temperature is room temperature.
Measurement result is shown in Fig. 1.As shown in Figure 1, the recovery rate of zeaxanthin is 0.18%, and the recovery rate of lutein is 0.13%.
Embodiment 2
Using corn flour as raw material, zeaxanthin and lutein are extracted according to the following steps:
1st step:It crushes
Corn flour is crushed, for use.
2nd step:Mixing
Corn flour is mixed with ethyl acetate according to 14% solid-liquid ratio, 100g corn flours is taken, is added to 700mL's In ethyl acetate, mix well.
3rd step:Extraction
50 DEG C of constant temperature, mechanical agitation+25KHz ultrasonic extraction 100min, filtering are extracted 2 times, and extracting solution is merged.
4th step:Concentration
Combined extracting solution is concentrated with Rotary Evaporators, obtains natural zeaxanthin and lutein crude extract.
Crude extract is freeze-dried by we, through weighing, obtains 7.54g powdered extracts.
Finally, we extract powdery by high performance liquid chromatography (condition of high performance liquid chromatography is same as Example 1) The content of zeaxanthin and the content of lutein are determined in object.Measurement result is shown in Fig. 2.As shown in Figure 2, zeaxanthin Recovery rate is 0.15%, and the recovery rate of lutein is 0.11%.
Embodiment 3
Using corn puffing powder as raw material, zeaxanthin and lutein are extracted according to the following steps:
1st step:It crushes
Corn puffing powder is crushed, for use.
2nd step:Mixing
Corn puffing powder is mixed with acetone according to 11% solid-liquid ratio, 100g corn puffing powder is taken, is added to 900mL's In acetone, mix well.
3rd step:Extraction
60 DEG C of constant temperature, 40KHz ultrasonic extraction 80min are extracted 1 time.
4th step:Concentration
Extracting solution is concentrated with Rotary Evaporators, obtains natural zeaxanthin and lutein crude extract.
Crude extract is freeze-dried by we, through weighing, obtains 6.8g powdered extracts.
Finally, we extract powdery by high performance liquid chromatography (condition of high performance liquid chromatography is same as Example 1) The content of zeaxanthin and the content of lutein are determined in object.Measurement result is shown in Fig. 3.From the figure 3, it may be seen that zeaxanthin Recovery rate is 0.22%, and the recovery rate of lutein is 0.19%.
Embodiment 4
Using hominy grits as raw material, zeaxanthin and lutein are extracted according to the following steps:
1st step:It crushes
Hominy grits is crushed, for use.
2nd step:Mixing
Hominy grits is mixed with petroleum ether according to 8% solid-liquid ratio, 100g hominy grits is taken, is added to the petroleum ether of 1200mL In, it mixes well.
3rd step:Extraction
50 DEG C of constant temperature, mechanical agitation+60KHz ultrasonic extraction 60min, filtering are extracted 2 times, and extracting solution is merged.
4th step:Concentration
Combined extracting solution is concentrated with Rotary Evaporators, obtains natural zeaxanthin and lutein crude extract.
Crude extract is freeze-dried by we, through weighing, obtains 7.5g powdered extracts.
Finally, we extract powdery by high performance liquid chromatography (condition of high performance liquid chromatography is same as Example 1) The content of zeaxanthin and the content of lutein are determined in object.Measurement result is shown in Fig. 4.As shown in Figure 4, zeaxanthin Recovery rate is 0.15%, and the recovery rate of lutein is 0.10%.
Embodiment 5
Using corn skin and grit as raw material, zeaxanthin and lutein are extracted according to the following steps:
1st step:It crushes
Corn skin and grit is crushed, for use.
2nd step:Mixing
Corn skin and grit is mixed with n-hexane according to 7% solid-liquid ratio, 100g corn skin and grits is taken, is being added to 1500mL just In hexane, mix well.
3rd step:Extraction
60 DEG C of constant temperature, magnetic agitation+80KHz ultrasonic extraction 40min, filtering are extracted 3 times, and extracting solution is merged.
4th step:Concentration
Combined extracting solution is concentrated with Rotary Evaporators, obtains natural zeaxanthin and lutein crude extract.
Crude extract is freeze-dried by we, through weighing, obtains 9.5g powdered extracts.
Finally, we extract powdery by high performance liquid chromatography (condition of high performance liquid chromatography is same as Example 1) The content of zeaxanthin and the content of lutein are determined in object.Measurement result is shown in Fig. 5.As shown in Figure 5, zeaxanthin Recovery rate is 0.30%, and the recovery rate of lutein is 0.25%.
Embodiment 6
Using corn cake fodder as raw material, zeaxanthin and lutein are extracted according to the following steps:
1st step:It crushes
Corn oil cake feed meal is broken, for use.
2nd step:Mixing
By corn cake fodder and the mixed organic solvents that are mixed in equal volume by acetone and petroleum ether according to 6% material Liquor ratio mixes, and takes 100g corn cake fodders, is added in the mixed organic solvents of 1700mL, mixes well.
3rd step:Extraction
70 DEG C of constant temperature, mechanical agitation extract 30min, extract 1 time.
4th step:Concentration
Extracting solution is concentrated with Rotary Evaporators, obtains natural zeaxanthin and lutein crude extract.
Crude extract is freeze-dried by we, through weighing, obtains 8.0g powdered extracts.
Finally, we extract powdery by high performance liquid chromatography (condition of high performance liquid chromatography is same as Example 1) The content of zeaxanthin and the content of lutein are determined in object.Measurement result is shown in Fig. 6.It will be appreciated from fig. 6 that zeaxanthin Recovery rate is 0.43%, and the recovery rate of lutein is 0.35%.
Embodiment 7
Using corn bran material as raw material, zeaxanthin and lutein are extracted according to the following steps:
1st step:It crushes
Corn bran feed powder is broken, for use.
2nd step:Mixing
Corn bran material is mixed with ethyl acetate according to 5% solid-liquid ratio, 100g corn bran material is taken, is added to 2000mL's In ethyl acetate, mix well.
3rd step:Extraction
80 DEG C of constant temperature, mechanical agitation extract 20min, and filtering is extracted 2 times, and extracting solution is merged.
4th step:Concentration
Combined extracting solution is concentrated with Rotary Evaporators, obtains natural zeaxanthin and lutein crude extract.
Crude extract is freeze-dried by we, through weighing, obtains 9.5g powdered extracts.
Finally, we extract powdery by high performance liquid chromatography (condition of high performance liquid chromatography is same as Example 1) The content of zeaxanthin and the content of lutein are determined in object.Measurement result is shown in Fig. 7.As shown in Figure 7, zeaxanthin Recovery rate is 0.36%, and the recovery rate of lutein is 0.27%.
Embodiment 8
Using corn protein powder as raw material, zeaxanthin and lutein are extracted according to the following steps:
1st step:It crushes
Corn protein powder is crushed, for use.
2nd step:Mixing
By corn protein powder and the mixed organic solvents that are mixed in equal volume by ethyl alcohol, ethyl acetate and n-hexane according to 10% solid-liquid ratio mixing, takes 100g corn protein powders, is added in the mixed organic solvents of 1000mL, mix well.
3rd step:Extraction
80 DEG C of constant temperature, magnetic agitation+80KHz ultrasonic extraction 20min, filtering are extracted 3 times, and extracting solution is merged.
4th step:Concentration
Combined extracting solution is concentrated with Rotary Evaporators, obtains natural zeaxanthin and lutein crude extract.
Crude extract is freeze-dried by we, through weighing, obtains 13.0g powdered extracts.
Finally, we extract powdery by high performance liquid chromatography (condition of high performance liquid chromatography is same as Example 1) The content of zeaxanthin and the content of lutein are determined in object.Measurement result is shown in Fig. 8.As shown in Figure 8, zeaxanthin Recovery rate is 0.26%, and the recovery rate of lutein is 0.18%.
By above-mentioned 8 embodiments, in conjunction with Fig. 1 to Fig. 8, it can be seen that:The extracting method of the present invention, by by organic solvent Extraction and heating, stirring, combination of ultrasound so that the recovery rate of zeaxanthin and lutein is improved, and DNA purity Also it is improved.
In addition, the extracting method reaction condition of the present invention is relatively mild, without using substances such as highly basic, although using organic molten Agent, but dosage is seldom, safe and non-toxic, it is environmentally friendly, highly promote and apply.
It should be noted that the invention is not limited in any way for above-described embodiment, it is all to use equivalent replacement or equivalent change The technical solution that the mode changed is obtained, all falls in protection scope of the present invention.

Claims (6)

1. it is a kind of from corn and its processing byproduct extract zeaxanthin and lutein method, which is characterized in that including with Lower step:
Step1:Using corn and/or its processing byproduct as raw material, raw material is crushed to powdery;
Step2:Above-mentioned raw materials are mixed with organic solvent with 5%~20% solid-liquid ratio;
Step3:At a temperature of 40 DEG C~80 DEG C, mixed liquor is extracted by the method for stirring and/or ultrasound;
Step4:Extracting solution is collected, concentration obtains natural zeaxanthin and lutein crude extract.
2. according to the method described in claim 1, it is characterized in that, in Step1, the processing byproduct includes:Maize flour Powder, corn puffing powder, hominy grits, corn skin and grit, corn protein powder feed, corn cake fodder and corn bran material.
3. according to the method described in claim 1, it is characterized in that, in Step2, the organic solvent is ethyl alcohol, acetic acid second Any one either arbitrary two kinds of mixing or arbitrary three kinds of mixing in ester, petroleum ether, acetone and n-hexane.
4. according to the method described in claim 1, it is characterized in that, in Step3, mixed liquor is carried out by the method for ultrasound When extraction, the power of ultrasonic wave is 25KHz~80KHz.
5. according to the method described in claim 1, it is characterized in that, in Step3, the time of extraction is 20min~120min, The number of extraction is 1 time~3 times.
6. according to the method described in claim 1, it is characterized in that, in Step4, concentrated using Rotary Evaporators.
CN201810044969.7A 2018-01-17 2018-01-17 A method of extracting zeaxanthin and lutein from corn and its by-product Pending CN108299265A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110241165A (en) * 2019-07-03 2019-09-17 齐鲁工业大学 A method of luteole is extracted from corn protein powder enzymatic hydrolysis jelly
CN112578047A (en) * 2020-12-10 2021-03-30 浙江艾兰得生物科技有限公司 High performance liquid chromatography detection method for xanthophyll and zeaxanthin content
CN114292527A (en) * 2021-12-28 2022-04-08 中国科学院兰州化学物理研究所 Method for extracting maize yellow component from maize

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101280121A (en) * 2008-05-27 2008-10-08 曹龙奎 Method for extracting corn flavochrome by microwave-ultrasonic
CN101759618A (en) * 2008-12-25 2010-06-30 中国科学院兰州化学物理研究所 Method for extracting lutein ester compounds form marigolds
CN104478774A (en) * 2014-12-12 2015-04-01 吕梁广汇生物科技股份有限公司 Method for extracting lutein from fresh marigold flowers as raw materials

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101280121A (en) * 2008-05-27 2008-10-08 曹龙奎 Method for extracting corn flavochrome by microwave-ultrasonic
CN101759618A (en) * 2008-12-25 2010-06-30 中国科学院兰州化学物理研究所 Method for extracting lutein ester compounds form marigolds
CN104478774A (en) * 2014-12-12 2015-04-01 吕梁广汇生物科技股份有限公司 Method for extracting lutein from fresh marigold flowers as raw materials

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110241165A (en) * 2019-07-03 2019-09-17 齐鲁工业大学 A method of luteole is extracted from corn protein powder enzymatic hydrolysis jelly
CN110241165B (en) * 2019-07-03 2021-05-18 齐鲁工业大学 Method for extracting zeaxanthin from corn gluten meal enzymolysis jelly
CN112578047A (en) * 2020-12-10 2021-03-30 浙江艾兰得生物科技有限公司 High performance liquid chromatography detection method for xanthophyll and zeaxanthin content
CN114292527A (en) * 2021-12-28 2022-04-08 中国科学院兰州化学物理研究所 Method for extracting maize yellow component from maize
CN114292527B (en) * 2021-12-28 2022-10-04 中国科学院兰州化学物理研究所 Method for extracting maize yellow component from maize

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Application publication date: 20180720