CN103461645B - Preparation method of cottonseed protein - Google Patents
Preparation method of cottonseed protein Download PDFInfo
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- CN103461645B CN103461645B CN201310382819.4A CN201310382819A CN103461645B CN 103461645 B CN103461645 B CN 103461645B CN 201310382819 A CN201310382819 A CN 201310382819A CN 103461645 B CN103461645 B CN 103461645B
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- cottonseed
- dephenolize
- cottonseed meal
- gossypol
- protein
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Abstract
The invention discloses a preparation method of cottonseed protein, which comprises the steps that (1) cottonseed meal is dephenolized; and (2) the cottonseed protein is extracted from the dephenolized cottonseed meal, wherein dephenolization of the cottonseed meal is to leach the cottonseed meal with a mixed solvent of alcohol and n-hexane, and a volume ratio of alcohol to n-hexane is (1-5):5. The dephenolized cottonseed meal is leached by a mixed aqueous solution of sodium hydroxide and sodium sulfite, and the cottonseed protein is obtained by acid precipitation of a leaching solution. With the adoption of the method, a removed rate of gossypol can reach above 80%; free gossypol (FG) is less than or equal to 400mg/kg; a yield of the cottonseed protein reaches above 60%; and the purity is greater than 90%.
Description
Technical field
The invention belongs to cottonseed processing field, be specifically related to the preparation method of cottonseed protein.
Background technology
China is the first in the world great Chan Mian state, and annual cottonseed output reaches 900 × 10
4more than t, its main producing region is in the North China Plain and Plain, northwest.Cottonseed is not only important vegetable oil material, but also contain the protein of about 20%, be the important oil plant and the protein crop that the world today are only second to soybean, therefore for countries in the world, the byproduct cottonseed meal after cottonseed gets oil becomes important plant protein resource.Owing to there being the existence of gossypol in cottonseed meal, existing cottonseed meal working method generally comprises two steps: cottonseed meal dephenolize (also referred to as detoxification), then from dephenolize cotton dregs, extracts cottonseed protein.At present, chemical method, biological fermentation process, solvent extration and liquid-liquid-solid three phase extraction method is mainly adopted to removing of gossypol in cottonseed meal; Alkali extraction-acid precipitation is mainly adopted to the extraction of cottonseed protein, salt carries or zymolysis technique.
(1) cotton dregs dephenolize technology
Chemical method removes gossypol in cottonseed meal, the chemical property of its technology utilization gossypol, makes it destroy under certain conditions or in bonding state.Conventional is add vitriol (ferrous sulfate, copper sulfate), and its metal ion and dregs of rice Free Gossypol form complex compound, aldehyde radical and hydroxyl in gossypol are lost activity, reaches detoxification object; Also have interpolation urea and gossypol to form Schiff's base affixture, salt adding makes gossypol be oxidized in neutral environment.Its shortcoming is that formed complex compound is still retained in cotton dregs, and the palatability of the dregs of rice is poor, not easily digested.
Biological fermentation process adopts yeast gossypol to be converted into other materials, to reach the object of detoxification.Because transformation mechanism is failed to understand, the control difficulty of processing condition is large, and detoxification efficiency cannot ensure; Cotton dregs after hot moulding leaches, in pre-treatment and dregs of rice drying course, protein is sex change, and its nutritive value also cannot be guaranteed; In addition, investment is also greatly a defect of this method.
Solvent extration utilizes gossypol solvability in a solvent, usually adopts methyl alcohol, acetone etc. to extract, and because problem of solvent residual adds the hazardness of product, limits the use range of the standby cottonseed protein of this legal system simultaneously.
(2) extractive technique of cottonseed protein
Though alkali extraction-acid precipitation is a kind of effective ways preparing cottonseed protein, in preparation process, produce a large amount of spent acid, alkali waste water; Although the lipidated protein of salt formulation preparation is high, extraction rate of protein is less than 35%; Enzymatic Extraction good product quality, but enzymolysis process controls difficulty greatly, and production cost is high.
Summary of the invention
The object of the invention is to solve the problems referred to above in the production of existing cottonseed protein, the preparation method of the cottonseed protein that a kind of gossypol decreasing ratio is high is provided.
It is as follows that the present invention realizes the technical scheme that above-mentioned purpose adopts:
. a kind of preparation method of cottonseed protein, cottonseed protein is extracted in the dephenolize and (2) that comprise (1) cottonseed meal from the cottonseed meal of dephenolize, it is characterized in that, the dephenolize of cottonseed meal is the mixed solvent lixiviate cottonseed meal with ethanol and normal hexane, wherein, the volume ratio of described ethanol and normal hexane is (1 ~ 5): 5.
Further, the volume ratio of described ethanol and normal hexane is (1 ~ 4): 5.
Further, during lixiviate dephenolize, the solid-liquid ratio of cottonseed meal and mixed solvent is 1:(3 ~ 6).
Further, during lixiviate dephenolize, extraction temperature is 40 ~ 50 DEG C.
The optimal conditions of cottonseed meal dephenolize is: the volume ratio of ethanol and normal hexane is 4:5, and the solid-liquid ratio of cottonseed meal and mixed solvent is 1:4, and extraction temperature is 50 DEG C.
Further, the method extracting cottonseed protein from the cottonseed meal of dephenolize is: carry out lixiviate with the mixed aqueous solution of sodium hydroxide and S-WAT to the cottonseed meal of dephenolize, and vat liquor acid is heavy obtains cottonseed protein.
Further, the mass ratio of described sodium hydroxide and S-WAT is 5:(2 ~ 5).
Further, during lixiviate cottonseed protein, the total concn of sodium hydroxide and S-WAT is 25 ~ 35g/L.
Further, during mixed aqueous solution lixiviate with sodium hydroxide and S-WAT, extraction time is 0.5 ~ 1.5 hour.
Further, during mixed aqueous solution lixiviate with sodium hydroxide and S-WAT, extraction temperature is 50 ~ 70 DEG C.
Further, pH when vat liquor acid is heavy is 4 ~ 6.
The optimal conditions that cottonseed protein extracts is: the mass ratio of sodium hydroxide and S-WAT is 1:1, and the total concn of sodium hydroxide and S-WAT is 30g/L, solid-liquid ratio 1:15, and extraction time is 1 hour, and extraction temperature is 60 DEG C.
Accompanying drawing explanation
Fig. 1 is that the volume ratio of ethanol and normal hexane in mixed solvent is to the influence curve of gossypol decreasing ratio.
Fig. 2 is the influence curve of solid-liquid ratio to gossypol decreasing ratio.
Fig. 3 is the influence curve of extraction temperature to gossypol decreasing ratio.
Fig. 4 is the influence curve of mass ratio to cottonseed protein yield and purity of sodium hydroxide and S-WAT in immersion liquid.
Fig. 5 is extraction time to the influence curve of cottonseed protein yield and purity.
Fig. 6 is Extracting temperature to the influence curve of cottonseed protein yield and purity.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further details.
The preparation method of cottonseed protein is as follows:
(1) by cottonseed meal raw material pulverizing;
(2) the cottonseed meal ethanol pulverized and the mixed solvent lixiviate of normal hexane, remove the gossypol in cottonseed meal;
(3), after the cottonseed meal of dephenolize is separated with mixed solvent, the cottonseed meal of dephenolize is obtained;
(4) cottonseed meal of dephenolize adds water, then adds sodium hydroxide and S-WAT, extracts cottonseed protein;
(5) the dephenolization cottonseed dregs of rice are after lixiviate, isolate vat liquor, and acid adding regulates pH to 4 ~ 6 of vat liquor, and acid is heavy, and precipitation is cottonseed protein.
The inventive method has no particular limits cottonseed meal, can be that cottonseed gets the residue after oil through milling process, also can be the residue after adopting solvent extraction method to get oil, in following instance, cottonseed meal raw material be the residue after No. six solvent extraction methods carry oil, and gossypol content is 2230mg/kg.
Step (2) is extraction temperature 40 DEG C, extraction time 1h, solid-liquid ratio 1:3(w/v, g/ml) time, the volume ratio of ethanol and normal hexane on the impact of gossypol decreasing ratio as shown in Figure 1, as can be seen from Figure 1, ethanol and the more little decreasing ratio being more conducive to gossypol of normal hexane ratio value, as when ethanol and normal hexane volume ratio are 5:5, gossypol decreasing ratio can reach more than 80%, for decreasing ratio during 5:1 only has 70%, therefore, during lixiviate, the volume ratio of ethanol and normal hexane controls in (1 ~ 5): 5.
Step (2) is temperature 40 DEG C, time 1h, time mixed solvent (ethanol: normal hexane=5:5), on the impact of gossypol decreasing ratio as shown in Figure 2, as can be seen from Figure 2, solid-liquid ratio is 1:3(g/ml to solid-liquid ratio) gossypol decreasing ratio can reach more than 80%, by comparison, when solid-liquid ratio is 1:1, gossypol decreasing ratio is low by 10%, and therefore, the solid-liquid ratio of cottonseed meal and mixed solvent controls in 1:(3 ~ 6).
Step (2) is at time 1h, mixed solvent (ethanol: normal hexane=5:5), solid-liquid ratio 1:3(g/ml) time, extraction temperature is on the impact of gossypol decreasing ratio as shown in Figure 3, as can be seen from Figure 3, extraction temperature can make gossypol decreasing ratio reach more than 80% at 40 ~ 50 DEG C.
The cottonseed meal of step (3) dephenolize can adopt prior art to carry out with being separated of mixed solvent, as squeezing, filtration, distillation, centrifugation etc.
When step (4) cottonseed protein extracts, sodium hydroxide and S-WAT total concn can be controlled in 25 ~ 35g/L.
Step (4) is at solid-liquid ratio 1:10, sodium hydroxide and S-WAT total concn are 30g/L, temperature 20 DEG C, during time 1h, sodium hydroxide and S-WAT under different mass ratio on the impact of cottonseed protein yield and purity as shown in Figure 4, as can be seen from Figure 4, the impact of different mass comparison cottonseed protein yield and purity is just in time contrary, in general, the mass ratio of sodium hydroxide and S-WAT controls in 5:(2 ~ 5), can high yield and purity be obtained.
Step (4) is temperature 20 DEG C, sodium hydroxide and S-WAT total concn are 30g/L, the mass ratio of sodium hydroxide and S-WAT is 5:5, and during solid-liquid ratio 1:10, extraction time on the impact of cottonseed protein yield and purity as shown in Figure 5, as can be seen from Figure 5, although extraction time is longer, cottonseed protein yield is higher, and cottonseed protein purity is fallen after rising on the contrary, therefore, extraction time is easy to control at 0.5 ~ 1.5 hour.
Step (4) is 1h in extraction time, sodium hydroxide and S-WAT total concn are 30g/L, the mass ratio of sodium hydroxide and S-WAT is 5:5, and during solid-liquid ratio 1:10, Extracting temperature on the impact of cottonseed protein yield and purity as shown in Figure 6, as can be seen from Figure 6, temperature is comparatively complicated on the impact of the purity of cottonseed protein, and humidity more high yield pulp1 is corresponding also higher, therefore, when ensureing purity, Extracting temperature controls at 50 ~ 70 DEG C.
Step (5) vat liquor adjust pH time, available common are machine acid or mineral acid, example hydrochloric acid, sulfuric acid, nitric acid, acetic acid etc.
the mensuration of gossypol content
Undertaken by " in animal-feed measuring method that is free and total gossypol " ISO 6866-1985.
Take 1-2g sample (to be accurate to 0.001 g), to be placed in 250ml tool plug Erlenmeyer flask, to add 20 granulated glass spherees, accurately add 50mL solvent orange 2 A with transfer pipet, jam-pack bottle stopper, put into vibrator vibration 1h (per minute about 120 times).Filter with the quantitative paper of drying, on funnel, add a cover a watch glass during filtration to reduce solvent evaporates, discard several filtrates at first, collect filtrate in 100mL tool plug Erlenmeyer flask.
With in valinche draws equal amounts double filtrate 5-10mL (every part about containing the gossypol of 50-100 μ g) brown volumetric flask a and b of respectively to two 25mL, if needed, be supplemented to 10 mL with solvent orange 2 A.
With Virahol-normal hexane mixed solvent dilution bottle a to scale, shake up, this solution is used as the reference solution of Specimen Determination liquid.
With the brown volumetric flask a of solvent orange 2 A respectively to two 25mL of pipette, extract 2 parts of 10mL
0and b
0in.
Bottle a is supplemented with Virahol-normal hexane mixed solvent
0to scale, shake up, this solution is used as the reference solution of blank determination liquid.
Add 2.0mL aniline in volumetric flask b and b
0in, boiling water bath heats 30min colour developing.
Be cooled to room temperature, with Virahol-normal hexane mixed solvent constant volume, shake up and leave standstill 1h.
Use 10mm colorimetric pool, at wavelength 440nm place, with spectrophotometer with a
0for reference solution measures blank determination liquid b
0absorbancy, take a as the absorbancy that reference solution measures Specimen Determination liquid b, from the absorbance of Specimen Determination liquid, deduct the absorbance of blank determination liquid, obtain correcting absorbance A.
Calculation formula:
In formula: X--free gossypol content, mg/kg;
A--corrects absorbancy;
M--sample mass, g;
V--measures the volume with filtrate, mL;
A--mass absorption coefficient, free gossypol is 62.5cm
-1g
-1l.
Recording total free gossypol content in cottonseed meal raw material is: 2230mg/kg.
Gossypol decreasing ratio: i.e. dephenolize gossypol efficiency, the larger removal effect of its value is better.
Calculation formula:
In formula: Y---gossypol decreasing ratio in cottonseed meal
M
always---gossypol content total in cottonseed
M
sample---gossypol content after sample dephenolize.
Solvent orange 2 A compound method: measure about 500mL Virahol, normal hexane mixed solvent (normal hexane: Virahol=6:4(v:v)), 2 mL 3-amino-1-propyl alcohol, 8 mL glacial acetic acids and 50 mL water in the volumetric flask of 1000 mL, then are settled to scale with normal hexane-isopropyl alcohol mixed solvent.
embodiment 1
(1) cottonseed meal is pulverized;
(2) the cottonseed meal ethanol pulverized and the mixed solvent lixiviate of normal hexane, remove the gossypol in cottonseed meal, wherein, the volume ratio of ethanol and normal hexane is 4:5, and the solid-liquid ratio of cottonseed meal and mixed solvent is 1:4(w/v, g/ml), extraction temperature is 50 DEG C, 1 hour time, gossypol decreasing ratio is 89.60%, dephenolize cotton dregs Free Gossypol (FG)≤400mg/kg;
(3), after the cottonseed meal of dephenolize is separated with mixed solvent, the cottonseed meal of dephenolize is obtained;
(4) cottonseed meal of dephenolize adds water, add sodium hydroxide and S-WAT again, extract cottonseed protein, wherein, the solid-liquid ratio of dephenolize cotton dregs and immersion liquid is 1:15, and temperature is 60 DEG C, and extraction time is 1h, in immersion liquid, the mass ratio of sodium hydroxide and S-WAT is 1:1, and the total concn of sodium hydroxide and S-WAT is 30g/L;
(5) the dephenolization cottonseed dregs of rice are after lixiviate, isolate vat liquor (supernatant liquor), and acid adding regulates the pH to 4.8 of vat liquor, and the heavy 10min of acid, centrifugal, precipitation is cottonseed protein, and cottonseed protein yield is 61.44%, and purity is 91.5%.
Claims (3)
1. the preparation method of a cottonseed protein, cottonseed protein is extracted in the dephenolize and (2) that comprise (1) cottonseed meal from the cottonseed meal of dephenolize, it is characterized in that, the dephenolize of cottonseed meal is the mixed solvent lixiviate cottonseed meal with ethanol and normal hexane, and wherein, the volume ratio of described ethanol and normal hexane is (1 ~ 5): 5, during dephenolize, the solid-liquid ratio of cottonseed meal and mixed solvent is 1:(3 ~ 6), during dephenolize, extraction temperature is 40 ~ 50 DEG C;
With the mixed aqueous solution of sodium hydroxide and S-WAT, lixiviate is carried out to the cottonseed meal of dephenolize, vat liquor acid is heavy obtains cottonseed protein, the mass ratio of described sodium hydroxide and S-WAT is 5:(2 ~ 5), during lixiviate, the total concn of sodium hydroxide and S-WAT is 25 ~ 35g/L, during mixed aqueous solution lixiviate with sodium hydroxide and S-WAT, extraction time is 0.5 ~ 1.5 hour, and extraction temperature is 50 ~ 70 DEG C.
2. the preparation method of cottonseed protein according to claim 1, is characterized in that: the volume ratio of described ethanol and normal hexane is (1 ~ 4): 5.
3. the preparation method of cottonseed protein according to claim 1, is characterized in that: pH when vat liquor acid is heavy is 4 ~ 6.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103875999A (en) * | 2014-03-07 | 2014-06-25 | 袁峻峰 | Cottonseed meal puffing and detoxifying method |
| CN104402967B (en) * | 2014-12-03 | 2018-02-06 | 环境保护部南京环境科学研究所 | One kind rapid extraction method of protein from simple grain cottonseed cotton-wool |
| CN106306329A (en) * | 2015-06-25 | 2017-01-11 | 南通海辰蛋白科技有限公司 | Extraction technology of cottonseed proteins |
| CN107011411B (en) * | 2017-04-28 | 2020-12-18 | 济南中棉生物科技有限公司 | Cottonseed protein production method capable of extracting multiple byproducts |
| CN110606866A (en) * | 2019-10-25 | 2019-12-24 | 仲恺农业工程学院 | Method for refining cottonseed protein |
| CN113768043A (en) * | 2021-08-09 | 2021-12-10 | 武汉轻工大学 | Method for reducing content of free gossypol in cottonseed meal and feed |
| CN115651760A (en) * | 2022-09-21 | 2023-01-31 | 新疆冠农果茸股份有限公司 | Cottonseed mixed oil refining method |
| CN116235895A (en) * | 2023-03-14 | 2023-06-09 | 西南科技大学 | Method for preparing food emulsifier based on cottonseed protein isolate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1919035A (en) * | 2006-09-21 | 2007-02-28 | 郑州新力德粮油科技有限公司 | Dephenolizing cotton protein producing method by cottonseed cold press mixed solvent primary leaching |
| CN102372763A (en) * | 2011-10-31 | 2012-03-14 | 新疆银隆农业国际合作股份有限公司 | Preparation method for industrial cotton seed protein, product prepared with same and application thereof |
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| PL2498619T3 (en) * | 2009-11-11 | 2017-10-31 | Siebte Pmi Verwaltungs Gmbh | Protein concentrates and isolates, and processes for the production thereof from toasted oilseed meal |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1919035A (en) * | 2006-09-21 | 2007-02-28 | 郑州新力德粮油科技有限公司 | Dephenolizing cotton protein producing method by cottonseed cold press mixed solvent primary leaching |
| CN102372763A (en) * | 2011-10-31 | 2012-03-14 | 新疆银隆农业国际合作股份有限公司 | Preparation method for industrial cotton seed protein, product prepared with same and application thereof |
Non-Patent Citations (3)
| Title |
|---|
| 棉籽脱毒技术;程霜;《四川粮油科技》;20010930(第3期);第17页右栏第2段、第18页左栏倒数第1段-右栏第1段及表2 * |
| 棉籽蛋白提取工艺的研究;陈琳等;《沈阳化工学院学报》;20091231;第23卷(第4期);第351-353页2.1碱法及盐类提取蛋白质工艺、2.2蛋白质纯度测试及结果、表1和表2、图1和图2 * |
| 综述棉籽的深加工及综合利用;郑晓吉等;《安徽农学通报》;20090610;第15卷(第11期);第55-57页 * |
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