CN100370011C - Method for extracting pumpkin seed oil and pumpkin seed protein - Google Patents
Method for extracting pumpkin seed oil and pumpkin seed protein Download PDFInfo
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- CN100370011C CN100370011C CNB2005101151809A CN200510115180A CN100370011C CN 100370011 C CN100370011 C CN 100370011C CN B2005101151809 A CNB2005101151809 A CN B2005101151809A CN 200510115180 A CN200510115180 A CN 200510115180A CN 100370011 C CN100370011 C CN 100370011C
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Abstract
The present invention discloses a method for extracting pumpkinseed oil and pumpkinseed protein, which aims to provide a method for extracting pumpkinseed oil with abundant linoleic acid and pumpkinseed protein with abundant arginine. The method of the present invention for extracting pumpkinseed oil and pumpkinseed protein comprises the following steps: budding pumpkinseeds as raw materials are processed by jordaning and enzymolysis; the oil water mixture obtained by enzymolysis is separated to obtain an oil phase and an aqueous phase, wherein the oil phase is pumpkinseed oil, and the aqueous phase is pumpkinseed protein solution. The method of the present invention adopts budding pumpkinseeds as raw materials, thereby increasing the effective components of pumpkinseeds, removing the anti-nutritional factor of pumpkinseeds effectively and keeping the stability of the functional component of the pumpkinseed protein and pumpkinseed oil well. The method of the present invention solves the technical problem that a plurality of effective components are not efficiently extracted from pumpkinseeds simultaneously, and the method has the advantages of little production equipment investment, short process and easy industrialization.
Description
Technical field
The present invention relates to a kind of extraction Semen Cucurbitae oil and the proteic method of Semen Cucurbitae in the food industry applications technical field.
Background technology
The proteic evaluation and exploration technology of Semen Cucurbitae oil and Semen Cucurbitae is the difficult problem of restriction Semen Cucurbitae industrialized developing always.Contain a large amount of natural nutrient components in the Semen Cucurbitae, high-quality protein (about 30-56%), Semen Cucurbitae contains a large amount of natural fats and oils (accounting for the 35%-64.4% of dry weight) simultaneously.Vitamin-E is main liposoluble vitamin, wherein vitamin-E in the Semen Cucurbitae
3Content be the 41-620mg/kg dry weight, also contain a certain amount of phylloquinone.Semen Cucurbitae oil is rich in polyunsaturated fatty acids such as linolic acid, oleic acid, can effectively prevent eczema, has anti-allergic effects.Semen Cucurbitae oil can be eliminated prostatic initial stage swelling, and urinary system and hyperplasia of prostate are had good curing and prophylactic effect.Simultaneously, also contain antinutritional factor in the Semen Cucurbitae: Weibull, phytic acid and casein inhibitor etc. have influenced the nutritive value of Semen Cucurbitae.Conventional separation method is difficult to effectively preserve the nutritive ingredient in the Semen Cucurbitae and the antinutritional factor in the Semen Cucurbitae, Semen Cucurbitae oil and Semen Cucurbitae albumen is effectively separated, and improves its trophic function.
Extract grease as traditional milling process, the high temperature in the expressing process makes the processed oil color and luster darker, and the functional component in the grease is destroyed, and loses biological function, the high shortcoming of Residual oil content in squeezing back Semen Cucurbitae protein sex change at high temperature and the grouts; Supercritical liquid extraction technique, equipment funds have high input, and turnout is low, the production cost height; Organic solvent hexane extraction, the hexane recovery system has high input, and the volatilization of solvent causes pollution to a certain degree.
Summary of the invention
The purpose of this invention is to provide a kind of extraction is rich in linoleic Semen Cucurbitae oil and is rich in the proteic method of arginine Semen Cucurbitae.
Extraction Semen Cucurbitae oil provided by the present invention and the proteic method of Semen Cucurbitae may further comprise the steps:
1) is raw material with the Semen Cucurbitae of germinateing, carries out defibrination, enzymolysis;
2) oil-water mixture that enzymolysis is obtained separates, and oil phase is a Semen Cucurbitae oil, and water is the Semen Cucurbitae protein solution.
The bud length of the Semen Cucurbitae of described germination is no more than 0.5 centimetre.
The Semen Cucurbitae of described germination can obtain in accordance with the following methods: with Semen Cucurbitae at 35-40 ℃, germination treatment 3-5 days.
Described defibrination can be in the Semen Cucurbitae of germinateing and adds the laggard capable defibrination of entry, and the granularity that makes slurries is below 20 microns; The described amount that adds entry be the Semen Cucurbitae quality that is used to germinate 6-10 doubly.
Described enzymolysis can be the pH value of the slurries that defibrination is obtained and is transferred to 8.2-9.0, and at 45-50 ℃, rotating speed is that 100 times/minute shaking tables were handled 5-8 hour.This enzymolysis process becomes the solubility quality protein with the Semen Cucurbitae storage protein by the proteolytic ferment hydrolysis that produces in self germination process, effectively improves the arginine and the linoleic content of Semen Cucurbitae.
In order to improve hydrolysis result, protein and greasy binding site are interrupted, allow grease fully discharge, described enzymolysis also can be and add Alcalase 2.4L FG/Flavourzyme in the slurries that defibrination obtains, the pH value is transferred to 8.2-9,45-50 ℃ of reaction 5-8 hour; The add-on of described Flavourzyme is the 50-100U/ml slurries.
The add-on of described Alcalase 2.4 L FG/Flavourzyme is preferably the 60U/ml slurries.
For improving oil yield, the oil-water mixture that obtains behind the described enzymolysis is taked the rapid pyrolysis in rapid freezing back of-10 ℃～-15 ℃ temperature to freeze or is adopted the citric acid of adding 10% to make albumen flocculation sex change, separates oil phase.
Described separation employing is revolved fraction profit centrifuge separator and is separated.
Further comprising the steps of in the described method: it is 100,000 daltonian ultrafiltration membrance filters that described water is adopted molecular weight, and the filtrate that obtains is Semen Cucurbitae albumen.
Described filtrate can be in vacuum tightness less than-0.09MPa, and temperature is less than concentrating under 55 ℃ the condition or being reverse osmosis concentration under the 0.25-0.35MPa at pressure.
Method of the present invention adopts the Semen Cucurbitae of germinateing as raw material, improved the effective constituent of Semen Cucurbitae, compare with the Semen Cucurbitae of not germinateing, linoleic acid content in the Semen Cucurbitae of germinateing has increased by 12.02%, and the content of arginine, L-glutamic acid, leucine and aspartic acid has increased by 18.75%, 9.21%, 15.79%, 12.5% respectively.Linoleic acid content reaches the 17.71g/100g Semen Cucurbitae in the Semen Cucurbitae oil that method of the present invention obtains, and the arginine in the Semen Cucurbitae albumen, L-glutamic acid, leucine and aspartate content reach 2.62g/100g Semen Cucurbitae, 3.86g/100g Semen Cucurbitae, 1.30g/100g Semen Cucurbitae and 1.59g/100g Semen Cucurbitae respectively.Method of the present invention has been removed the antinutritional factor in the Semen Cucurbitae effectively, the stability that has kept the functional component of Semen Cucurbitae albumen and Semen Cucurbitae oil preferably, solved the technical matters problem of plurality of active ingredients in the high efficiency extraction Semen Cucurbitae simultaneously, improved content of effective, the production unit less investment, technology is brief, is easy to industrialization.
Description of drawings
Fig. 1 is the preparation flow figure that is rich in the instant Semen Cucurbitae albumen of arginine and is rich in the linolic acid Semen Cucurbitae oil.
Embodiment
Experimental technique among the following embodiment if no special instructions, is ordinary method.
Embodiment 1, the preparation of being rich in the instant Semen Cucurbitae albumen of arginine and being rich in the linolic acid Semen Cucurbitae oil.
The preparation flow that is rich in the instant Semen Cucurbitae albumen of arginine and is rich in the linolic acid Semen Cucurbitae oil as shown in Figure 1, concrete steps are as follows:
1, select full seed, the Semen Cucurbitae 100g of no mechanical injury and disease and pest supplies with adequate water at 35 ℃, carries out the germination treatment of 3-5d, and selection bud length is no more than 0.5 centimetre seedling as raw material.
2, the pumpkin seedling and without the amino acid of the Semen Cucurbitae of germination treatment and linoleic acid content measure according to document (the Han Yashan chief editor. " food chemistry experiment instruction ". China Agricultyre University Press, 1996.) method described carries out, step is as follows:
Raw material → drying → pulverize → sieve → weigh → filter paper pocket → usefulness the ether of packing into refluxes in soxhlet's extractor and got oil sample in 3 hours.
Amino acid whose mensuration: hydrochloric acid hydrolysis is measured 15 seed amino acids except that methionine(Met), Gelucystine and tryptophane, measures with Hitachi's L-8800 amino acidanalyser.
The lithium hydroxide of the mensuration of tryptophane: 4mol/L, 110 ℃, after the hydrolysis in 24 hours, 6mol/L hydrochloric acid is neutralized to pH4.3,50ml volumetric flask constant volume, the centrifuging and taking supernatant liquor separates with the anti-phase liquid spectrum of Tianjin, island LC10A, and Tianjin, island SPD10A UV-detector detects.
The mensuration of methionine(Met), Gelucystine: adopt GB/P 18246-2000 method.
Carry out 3 times with the test of upper amino acid sample and repeat, wherein two groups of parallel sample relative deviations are got mean value as a result less than 10.
The pumpkin seedling of determination step 1 and show without the result of the various aminoacids contents of the Semen Cucurbitae of germination treatment, the amino acid whose content of spent meal of the pumpkin seedling of step 1 is the 18.73g/100g Semen Cucurbitae, the amino acid whose content of spent meal without the Semen Cucurbitae of germination treatment is the 16.74g/100g Semen Cucurbitae, and the spent meal aminoacids content of pumpkin seedling has increased by 11.89% than the Semen Cucurbitae without germination treatment.
The pumpkin seedling of determination step 1 and without the aminoacids content of the Semen Cucurbitae of germination treatment according to the method described above, the result shows that the proteic arginic content of the pumpkin seedling of step 1 is the 2.66g/100g Semen Cucurbitae, without the proteic arginic content of the Semen Cucurbitae of germination treatment is the 2.24g/100g Semen Cucurbitae, and the arginine content of pumpkin seedling has increased by 18.75% than the Semen Cucurbitae without germination treatment; The content of the proteic L-glutamic acid of pumpkin seedling of step 1 is the 3.91g/100g Semen Cucurbitae, content without the proteic L-glutamic acid of Semen Cucurbitae of germination treatment is the 3.58g/100g Semen Cucurbitae, and the L-glutamic acid content of pumpkin seedling has increased by 9.22% than the Semen Cucurbitae without germination treatment; The proteic leucic content of the pumpkin seedling of step 1 is the 1.32g/100g Semen Cucurbitae, the content of aspartic acid is the 1.62g/100g Semen Cucurbitae, the content that is 1.14g/100g Semen Cucurbitae, aspartic acid without the proteic leucic content of the Semen Cucurbitae of germination treatment is the 1.44g/100g Semen Cucurbitae, and the leucic content of pumpkin seedling, the content of aspartic acid have increased by 15.79% and 12.5% respectively than the Semen Cucurbitae without germination treatment.
Measure linoleic acid content in the Semen Cucurbitae:
Adopt the HP6890 gas chromatography to measure linoleic acid content, chromatographiccondition is: the opening for feed temperature: 220 ℃; Splitting ratio is: 20: 1.Chromatographic column HP19091N-2B (30m * 320 μ m * 0.50 μ m); Nitrogen constant current speed is: 3.1ml/min.Post case heating schedule: 200 ℃ keep 10min after, be warming up to 220 ℃ with the speed of 10 ℃/min and keep 4min; Speed with 2 ℃/min is warming up to 230 ℃ of maintenances 5 minutes; Being warming up to 250 ℃ with 10 ℃/minute speed kept 2 minutes.Hydrogen flame detector: temperature is 275 ℃.Hydrogen flow rate: 45ml/min; Air velocity 450ml/ branch.
According to the pumpkin seedling of the method determination step 1 of foregoing description and 100g linoleic acid content without the Semen Cucurbitae of germination treatment, the result shows that the linoleic content in the pumpkin seedling grease of step 1 is the 18.83g/100g Semen Cucurbitae, without linoleic content in the grease of the Semen Cucurbitae of germination treatment is the 16.81g/100g Semen Cucurbitae, and the linoleic acid content of pumpkin seedling has increased by 12.02% than the Semen Cucurbitae without germination treatment.
3, defibrination
The pumpkin seedling of cleaning step 1 is fully soaked, and cleans the adhesion that produces because of germination process.After adopting 2% (percentage) hydrogen peroxide cleaning and sterilization then, adopt pure water to clean.Add raw material and weigh 6 times of water,, the slurry granularity is controlled at below 20 microns with the abundant defibrination of colloidal mill.
4, enzymolysis
The pH value of the slurries that step 3 is obtained transfers to pH8.5, is 40 ℃ in temperature and places 2 hours down.Add the Alcalase 2.4L FG/Flavourzyme of NOVO company subsequently in slurries, its add-on is the 60U/ml slurries.The pH value is transferred to 9, and at 50 ℃, rotating speed is 100 times/minute shaking table reactions 5 hours.
5, profit centrifugation
After citric acid with 10% transfers to 6 with the pH of enzymolysis solution,, adopt and revolve the fraction oily water separation technique, Semen Cucurbitae oil is separated according to the density variation of grease and water and emulsion.Employing is revolved fraction profit centrifuge separator and is carried out the profit centrifugation, continuously Semen Cucurbitae oil is separated, and upper oil phase is taken out, and per 100 gram Semen Cucurbitae obtain the 44.14g Semen Cucurbitae oil.According to the linoleic acid content in the method mensuration Semen Cucurbitae oil of foregoing description, the result shows that linoleic content is the 40.12g/100g Semen Cucurbitae oil, is scaled the 17.71g/100g Semen Cucurbitae, and linoleic extraction yield is 94.04%.
It is 7-8 that lower floor's water after centrifugal is adjusted pH value of solution with 5% sodium hydroxide solution, and adopting molecular weight is 100,000 daltonian ultrafiltration membrance filters.Right vacuum concentration, vacuum tightness should be less than-0.09Mpa, and thickening temperature is less than 55 ℃.Carry out spraying drying again after concentrating, spraying drying air outlet temperature is less than 92 ℃, and per 100 gram Semen Cucurbitae obtain the instant protein powder of 50.6g.
Method according to foregoing description is measured spent meal aminoacids content in the Semen Cucurbitae protein powder: the result shows that the amino acid whose content of spent meal is the 17.69g/100g Semen Cucurbitae, and the amino acid whose extraction yield of spent meal is 94.46%.
Measure the aminoacids content of Semen Cucurbitae protein powder according to the method described above, and be scaled the content in the 100g Semen Cucurbitae, the result shows that the arginic content of Semen Cucurbitae protein powder is the 2.62g/100g Semen Cucurbitae, and arginic extraction yield is 98.49%; The content of the L-glutamic acid of Semen Cucurbitae protein powder is the 3.86g/100g Semen Cucurbitae, and the extraction yield of L-glutamic acid is 98.72%; The leucic content of Semen Cucurbitae protein powder is the 1.30g/100g Semen Cucurbitae, and leucic extraction yield is 98.48%; The content of the aspartic acid of Semen Cucurbitae protein powder is the 1.59g/100g Semen Cucurbitae, and the extraction yield of aspartic acid is 98.15%.
Claims (10)
1. one kind is extracted Semen Cucurbitae oil and the proteic method of Semen Cucurbitae, may further comprise the steps:
1) is raw material with the Semen Cucurbitae of germinateing, carries out defibrination; The pH value of the slurries that obtain is transferred to 8.2-9, places at 45-50 ℃ and carried out enzymolysis in 5-8 hour;
2) oil-water mixture that enzymolysis is obtained separates, and oil phase is a Semen Cucurbitae oil, and water is the Semen Cucurbitae protein solution.
2. method according to claim 1 is characterized in that: the bud length of the Semen Cucurbitae of described germination is no more than 0.5 centimetre.
3. method according to claim 2 is characterized in that: the Semen Cucurbitae of described germination obtains in accordance with the following methods: with Semen Cucurbitae at 35-40 ℃, germination treatment 3-5 days.
4. method according to claim 1 is characterized in that: described defibrination is for adding the laggard capable defibrination of entry in the Semen Cucurbitae of germinateing, the granularity that makes slurries is below 20 microns; The described amount that adds entry be the Semen Cucurbitae quality that is used to germinate 6-10 doubly.
5. according to claim 1,2,3 or 4 described methods, it is characterized in that: described enzymolysis was transferred to 8.2-9 for add Alcalase 2.4 L FG/Flavourzyme in the slurries that defibrination obtains with the pH value, 45-50 ℃ of shaking table reaction 5-8 hour; The add-on of described Alcalase 2.4 L FG/Flavourzyme is the 50-100U/ml slurries.
6. method according to claim 5 is characterized in that: the add-on of described FG/Flavourzyme is the 60U/ml slurries.
7. method according to claim 1, it is characterized in that: the oil-water mixture that obtains behind the described enzymolysis is taked-10 ℃～-15 ℃ rapid pyrolysis in rapid freezing back to freeze or is adopted the citric acid of adding 10% to make the pH of enzymolysis solution transfer to 6 back albumen flocculations, separates oil phase.
8. according to claim 1,2,3 or 4 described methods, it is characterized in that: described separation employing is revolved fraction profit centrifuge separator and is separated.
9. according to claim 1 or 2 or 3 or 4 described methods, it is characterized in that: further comprising the steps of in the described method: described water is adjusted pH value 7-8 with 5% sodium hydroxide solution, adopting molecular weight is 100,000 daltonian ultrafiltration membrance filters, and the filtrate that obtains is Semen Cucurbitae albumen.
10. method according to claim 9 is characterized in that: less than-0.09MPa, temperature is less than concentrating under 55 ℃ the condition or being reverse osmosis concentration under the 0.25-0.35MPa at pressure in vacuum tightness for described filtrate; Carry out spraying drying again after concentrating, described spray-dired air outlet temperature is less than 92 ℃.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101455240B (en) * | 2008-12-29 | 2011-04-06 | 东北农业大学 | Pumpkin seed oil extraction method using water enzyme method |
| RU2550076C2 (en) * | 2013-04-16 | 2015-05-10 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Астраханский государственный университет" | Method for production and composition of pumpkin seed oil |
| CN106433966A (en) * | 2016-10-21 | 2017-02-22 | 乌鲁木齐上善元生物科技有限公司 | Production equipment for preparing safflower seed oil through freeze refining method |
| CN109938116A (en) * | 2019-04-01 | 2019-06-28 | 湖南康琪壹佰生物科技有限公司 | A kind of pumpkin seed oil and preparation method thereof improving prostatic function |
| CN112410113A (en) * | 2019-08-23 | 2021-02-26 | 黑龙江赛美生物科技开发有限公司 | Method for preparing pumpkin seed oil by industrial enzyme method |
| CN113881488A (en) * | 2020-08-17 | 2022-01-04 | 丰益(上海)生物技术研发中心有限公司 | Strong-fragrance grease and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1263107A (en) * | 1999-02-11 | 2000-08-16 | 中国科学院福建物质结构研究所 | Ribosome deactivated protein-pumpkin protein |
| CN1393144A (en) * | 2001-07-02 | 2003-01-29 | 刘仁健 | Health-care food and composite beverage made of pumpkin and its preparing process |
| CN1491586A (en) * | 2003-09-02 | 2004-04-28 | 江南大学 | Method for preparing pumpkin mixed juice by enzyme engineering technology |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1263107A (en) * | 1999-02-11 | 2000-08-16 | 中国科学院福建物质结构研究所 | Ribosome deactivated protein-pumpkin protein |
| CN1393144A (en) * | 2001-07-02 | 2003-01-29 | 刘仁健 | Health-care food and composite beverage made of pumpkin and its preparing process |
| CN1491586A (en) * | 2003-09-02 | 2004-04-28 | 江南大学 | Method for preparing pumpkin mixed juice by enzyme engineering technology |
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