CN102504946B - Method for refining camellia seed crude oil beneficial to people with high blood pressure, high blood sugar and high blood fat - Google Patents
Method for refining camellia seed crude oil beneficial to people with high blood pressure, high blood sugar and high blood fat Download PDFInfo
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- Fats And Perfumes (AREA)
- Edible Oils And Fats (AREA)
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Abstract
The invention relates to a method for refining camellia seed crude oil, in particular to a method for refining camellia seed crude oil by using immobilized phospholipase A1. The technical scheme of the invention is realized by refining the crude oil of the camellia seeds by using the immobilized phospholipase A1 through the following steps: a. an immobilized phospholipase; b. performing pretreatment on crude oil of camellia seeds; c. adding immobilized phospholipase into the crude oil of the camellia seeds; d. and (4) stirring and centrifuging to realize refining of the camellia seed crude oil by using the immobilized phospholipase A. The method for refining the camellia seed crude oil has the beneficial effects that the loss of unsaturated fatty acid in the method for refining the camellia seed crude oil is 1-3%, and is reduced by 15-20% compared with the method for chemically refining the camellia seed oil. And the degumming of the immobilized phospholipid A1 can reduce the phosphorus content in the oil to be below 5mg/kg, improve the heat resistance of the immobilized phospholipase A1, keep higher activity in a wider pH range, reduce the sensitivity to the reaction environment and ensure that the operation condition is easier to control and implement.
Description
Technical field
The present invention relates to a kind of method of refining oil-tea camellia seed crude oil, relate in particular to a kind of method of utilizing the oil-tea camellia seed crude oil of immobilized phospholipase A1 to carry out refining.
Background technology
Tea seed (camellia Oleifera Ahel) is the distinctive woody oleiferous plants of China, mainly is distributed in mountain area and the hills of southern 14 provinces of China (district), and the whole nation has camellia oleifera lam to be about 4,000,000 hectares at present.Produce tea seed per year above 600,000 tons.The tea oil that extracts from the oil tea seed has very high nutritive value and nourishing function, and its lipid acid is formed similar to sweet oil, and the title of " east sweet oil " is arranged.Contain tea-polyphenol and camellianin in the tea oil, abundant VE, VD, VK and carotene and squalene, long-term edible, can strengthen blood vessel elasticity and toughness, delay atherosclerosis, increase the stomach absorptive function, promote internal secretion body of gland hormone secretion, the control neural function descends, and improves body immunity etc.Tea oil is classified as the healthy edible vegetables oil that emphasis is promoted by Food and Argriculture OrganizationFAO.
Camellia seed oil is commonly called as tea oil, has another name called Camellia oil, camellia seed oil, is the senior edible vegetable oil of pure natural that extracts common oil tea (the Camellia oleifera Abel) mature seed from Theaceae Camellia plant.Oil tea is commonly called as camellia, wild tea, spends tea in vain, is the distinctive a kind of high-quality edible oil materials plant of China.
Tea oil (camellia Oil) is the high-quality healthy edible vegetable oil fat that extracts from tea seed, is the natural green food of a kind of natural, health, health care, and good reputations such as " long life oil ", " king in the oil " are arranged.
Tea oil is to be grouped into by one-tenth such as lipid acid, camellin, phospholipid, saponin(e, vitamin-E, tannins.The unsaturated fatty acid content of Camellia oil is abundant, up to 93%.Wherein monounsaturated fatty acids content has surpassed more than 75%, have in addition up to 90%.All the other are only multiple unsaturated fatty acidss such as linolic acid, linolenic acid.
Coming unstuck is a important step in the vegetable oil refining process, is the prerequisite that guarantees that physical refining carries out smoothly, most important to improving refining yield and oil quality.Colloid removes not thorough, has both influenced the deep processing of oil product and the stability of oil product, also influences the cooking consumption of oil product.The main purpose of coming unstuck is the phosphatide that removes in the oil, and phosphatide divides hydrated phospholipid and nonhydratable phosphatide, in degumming technology, hydrated phospholipid can be removed by the method for simple hydration degum, nonhydratable phosphatide has obvious hydrophobic, difficulty is combined with water in hydration degum, removes comparatively difficulty.Unsaturated fatty acid content is higher in the tea oil, accounts for about 80%, uses chemical degumming, and is temperature required higher, and easily the contained unsaturated fatty acids of oxidation tea oil causes the more original effects of tea-seed oil to be affected.The pigment material that forms because temperature is too high can be deepened the color of tea oil, and this type of material decolorization in the back is difficult to remove, and this has just influenced the quality of processed oil.
Development through decades, particularly physical refining successful implementation, people have released multiple Degumming method, as utilize that traditional hydration degum, simple acid system come unstuck, Special comes unstuck and enzyme method for degumming etc., it is a new and high technology of oil and fat refining that applying immobilized phospholipase A1 (all subscripts all should become normal digital 1) comes unstuck, and this technology has huge using value aspect the economic benefit that improves oil prodution industry and the environmental-protecting performance.
Summary of the invention
Purpose of the present invention at first is to have guaranteed in the refining process that unsaturated fatty acids is not destroyed in the tea-seed oil, especially linolic acid and linolenic acid, and the ratio of these two kinds of unsaturated fatty acidss directly affects the effect of tea-seed oil.
Technical scheme of the present invention may further comprise the steps for a kind of refining oil-tea camellia seed crude oil method useful to three high crowds is provided:
A, phospholipase A1 is joined the pH value is among 7 the HAc-NaAc or citric acid solution, obtains enzyme liquid, and the concentration of the phospholipase A1 of described enzyme liquid is 1-3mg/ml; To be 6-9 with the volume ratio with enzyme liquid through pretreated macroporous resin: 1 ratio be mixed, and obtains mixed solution; The container that takes up mixed solution is placed on the shaking table with 150-180 rev/min tachyphylaxis 2-4 hour, add concentration then and be glutaraldehyde cross-linking 1-6 hour of 0.03-0.24%, crosslinking temperature control is at 3-15 ℃, filter cake is collected in vacuum filtration, gained is immobilized phospholipase A1, to put into refrigerator, standing and drying in 0-5 ℃ after the filter cake dispersion;
B, get oil-tea camellia seed crude oil and remove hydrated phospholipid in the oil-tea camellia seed crude oil through the hydration degum method, adding mass concentration in the treated oil-tea camellia seed crude oil then is the citric acid solution of 40-50%, the quality of described citric acid solution is the 0.1-2% of oil-tea camellia seed crude oil, and stirred 10-30 minute with 1000-1500 rev/min speed, it is 6.0-7.5 that the NaOH solution that adds mass concentration again in the treated oil-tea camellia seed crude oil and be 2-4% makes the pH value of oil-tea camellia seed crude oil;
The immobilized phospholipase A1 that adds the 0.05-0.5% of oil-tea camellia seed crude oil quality in c, the oil-tea camellia seed crude oil that under 40-60 ℃ of condition, obtains in the described step b;
D, the oil-tea camellia seed crude oil that the adds immobilized phospholipase A1 speed with 50-120 rev/min was stirred 3-8 hour, again with the centrifugal 3-5 of 8000-10000 rev/min speed minute, remove the impurity in the heavy phase, namely obtain the refining oil-tea camellia seed crude oil.
Preferably, among a of step described in the aforesaid method 20-50mg phospholipase A1 being joined 200-500mL, pH value is among 7 the HAc-NaAc or citric acid solution.
Preferably, among the b of step described in the aforesaid method step of pre-treatment macroporous resin for to be soaked in the dehydrated alcohol macroporous resin standby.
Preferably, adding mass concentration among the c of step described in the aforesaid method in the treated oil-tea camellia seed crude oil is that to make the pH value of oil-tea camellia seed crude oil be 6.5-7.2 for 3% NaOH solution.
Preferably, the immobilized enzyme that adds the 0.25-0.48% of oil-tea camellia seed crude oil quality in the oil-tea camellia seed crude oil that under 55-58 ℃ of condition, obtains in the described steps d among the c of step described in the aforesaid method.
Preferably, 0.25% the immobilized enzyme that adds the oil-tea camellia seed crude oil quality in the oil-tea camellia seed crude oil that under 56 ℃ of conditions, obtains in the described steps d among the c of step described in the aforesaid method.
Preferably, in the steps d oil-tea camellia seed crude oil that the adds immobilized enzyme speed with 100-120 rev/min was stirred 3-8 hour described in the aforesaid method, and with 9000 rev/mins speed centrifugal 4 minutes.
Preferably, may further comprise the steps in the aforesaid method:
A, the 25mg phospholipase A1 is joined 250mL, pH value is among 7 the HAc-NaAc or citric acid solution, obtains enzyme liquid, and the concentration of the phospholipase A1 of described enzyme liquid is 1mg/ml; To be that 7: 1 ratio is mixed with volume ratio through pretreated macroporous resin and enzyme liquid, obtain mixed solution; The container that takes up mixed solution is placed on the shaking table with 160 rev/mins tachyphylaxis 3 hours, added concentration then and be 0.2% glutaraldehyde cross-linking 3 hours, crosslinking temperature control is at 9 ℃, filter cake is collected in vacuum filtration, gained is immobilized phospholipase A1, to put into refrigerator, standing and drying in 2 ℃ after the filter cake dispersion;
B, get oil-tea camellia seed crude oil and remove hydrated phospholipid in the oil-tea camellia seed crude oil through the hydration degum method, adding mass concentration in the treated oil-tea camellia seed crude oil then is the citric acid solution of 40-50%, the quality of described citric acid solution is 1% of oil-tea camellia seed crude oil, and stirred 20 minutes with 1200 rev/mins speed, adding mass concentration again in the treated oil-tea camellia seed crude oil and be 3% NaOH solution, to make the pH value of oil-tea camellia seed crude oil be 7;
0.3% the immobilized phospholipase A1 that adds the oil-tea camellia seed crude oil quality in c, the oil-tea camellia seed crude oil that under 40-60 ℃ of condition, obtains in the described step b;
D, the oil-tea camellia seed crude oil that the adds immobilized phospholipase A1 speed with 50-120 rev/min was stirred 5 hours, again with the centrifugal 3-5 of 8000-10000 rev/min speed minute, remove the impurity in the heavy phase, namely obtain the refining oil-tea camellia seed crude oil.
Beneficial effect of the present invention is that unsaturated fatty acids has lost 1-3% in the method for refining oil-tea camellia seed crude oil of the present invention, has reduced 15-20% than chemical refining camellia seed oil.And immobilization phosphatide A1 comes unstuck and phosphorus content in the oil can be dropped to below the 5mg/kg, the thermotolerance of the phospholipase A1 after the immobilization is improved, can in wideer pH scope, keep higher activity, the susceptibility of reaction environment is reduced, make the easier control of operational condition and enforcement.But more than the phospholipase A1 successive reaction 20h after the immobilization, can also recycle and reuse, enzymic activity still keeps more than 50% after 5 times, improved the efficient of coming unstuck, improved 10-30% than existing method, reduced production costs, cost has reduced 30-50% than existing method, but the high long-time continuous operation of the present invention's stability, the present invention can carry out the large-scale industry operation.
Embodiment
By describing technology contents of the present invention, structural attitude in detail, realized purpose and effect, give explanation below in conjunction with embodiment is detailed.
Embodiment 1
Realize by following steps with immobilized phospholipase A1 refining oil-tea camellia seed crude oil in the present embodiment:
A, the 5mg phospholipase A1 is joined 50ml, the pH value is among 7 the HAc-NaAc or citric acid solution, to obtain enzyme liquid, and the concentration of the phospholipase A1 of described enzyme liquid is 1mg/ml; To be that 6: 1 ratio is mixed with volume ratio through pretreated macroporous resin and enzyme liquid, obtain mixed solution; The container that takes up mixed solution is placed on the shaking table with 150 rev/mins tachyphylaxis 2 hours, added concentration then and be 0.03% glutaraldehyde cross-linking 1 hour, crosslinking temperature control is at 3 ℃, filter cake is collected in vacuum filtration, gained is immobilized phospholipase A1, to put into refrigerator, standing and drying in 0 ℃ after the filter cake dispersion;
B, get oil-tea camellia seed crude oil and remove hydrated phospholipid in the oil-tea camellia seed crude oil through the hydration degum method, adding mass concentration in the treated oil-tea camellia seed crude oil then is the citric acid solution of 40-50%, the quality of described citric acid solution is 0.1% of oil-tea camellia seed crude oil, and stirred 10 minutes with 1000 rev/mins speed, adding mass concentration again in the treated oil-tea camellia seed crude oil and be 2% NaOH solution, to make the pH value of oil-tea camellia seed crude oil be 6.0;
0.05% the immobilized phospholipase A1 that adds the oil-tea camellia seed crude oil quality in c, the oil-tea camellia seed crude oil that under 40 ℃ of conditions, obtains in the described step b;
Carry out after refining oil-tea camellia seed crude oil handles with present embodiment, the phosphorus content of oil-tea camellia seed crude oil is at 3mg/kg, and phosphorus content has reduced more than 95% when not coming unstuck, and after measured, the enzyme activity of immobilized enzyme is between 50～80% in the present embodiment.
Be soaked in 500～600ml dehydrated alcohol 5～15g macroporous resin standby among the present embodiment step a.
Embodiment 2
Realize by following steps with immobilized phospholipase A1 refining oil-tea camellia seed crude oil in the present embodiment:
A, the 20mg phospholipase A1 is joined 100ml, the pH value is among 7 the HAc-NaAc or citric acid solution, to obtain enzyme liquid, and the concentration of the phospholipase A1 of described enzyme liquid is 1mg/ml; To be that 7: 1 ratio is mixed with volume ratio through pretreated macroporous resin and enzyme liquid, obtain mixed solution; The container that takes up mixed solution is placed on the shaking table with 170 rev/mins tachyphylaxis 3 hours, added concentration then and be 0.1% glutaraldehyde cross-linking 3 hours, crosslinking temperature control is at 3 ℃, filter cake is collected in vacuum filtration, gained is immobilized phospholipase A1, to put into refrigerator, standing and drying in 3 ℃ after the filter cake dispersion;
B, get oil-tea camellia seed crude oil and remove hydrated phospholipid in the oil-tea camellia seed crude oil through the hydration degum method, adding mass concentration in the treated oil-tea camellia seed crude oil then is the citric acid solution of 40-50%, the quality of described citric acid solution is 0.5% of oil-tea camellia seed crude oil, and stirred 20 minutes with 1200 rev/mins speed, adding mass concentration again in the treated oil-tea camellia seed crude oil and be 3% NaOH solution, to make the pH value of oil-tea camellia seed crude oil be 7;
0.3% the immobilized phospholipase A1 that adds the oil-tea camellia seed crude oil quality in c, the oil-tea camellia seed crude oil that under 50 ℃ of conditions, obtains in the described step b;
Carry out after refining oil-tea camellia seed crude oil handles with present embodiment, the phosphorus content of oil-tea camellia seed crude oil is at 5mg/kg, and phosphorus content has reduced more than 95% when not coming unstuck, and after measured, the enzyme activity of immobilized enzyme is between 50～80% in the present embodiment.
Embodiment 3
Realize by following steps with immobilized phospholipase A1 refining oil-tea camellia seed crude oil in the present embodiment:
A, the 50mg phospholipase A1 is joined 500ml, the pH value is among 7 the HAc-NaAc or citric acid solution, to obtain enzyme liquid, and the concentration of the phospholipase A1 of described enzyme liquid is 3mg/ml; To be that 9: 1 ratio is mixed with volume ratio through pretreated macroporous resin and enzyme liquid, obtain mixed solution; The container that takes up mixed solution is placed on the shaking table with 180 rev/mins tachyphylaxis 4 hours, added concentration then and be 0.24% glutaraldehyde cross-linking 6 hours, crosslinking temperature control is at 15 ℃, filter cake is collected in vacuum filtration, gained is immobilized phospholipase A1, to put into refrigerator, standing and drying in 5 ℃ after the filter cake dispersion;
B, get oil-tea camellia seed crude oil and remove hydrated phospholipid in the oil-tea camellia seed crude oil through the hydration degum method, adding mass concentration in the treated oil-tea camellia seed crude oil then is the citric acid solution of 40-50%, the quality of described citric acid solution is 2% of oil-tea camellia seed crude oil, and stirred 30 minutes with 1500 rev/mins speed, adding mass concentration again in the treated oil-tea camellia seed crude oil and be 4% NaOH solution, to make the pH value of oil-tea camellia seed crude oil be 7.5;
The immobilized phospholipase A1 that adds the 0.05-0.5% of oil-tea camellia seed crude oil quality in c, the oil-tea camellia seed crude oil that under 40-60 ℃ of condition, obtains in the described step b;
D, the oil-tea camellia seed crude oil that the adds immobilized phospholipase A1 speed with 120 rev/mins was stirred 8 hours, with 10000 rev/mins speed centrifugal 5 minutes again, remove the impurity in the heavy phase, namely obtain the refining oil-tea camellia seed crude oil.
Carry out after refining oil-tea camellia seed crude oil handles with present embodiment, the phosphorus content of oil-tea camellia seed crude oil is at 4mg/kg, and phosphorus content has reduced more than 95% when not coming unstuck, and after measured, the enzyme activity of particulate state immobilized enzyme is between 50～80% in the present embodiment.
The different method of refining contrast of table 1 situation
As shown in table 1, the present invention compares with existing method of refining: unsaturated fatty acids has lost 1-3% in the method for refining oil-tea camellia seed crude oil of the present invention, has reduced 15-20% than enzymatic degumming.The storage rate of functional components such as squalene, vitamin-E and sterol is 92-95%, has improved 10-15% than additive method.And immobilization phosphatide A1 comes unstuck and phosphorus content in the oil can be dropped to below the 5mg/kg, the thermotolerance of the phospholipase A1 after the immobilization is improved, can in wideer pH scope, keep higher activity, the susceptibility of reaction environment is reduced, make the easier control of operational condition and enforcement.But more than the phospholipase A1 successive reaction 20h after the immobilization, can also recycle and reuse, enzymic activity still keeps more than 50% after 5 times, improved the efficient of coming unstuck, improved 10-30% than existing method, reduced production costs, cost has reduced 30-50% than existing method, but the high long-time continuous operation of the present invention's stability, the present invention can carry out the large-scale industry operation.
The above only is embodiments of the invention; be not so limit claim of the present invention; every equivalent structure or equivalent flow process conversion that utilizes description of the present invention to do; or directly or indirectly be used in other relevant technical fields, all in like manner be included in the scope of patent protection of the present invention.
Claims (3)
1. a refining oil-tea camellia seed crude oil method useful to three high crowds is characterized in that, may further comprise the steps:
A, phospholipase A1 is joined the pH value is among 7 the HAc-NaAc or citric acid solution, obtains enzyme liquid, and the concentration of the phospholipase A1 of described enzyme liquid is 1mg/ml; To be that the ratio of 6-9:1 is mixed with the volume ratio through pretreated macroporous resin and enzyme liquid, obtain mixed solution; The container that takes up mixed solution is placed on the shaking table with 150-180 rev/min tachyphylaxis 2-4 hour, add concentration then and be glutaraldehyde cross-linking 1-6 hour of 0.03-0.24%, crosslinking temperature control is at 3-15 ℃, filter cake is collected in vacuum filtration, gained is immobilized phospholipase A1, to put into refrigerator, standing and drying in 0-5 ℃ after the filter cake dispersion;
B, get oil-tea camellia seed crude oil and remove hydrated phospholipid in the oil-tea camellia seed crude oil through the hydration degum method, adding mass concentration in the treated oil-tea camellia seed crude oil then is the citric acid solution of 40-50%, the quality of described citric acid solution is the 0.1-2% of oil-tea camellia seed crude oil, and stirs 10-30 minute with 1000-1500 rev/min speed; Adding mass concentration again in the treated oil-tea camellia seed crude oil and be 3% NaOH solution, to make the pH value of oil-tea camellia seed crude oil be 7;
0.25% the immobilized enzyme that adds the oil-tea camellia seed crude oil quality in c, the oil-tea camellia seed crude oil that under 56 ℃ of conditions, obtains in the described step b;
D, the oil-tea camellia seed crude oil that the adds immobilized phospholipase A1 speed with 50-120 rev/min was stirred 3-8 hour, again with the centrifugal 3-5 of 8000-10000 rev/min speed minute, remove the impurity in the heavy phase, namely obtain the refining oil-tea camellia seed crude oil.
2. the refining oil-tea camellia seed crude oil method useful to three high crowds according to claim 1 is characterized in that the step of pre-treatment macroporous resin is for to be soaked in the dehydrated alcohol macroporous resin standby among the described step b.
3. the refining oil-tea camellia seed crude oil method useful to three high crowds according to claim 1, it is characterized in that, in the described steps d oil-tea camellia seed crude oil that the adds immobilized enzyme speed with 100-120 rev/min was stirred 3-8 hour, and with 9000 rev/mins speed centrifugal 4 minutes.
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| CN106459828A (en) * | 2014-06-05 | 2017-02-22 | Gea韦斯伐里亚分离机集团有限公司 | Method and device for processing an organic oil in steps |
| CN104651040A (en) * | 2015-01-30 | 2015-05-27 | 国粮武汉科学研究设计院有限公司 | Method for degumming fragrant rap oil through enzymic process |
| CN105296145B (en) * | 2015-10-13 | 2019-04-09 | 中国林业科学研究院亚热带林业研究所 | A kind of processing method of tea oil base oil for cosmetic |
| CN111635830B (en) * | 2020-06-04 | 2023-03-24 | 合肥工业大学 | Method for preparing tea polyphenol esterified tea seed oil by mesoporous material immobilized enzyme |
| CN112430501A (en) * | 2020-12-18 | 2021-03-02 | 江西省粮油科学技术研究所 | Degumming method of cornus wisoniana raw oil |
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