CN113684092A - Preparation method of nitraria seed oil for increasing vitamin E content - Google Patents
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
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- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/104—Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
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Abstract
The invention discloses a preparation method of nitraria seed oil for improving vitamin E content. Respectively obtaining the nitraria seed oil with high acid value and the nitraria seed oil with low acid value by adopting supercritical carbon dioxide fractional extraction. The high acid value oil is processed by refining processes such as degumming, deacidification, decoloration, deodorization and the like to obtain light yellow transparent nitrariatangutorum seed oil, and the low acid value oil is processed by centrifugation and membrane filtration to obtain yellow transparent nitrariatangutorum seed oil. Research shows that the fatty acid compositions of the high-acid-value oil and the low-acid-value oil are basically consistent, but V in the low-acid-value nitraria seed oilEThe content of the nitraria seed oil is far higher than that of the refined nitraria seed oil with high acid value, the process can effectively retain active ingredients in the nitraria seed oil, and the quality of the nitraria seed oil is improved.
Description
Technical Field
The invention relates to the technical field of nitraria seed oil production, in particular to a preparation method of nitraria seed oil for improving vitamin E content.
Background
The white thorn (Nitraria) is a multi-branch, salt and alkali resistant, droughty type low shrub of Zygophyllaceae, and has the physiological characteristics of drought resistance, high temperature resistance, strong water retention capacity and the like. The nitraria tangutorum bobr has rich resources and wide distribution, and is wild in the northwest desert, the north China and the northeast coastal areas, Zhangjiakou dam, Tianjin, Cangzhou and the like. According to statistics, the nitraria tangutorum bobr basins are distributed in pollution-free areas with the altitude of more than 3000 m, 6-10 ten thousand tons of nitraria tangutorum bobr can be produced every year, and the method has great development value.
The nitraria tangutorum bobr fruits have higher economic and medicinal values and are well researched, developed and applied. In the process of utilizing the nitraria tangutorum bobr, a large amount of nitraria tangutorum bobr seeds are produced. The nitraria seed oil is reported to have high content of unsaturated fatty acid, wherein the content of linoleic acid is up to 65.85% (Soxhlet, Gaohang, Wanwang Cynanchum. Tanggute white stings in China: research and development of chemical components of seed oil by carbon dioxide supercritical extraction (English) [ J ]. research and development of natural products, 2004(01):16-18.), and is a functional oil rich in unsaturated fatty acid which is few in nature. In addition, researches show that the nitraria seed oil is rich in tocopherol and sterol compounds and is potential functional vegetable oil.
Some methods for extracting Nitraria tangutorum bobr seed oil have been disclosed, for example, in the text of the research (English) on the supercritical carbon dioxide extraction of chemical components of Nitraria tangutorum bobr, China, Vol.16, No. 1 of 2004, Natural products research and development, supercritical CO is used2The fluid technology is carried out at the pressure of 22.0MPa, the temperature of 42 ℃ and CO2The tangut nitraria tangutorum bobr seeds are extracted for 8 hours under the condition of the flow rate of 46L/h, and the oil yield is 11.6 percent; the same supercritical CO is used in the national patent CN2005100418792The fluid technology is carried out at the pressure of 15-45 MPa, the temperature of 25-50 ℃ and CO2Extracting the Nitraria tangutorum bobr seeds for 6 hours under the condition of the flow rate of 45-250L/h, wherein the oil yield is 10.13%; in "CN 201110374709", a method for extracting nitraria seed oil by using subcritical fluid is described, and the yield of oil is about 12%. And "supercritical CO" in "food research and development" 2015 3, 36 th volume, 6 th2The best technology for extracting Siberian Nitraria seed oil is disclosed as the research article, wherein the optimal technology is that the extraction pressure is 40MPa, the extraction temperature is 55 ℃, and CO is adopted2The flow rate is 10L/min, and the yield under the condition is 4.63 percent.
The supercritical carbon dioxide extraction technology has the advantages of no residue, low extraction temperature, high retention rate of active substances and the like, and is selected as the extraction technology of the nitraria seed oil in most researches. However, long-term research shows that the nitraria seed oil obtained by the conventional supercritical carbon dioxide extraction method has the defects of high acid value and dark color, and can be further applied only by refining. However, the oil refining process requires chemical reagents and high-temperature treatment, which is quite serious in damage to active ingredients, and is contrary to the initial heart of selecting the supercritical carbon dioxide extraction technology. Therefore, a new technology for extracting the nitraria seed oil by using supercritical carbon dioxide needs to be researched, so that the damage of the refining process to the quality of the grease is reduced.
Disclosure of Invention
The invention aims to solve the problem that an innovative scheme is provided aiming at the defects in the prior art, in particular to a scheme for improving the content of vitamin E in the preparation process of nitraria tangutorum bobr seed oil.
In order to solve the problems, the invention adopts the following scheme: a preparation method of nitraria seed oil for improving vitamin E content comprises the following steps:
(1) using supercritical carbon dioxide to extract the nitraria seed by stages to obtain nitraria seed oil with high acid value and nitraria seed oil with low acid value;
(2) degumming: preheating the nitraria seed oil with high acid value to 70-80 ℃, adding phosphoric acid accounting for 0.1-0.3% of the total weight of the oil and boiling water accounting for 2-4% of the total weight of the oil, continuously stirring for more than 60min, and removing a water layer to obtain degummed oil;
(3) deacidifying: cooling the degummed oil to 40-45 ℃, slowly adding the prepared alkali liquor while stirring, and then keeping the temperature and continuously stirring for 40-60 min; after stirring, heating to 65-75 ℃, then preserving heat and stirring for 30-50 min, then stopping heating and stirring, and after standing and layering, separating soapstock from the bottom; heating the oil to 80-90 ℃, adding hot water of 90-100 ℃ accounting for 3-5% of the weight of the oil for washing, slowly stirring for 3-5 min, standing, and discharging water washing liquid from the bottom of the tank after layering; finally transferring the washed oil to vacuum drying equipment, and carrying out vacuum drying at 100-120 ℃ until the oil is clear to obtain deacidified oil;
(4) and (3) decoloring: adding activated clay accounting for 2-5% of the weight of the oil into the dried deacidified oil, stirring for 40-60 min under a vacuum condition, and separating and removing the activated clay to obtain the decolored oil;
(5) deodorizing: heating the decolored oil to 180-220 ℃, and deodorizing for 2-4 h under a vacuum-pumping condition to obtain light yellow clarified nitraria seed oil;
(6) centrifuging the low-acid-value nitraria seed oil, and passing through an ultrafiltration membrane to obtain yellow clear nitraria seed oil.
Further, the nitraria tangutorum bobr seeds are cleaned before supercritical carbon dioxide fractional extraction, dried in the sun and then crushed or crushed by a crusher or a grain crusher, and the moisture content of the nitraria tangutorum bobr seeds is less than 10 percent before crushing.
Further, crushing the nitraria tangutorum bobr seeds, then performing fractional extraction by using supercritical carbon dioxide, firstly, keeping the extraction pressure at 25MPa for 1h to obtain nitraria tangutorum bobr seed oil with high acid value, then, adjusting the extraction pressure to 35MPa, and continuing the extraction for 3h to obtain the nitraria tangutorum bobr seed oil with low acid value.
Further, the alkali liquor used during deacidification of the high-acid-value nitraria tangutorum bobr seed oil is a sodium hydroxide solution or a potassium hydroxide solution, and preferably a potassium hydroxide solution; the water washing process was performed twice.
Further, after the low-acid-value nitraria seed oil is centrifuged at the rotating speed of 5000rpm, yellow clear nitraria seed oil is obtained through an ultrafiltration membrane with the molecular weight cutoff of 5 ten thousand.
Further, when potassium hydroxide is used for deacidification, the separated soapstock and the water washing liquid discharged from the bottom of the tank are uniformly mixed and homogenized to obtain the orange yellow milky plant nutrient solution rich in organic matters and potassium elements.
The invention has the following technical effects: and determining that the crushing by using a grain crusher is the optimal crushing mode by comparing the influence of different crushing modes on the supercritical extraction of the nitraria seed oil.
By researching the influence of various process parameters on the oil yield and the oil acid value of the nitraria tangutorum bobr seeds in the extraction process, the oil with high acid value is obtained by extracting for 1h under 25MPa, then the extraction pressure is increased to 35MPa, and the extraction is continued for 3h to obtain the oil with low acid value. Refining the high-acid-value oil into light yellow transparent refined nitrariatangutorum seed oil through processes of degumming, deacidification, decoloration, deodorization and the like; and centrifuging the low-acid-value oil and filtering by using an ultrafiltration membrane to obtain yellow and transparent nitraria seed oil. The process only needs to refine the high-acid-value nitraria seed oil, greatly reduces the workload, reduces the waste water and waste residues generated in the oil refining process, and perfectly keeps the low-acidV in Nitraria seed oilEAnd active substances are added, so that the quality of the nitraria seed oil is improved.
Drawings
FIG. 1 shows the oil output in each time period under different extraction pressure conditions;
FIG. 2 shows the acid value of Nitraria sibirica seed oil at different extraction pressure conditions for each time period.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
Example 1:
a method for preparing Nitraria seed oil with improved vitamin E content is provided.
1.1 influence of the extent of crushing of Nitraria tangutorum bobr seeds on supercritical carbon dioxide extraction.
Cleaning Nitraria tangutorum bobr seeds, drying in the sun until the water content is less than 10%, crushing with grain crusher (the distance between two rollers is 1mm), and pulverizing with Chinese medicinal pulverizer to 20 mesh and 40 mesh. Respectively taking 7kg of the materials with different crushing degrees, adding the materials into an extraction kettle, introducing supercritical carbon dioxide fluid, and extracting for 4 hours at the extraction pressure of 30MPa and the extraction temperature of 45 ℃, wherein the results are shown in Table 1.
Table 1 influence of different crushing degree of nitraria tangutorum bobr seeds on supercritical carbon dioxide extraction.
As shown in table 1, the crushed nitraria tangutorum bobr seeds are very easy to be caked into hard blocks under the high pressure of supercritical carbon dioxide extraction, the more the crushing is, the more serious the caking phenomenon is, the serious influence is caused on the discharge after the extraction, and the penetrability and the fluidity of the carbon dioxide in the materials are deteriorated due to the caking of the materials, so that the oil yield of the crushed nitraria tangutorum bobr seeds with 40 meshes is lower than the oil yield of 20 meshes. The nitraria tangutorum bobr seeds crushed by the grain crusher have large gaps among materials, cannot be extruded into blocks in the extraction process, and have good carbon dioxide circulation in the materials, so that higher oil yield can be obtained, and the extraction after crushing the nitraria tangutorum bobr seeds is the best treatment method.
1.2 the nitraria seed oil is extracted by supercritical carbon dioxide in a grading way.
Adding crushed nitraria tangutorum bobr seeds into an extraction kettle, introducing supercritical carbon dioxide fluid, extracting for 4 hours at the extraction temperature of 45 ℃ under the extraction pressure of 30MPa, separating the nitraria tangutorum bobr seed oil in each time period from a separation kettle when extracting for 0.5, 1, 1.5, 2, 2.5, 3 and 4 hours, weighing the oil weight, observing the color of the oil in each time period, and measuring the acid value, wherein the results are shown in a table 2.
As shown in Table 2, the amount of oil output, the color and the acid value of the Nitraria sibirica pall seed oil obtained in each stage of extraction are different, and the acid value of the Nitraria sibirica pall seed oil is gradually reduced along with the extraction time. The nitraria tangutorum bobr seed oil obtained 1h before extraction has higher acid value and is high acid value oil, and the nitraria tangutorum bobr seed oil obtained 1h after extraction has the acid value less than 3mgKOH/g, meets the limit standard of edible vegetable oil acid value in GB2716, and is low acid value oil.
Table 2 comparison of nitraria seed oil at various time periods during the extraction.
Then, the effect of extraction pressures of 35, 30 and 25MPa on the amount of white spine seed oil output (see fig. 1) and the effect on acid value (see fig. 2) were compared. As shown in the figure, the oil yield of the nitraria seed oil is increased along with the increase of the extraction pressure, but the acid value is not obviously changed along with the extraction pressure, the nitraria seed oil extracted in the first 1h is still high-acid-value oil, and the nitraria seed oil extracted in the subsequent 1h is low-acid-value oil. In order to improve the proportion of low-acid-value oil in the total oil output as much as possible and ensure the oil yield, high-acid-value oil is obtained by extracting for 1h under 25MPa, then the extraction pressure is increased to 35MPa, and the extraction is continued for 3h to obtain the low-acid-value oil.
1.3 refining the nitraria seed oil with high acid value.
1.3.1 degumming
Preheating the nitraria seed oil with high acid value to 80 ℃, adding phosphoric acid accounting for 0.2 percent of the total weight of the oil and boiling water accounting for 3 percent of the total weight of the oil, continuously stirring for more than 60min, and removing a water layer to obtain the degummed oil.
1.3.2 Deacidification
Cooling the degummed oil to 40 deg.C, slowly adding the prepared potassium hydroxide solution while stirring, and keeping the temperature and stirring for 40 min. Heating to 65 deg.C after stirring, stirring for 30min, stopping heating and stirring, standing for 3 hr, and separating soapstock from bottom. Heating the oil to 85 deg.C, adding 90 deg.C hot water 5 wt% of the oil, washing with water, slowly stirring for 5min, standing for layering for 3 hr, discharging the water washing solution from the bottom of the tank, and washing with water twice. And finally transferring the oil after water washing to vacuum drying equipment, and drying in vacuum at 100 ℃ until the oil is clear to obtain the deacidified oil.
Uniformly mixing and homogenizing the deacidified soapstock and part of the washing waste liquid to obtain orange yellow milky nutrient solution rich in organic matters and potassium elements, and the orange yellow milky nutrient solution can be used for plant fertilizers.
1.3.3 decolorization
Adding activated clay 3.5% of the oil weight into the dried deacidified oil, performing plate-frame filter pressing for 60min under a vacuum condition to remove clay, and thus obtaining the decolored oil.
1.3.4 deodorization
Heating the decolorized nitraria seed oil to 220 ℃, and deodorizing for 4 hours under the condition of vacuumizing and adjusting price to obtain light yellow clarified nitraria seed oil.
1.4 treating the nitraria seed oil with low acid value.
Centrifuging the low acid value oil at the rotating speed of 5000rpm, and passing through an ultrafiltration membrane with the molecular weight cutoff of 5 ten thousand to obtain yellow clarified nitraria seed oil.
1.5 index determination of the nitraria seed oil extracted by supercritical fluid.
The content and the type of the fatty acid of different Nitraria seed oil are measured, the result is shown in Table 3, the Nitraria seed oil with high acid value and Nitraria seed oil with low acid value have almost no difference in the type and the content of the fatty acid, and the content of unsaturated fatty acid, especially linoleic acid and oleic acid is very high, so that the Nitraria seed oil is the highly unsaturated fatty acid vegetable oil which is rarely seen in nature, and has great application potential. Then, V in different Nitraria sibirica seed oils was determinedEThe contents, results are shown in Table 4,it can be seen that V is in the refined p-nitraria seed oilEThe content influence is very large, more than half of VEIs lost in refining process, and a large amount of V is retained in unrefined low-acid-value nitraria seed oilEAnd has stronger activity.
TABLE 3 comparison of fatty acid contents of different Nitraria seed oils
TABLE 4 different Nitraria seed oils VEAnd (4) comparing the contents.
Example 2:
a method for preparing Nitraria seed oil with improved vitamin E content is provided.
1.1 crushing Nitraria seed.
Cleaning Nitraria tangutorum bobr seeds, drying in the sun until the water content is less than 10%, and crushing by using a grain crusher.
1.2 extracting the nitraria seed oil with high acid value by supercritical carbon dioxide.
Adding crushed Nitraria seed 7kg into extraction kettle, introducing supercritical carbon dioxide fluid, extracting at extraction temperature of 45 deg.C under extraction pressure of 25MPa for 1 hr, separating Nitraria seed oil 113.2g with high acid value from separation kettle, and measuring acid value to be 4.5 mgKOH/g.
1.3 extracting the nitraria seed oil with low acid value by supercritical carbon dioxide.
After the high acid value oil is extracted, the extraction pressure is increased to 35MPa, then the extraction is continued for 3 hours, 215.7g of low acid value oil is separated, and the acid value is measured to be 1.6 mgKOH/g.
1.4 refining the nitraria seed oil with high acid value.
1.4.1 degumming
Preheating the nitraria seed oil with high acid value to 80 ℃, adding phosphoric acid accounting for 0.2 percent of the total weight of the oil and boiling water accounting for 3 percent of the total weight of the oil, continuously stirring for more than 60min, and removing a water layer to obtain the degummed oil.
1.4.2 Deacidification
Cooling the degummed oil to 40 deg.C, slowly adding the prepared sodium hydroxide solution while stirring, and keeping the temperature and stirring for 40 min. Heating to 65 deg.C after stirring, stirring for 30min, stopping heating and stirring, standing for 3 hr, and separating soapstock from bottom. Heating the oil to 85 deg.C, adding 90 deg.C hot water 5 wt% of the oil, washing with water, slowly stirring for 5min, standing for layering for 3 hr, discharging the water washing solution from the bottom of the tank, and washing with water twice. And finally transferring the oil after water washing to vacuum drying equipment, and drying in vacuum at 100 ℃ until the oil is clear to obtain the deacidified oil.
1.4.3 decolorization
Adding activated clay 4 wt% of the oil into the dried deacidified oil, performing plate-frame filter pressing for 60min under vacuum condition to remove clay to obtain decolorized oil.
1.4.4 deodorization
Heating decolorized Nitraria seed oil to 220 deg.C, deodorizing for 4 hr under vacuum condition to obtain pale yellow clarified Nitraria seed oil 96.5g, and measuring VEThe content was 22.1mg/100 g.
1.5 treating the nitraria seed oil with low acid value.
Centrifuging low acid value oil at 5000rpm, passing through ultrafiltration membrane with molecular weight cutoff of 5 ten thousand to obtain yellow clarified Nitraria seed oil 214.1g, and measuring VEThe content was 69.4mg/100 g.
Claims (6)
1. A preparation method of nitraria seed oil for improving vitamin E content is characterized by comprising the following steps:
(1) using supercritical carbon dioxide to extract the nitraria seed by stages to obtain nitraria seed oil with high acid value and nitraria seed oil with low acid value;
(2) degumming: preheating the nitraria seed oil with high acid value to 70-80 ℃, adding phosphoric acid accounting for 0.1-0.3% of the total weight of the oil and boiling water accounting for 2-4% of the total weight of the oil, continuously stirring for more than 60min, and removing a water layer to obtain degummed oil;
(3) deacidifying: cooling the degummed oil to 40-45 ℃, slowly adding the prepared alkali liquor while stirring, and then keeping the temperature and continuously stirring for 40-60 min; after stirring, heating to 65-75 ℃, then preserving heat and stirring for 30-50 min, then stopping heating and stirring, and after standing and layering, separating soapstock from the bottom; heating the oil to 80-90 ℃, adding hot water of 90-100 ℃ accounting for 3-5% of the weight of the oil for washing, slowly stirring for 3-5 min, standing, and discharging water washing liquid from the bottom of the tank after layering; finally transferring the washed oil to vacuum drying equipment, and carrying out vacuum drying at 100-120 ℃ until the oil is clear to obtain deacidified oil;
(4) and (3) decoloring: adding activated clay accounting for 2-5% of the weight of the oil into the dried deacidified oil, stirring for 40-60 min under a vacuum condition, and separating and removing the activated clay to obtain the decolored oil;
(5) deodorizing: heating the decolored oil to 180-220 ℃, and deodorizing for 2-4 h under a vacuum-pumping condition to obtain light yellow clarified nitraria seed oil;
(6) centrifuging the low-acid-value nitraria seed oil, and passing through an ultrafiltration membrane to obtain yellow clear nitraria seed oil.
2. The method for preparing nitraria seed oil with improved vitamin E content according to claim 1, wherein nitraria seed is cleaned before supercritical carbon dioxide fractional extraction, dried in the sun and then crushed or shredded by a crusher or a grain crusher, and the moisture content of the nitraria seed is less than 10% before crushing.
3. The method for preparing nitraria seed oil with improved vitamin E content according to claim 1, characterized in that nitraria seed is crushed and then extracted by supercritical carbon dioxide in a grading manner, the extraction pressure is kept at 25MPa for 1h to obtain nitraria seed oil with high acid value, the extraction pressure is adjusted to 35MPa, and the extraction is continued for 3h to obtain nitraria seed oil with low acid value.
4. The method for preparing nitraria seed oil with improved vitamin E content according to claim 1, characterized in that the alkali solution used for deacidifying the nitraria seed oil with high acid value is sodium hydroxide solution or potassium hydroxide solution; the water washing process was performed twice.
5. The method for preparing the nitraria seed oil with the improved vitamin E content according to claim 1, characterized in that the nitraria seed oil with the low acid value is centrifuged at 5000rpm, and then a yellow clear nitraria seed oil is obtained by an ultrafiltration membrane with the molecular weight cutoff of 5 ten thousand.
6. A plant fertilizer based on a preparation process of nitraria seed oil is characterized in that when potassium hydroxide solution is used for deacidification, separated soapstock and water washing liquor discharged from a tank bottom are uniformly mixed and homogenized to obtain orange yellow emulsion nutrient solution.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1687340A (en) * | 2005-03-23 | 2005-10-26 | 中国科学院西北高原生物研究所 | Supercritical Co2 extracting technique for oil of Nitraria seeds and application in lowering blood fat thereof |
| CN103045357A (en) * | 2012-12-24 | 2013-04-17 | 河南大学 | Extraction and refining method for eucommia seed oil |
| CN107858197A (en) * | 2017-11-01 | 2018-03-30 | 广东金妮宝科技发展有限公司 | A kind of production and processing method of low acid value high-quality edible oil tea-seed oil |
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- 2021-09-03 CN CN202111025250.7A patent/CN113684092A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1687340A (en) * | 2005-03-23 | 2005-10-26 | 中国科学院西北高原生物研究所 | Supercritical Co2 extracting technique for oil of Nitraria seeds and application in lowering blood fat thereof |
| CN103045357A (en) * | 2012-12-24 | 2013-04-17 | 河南大学 | Extraction and refining method for eucommia seed oil |
| CN107858197A (en) * | 2017-11-01 | 2018-03-30 | 广东金妮宝科技发展有限公司 | A kind of production and processing method of low acid value high-quality edible oil tea-seed oil |
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| 王兴国等: "《食用油精准适度加工理论与实践》", 中国轻工业出版社, pages: 163 * |
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