CN109400664B - Method for extracting rice oil phytosterol - Google Patents
Method for extracting rice oil phytosterol Download PDFInfo
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- CN109400664B CN109400664B CN201811544562.7A CN201811544562A CN109400664B CN 109400664 B CN109400664 B CN 109400664B CN 201811544562 A CN201811544562 A CN 201811544562A CN 109400664 B CN109400664 B CN 109400664B
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- C07J9/00—Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of more than two carbon atoms, e.g. cholane, cholestane, coprostane
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Abstract
The invention discloses a method for extracting rice oil phytosterol, which comprises the steps of putting rice oil and an adsorbent into a ball mill together for ball milling, filtering obtained ball milling liquid, eluting a filter cake by using a solvent to obtain a phytosterol crude product solution, concentrating to obtain the phytosterol crude product, and recrystallizing by using ethanol to obtain the rice oil phytosterolAn alcohol product; the adsorbent is attapulgite, silica gel, active carbon,β-cyclodextrin, hydroxypropyl-β-one or more of cyclodextrin, sepiolite, basic alumina. By the method, the rice oil phytosterol has high extraction efficiency, and the rice oil and the adsorbent are fully mixed and contacted under the action of repeated mechanical stress, so that the phytosterol is easier to separate. The method has the advantages of high extraction rate of the phytosterol, simple process, convenient operation and the like.
Description
Technical Field
The invention belongs to the technical field of deep processing of grease, and relates to a method for extracting rice oil phytosterol.
Background
Rice Oil (Rice Bran Oil) (Rice Bran Oil) is also known as Rice germ Oil, and is also called brown Rice Oil in Japan, and south-east Asia countries and Taiwan regions. Most of the micronutrient ingredients in the rice are lost along with the falling of rice bran in the rice finishing process. The rice oil is prepared from fresh rice bran serving as a raw material through scientific process extraction and processing, and has the following nutrients: 1. the rice oil is rich in oryzanol, the oryzanol is a unique nutritional component of rice oil, and the oryzanol is a strong antioxidant and has the unique effects of regulating vegetative nerves, improving sleep and effectively relieving fatigue. 2. Is rich in natural vitamin E (tocotrienol), and has strong antioxidant effect. 3. The phytosterol is an alcohol compound with cyclopentane perhydrophenanthrene (steroid nucleus) as a skeleton, and has important effects of reducing cholesterol concentration, reducing blood fat, resisting inflammation and cancer, improving immunity and the like.
Phytosterol is a triterpenoid alcohol compound widely present in plants, and particularly has a high content in unsaponifiable matters in vegetable oil and deodorized distillates during refining of the vegetable oil. Zhangsheng et al extracted phytosterol from rice bran by ultrasonic method, and determined phytosterol content to be 4.612 mg/g by performing process optimization through single factor experiment and orthogonal experiment (research on process for extracting phytosterol from rice bran by ultrasonic method, food research and development, 2007). Zhangyunhuan et al screened the best condition for extracting sterol by ultrasonic-assisted organic solvent through single factor and response surface optimization test with the extraction rate of 8.99mg/g (research on optimization of extraction condition of phytosterol in wheat germ, grain and grease, 2018, stage 5). However, these methods have expensive equipment, high preparation cost, excessive chemical reagent residue, are not suitable for eating, and have poor extraction effect. Therefore, the above methods are more or less unable to meet the requirements of industrial production.
Mechanochemistry (also called Mechanochemistry) is a subject of studying the change of physicochemical properties of substances induced by mechanical force. The mechanochemical extraction technology is a novel organic solvent-free extraction technology, and is a green extraction technology which combines the mechanochemical principle with the extraction of natural bioactive components. Compared with the traditional extraction method, the extraction process adopts specific grinding equipment for pretreatment, reduces or eliminates the use of organic solvents, and has the advantages of high product extraction rate and purity, short extraction time, simple process flow, low cost and the like. The technology is an efficient, green and environment-friendly extraction technology, and is expected to replace the traditional extraction method. At present, no report of adopting the technology to assist in extracting the rice oil phytosterol is found.
Disclosure of Invention
The invention aims to overcome the problems in the existing rice oil phytosterol extraction process and provides a novel method for extracting the rice oil mechanochemical phytosterol, which has simple process and is environment-friendly.
The research idea of the invention is as follows: under the action of mechanical force, the rice oil and the adsorbent are co-ground, so that the rice oil and the adsorbent are fully mixed under the action of repeated mechanical stress, and the phytosterol is quickly and efficiently extracted and separated at normal temperature.
The technical scheme adopted by the invention is as follows:
a method for extracting rice oil phytosterol is characterized in that rice oil and an adsorbent are put into a ball mill together for ball milling, the obtained ball milling liquid is filtered, a filter cake is eluted by a solvent to obtain a phytosterol crude product solution, the phytosterol crude product is obtained by concentration, and then the rice oil phytosterol product is obtained by ethanol recrystallization; the adsorbent is attapulgite, silica gel, active carbon,β-cyclodextrin, hydroxypropyl-β-one or more of cyclodextrin, sepiolite, basic alumina.
The extraction method of the rice oil phytosterol is characterized in that the ratio of the mass of the adsorbent to the volume of the rice oil is 1-15: 100, the unit of the mass is g, and the unit of the volume is mL.
The extraction method of the rice oil phytosterol is characterized in that the ball mill is a high-energy planetary ball mill or a high-energy oscillating ball mill.
The extraction method of the rice oil phytosterol is characterized in that the ball mill is a high-energy planetary ball mill, and the ball milling speed of the ball mill is 100-500 rpm.
The extraction method of the rice oil phytosterol is characterized in that the ball milling time is 0.5-14 hours; the mass sum of the rice oil and the adsorbent is recorded as the mass of the feed liquid, and the mass ratio of the feed liquid to the ball milling medium adopted by the ball mill is 1: 3-15.
The extraction method of the rice oil phytosterol is characterized in that the ball mill is a high-energy oscillating ball mill, and the ball milling frequency of the ball mill is 10-30 Hz.
The extraction method of the rice oil phytosterol is characterized in that the ball milling time is 0.5-5 hours; the mass sum of the rice oil and the adsorbent is recorded as the mass of the feed liquid, and the mass ratio of the feed liquid to the ball milling medium adopted by the ball mill is 1: 5-20.
The extraction method of the rice oil phytosterol is characterized in that ball milling media adopted by a ball mill are one or two of stainless steel ball milling beads, alumina ball milling beads and zirconia ball milling beads, and the diameter of the ball milling media is 5-40 mm.
The extraction method of the rice oil phytosterol is characterized in that the adsorbent is one or two of β -cyclodextrin, silica gel and attapulgite.
The extraction method of the rice oil phytosterol is characterized in that the solvent is n-hexane, ethyl acetate or isopropanol.
Putting the mass of the adsorbent and the volume of the rice oil into a high-energy planetary ball mill according to a ratio of 3%, adding a proper amount of stainless steel balls for milling, performing ball milling at a rotating speed of 500 rpm for 0.5-12 h by 100-; eluting the filter cake with n-hexane to obtain crude phytosterol, concentrating, and recrystallizing the crude phytosterol with ethanol to obtain rice oil phytosterol. Or putting the mass of the adsorbent and the volume of the rice oil into a vibration ball mill according to the proportion of 5%, adding a proper amount of stainless steel balls for milling, carrying out ball milling at the frequency of 10-30Hz for 0.5-5 h, taking out the ball milling liquid, filtering, eluting a filter cake by using n-hexane to obtain a phytosterol crude product, concentrating, and recrystallizing the phytosterol crude product by using ethanol to obtain the rice oil phytosterol.
Compared with the prior art, the invention has the beneficial effects that:
(1) the extraction efficiency is high, and the rice oil and the adsorbent are fully mixed and contacted under the action of repeated mechanical stress, so that the phytosterol is easier to separate;
(2) the extraction process does not need heating, so that the energy consumption is reduced;
(3) the process is simple, the process flow is simplified, and the production cost is reduced;
(4) compared with the traditional process, the product has better color and luster;
(5) the method has the advantages of simple process operation, high efficiency, normal temperature operation, low energy consumption and easy large-scale industrial production.
In conclusion, the method has the advantages of simple process, convenient operation, high product yield, low production cost, environmental protection and the like, and is a rice oil phytosterol extraction method with better popularization and application prospects.
Detailed Description
The present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the invention.
The method for calculating the phytosterol content in rice oil in the product described in the following examples is as follows:
quantitative analysis of phytosterols: to be provided withβ-The sitosterol standard substance is used as a reference substance, and the phytosterol content is determined by adopting an ultraviolet spectrophotometry method.
Example 1
Putting 60 mL of rice oil, 3 g of attapulgite and 420 g of steel balls with the diameter of 15 mm into a 300 mL ball milling tank of a high-energy planetary ball mill, carrying out ball milling for 0.5 h at the rotating speed of 300 rpm, taking ball milling liquid, filtering, eluting a filter cake by using n-hexane to obtain a phytosterol crude product solution, concentrating to obtain the phytosterol crude product, and recrystallizing by using ethanol to obtain the rice oil phytosterol with the purity of 89%, wherein the phytosterol crude product is 0.72 g.
Example 2
10 mL of rice oil, 0.5 g of alkaline alumina and two steel balls with the diameter of 15 mm are put into a 50 mL ball milling tank of a high-energy oscillating ball mill, ball milling is carried out for 2 h at the frequency of 20 Hz, ball milling liquid is taken out, filtering is carried out, a filter cake is eluted by normal hexane to obtain a phytosterol crude product solution, concentration is carried out to obtain the phytosterol crude product, and then ethanol recrystallization is carried out to obtain the rice oil phytosterol 0.11 g, wherein the purity is 87%.
Example 3
Mixing 60 mL rice oil, 3 gβAnd (3) putting the cyclodextrin and 420 g of alumina ball milling beads with the diameter of 15 mm into a 300 mL ball milling tank of a high-energy planetary ball mill, carrying out ball milling at the rotating speed of 400 rpm for 2 h, taking ball milling liquid, filtering, eluting a filter cake by using n-hexane to obtain a phytosterol crude product solution, concentrating to obtain the phytosterol crude product, and recrystallizing by using ethanol to obtain 0.74 g of rice oil phytosterol with the purity of 91%.
Example 4
Putting 10 mL of rice oil, 0.4 g of sepiolite, 0.2g of silica gel and two zirconia beads with the diameter of 15 mm into a 50 mL ball milling tank of a high-energy oscillating ball mill, carrying out ball milling for 1 h at the frequency of 25 Hz, taking ball milling liquid, filtering, eluting a filter cake with isopropanol to obtain a phytosterol crude product solution, concentrating to obtain the phytosterol crude product, and recrystallizing with ethanol to obtain 0.10 g of rice oil phytosterol with the purity of 93%.
Example 5
Putting 60 mL of rice oil, 3 g of silica gel and 480 g of alumina ball milling beads with the diameter of 10 mm into a 300 mL ball milling tank of a high-energy planetary ball mill, carrying out ball milling for 1.5 h at the rotating speed of 300 rpm, taking ball milling liquid, filtering, eluting a filter cake by using n-hexane to obtain a phytosterol crude product solution, concentrating to obtain the phytosterol crude product, and recrystallizing by using ethanol to obtain 0.80 g of rice oil phytosterol with the purity of 88%.
Example 6
60 mL of rice oil and 3 g of hydroxypropyl-βAnd (3) putting cyclodextrin and 480 g of steel balls with the diameter of 20 mm into a 300 mL ball milling tank of a high-energy planetary ball mill, carrying out ball milling for 2 h at the rotating speed of 300 rpm, taking ball milling liquid, filtering, eluting a filter cake by using ethyl acetate to obtain a phytosterol crude product solution, concentrating to obtain the phytosterol crude product, and recrystallizing by using ethanol to obtain 0.78 g of rice oil phytosterol with the purity of 94%.
Example 7
Mixing 10 mL rice oil, 0.2gβAnd (3) putting cyclodextrin and 0.1 g of attapulgite, putting two alumina ball milling beads with the diameter of 12 mm into a 50 mL ball milling tank of a high-energy oscillating ball mill, carrying out ball milling for 1.5 h at the frequency of 30Hz, taking ball milling liquid, filtering, eluting a filter cake by using normal hexane to obtain a phytosterol crude product solution, concentrating to obtain the phytosterol crude product, and recrystallizing by using ethanol to obtain 0.14 g of rice oil phytosterol with the purity of 95%.
The statements in this specification merely set forth a list of implementations of the inventive concept and the scope of the present invention should not be construed as limited to the particular forms set forth in the examples.
Claims (8)
1. A method for extracting rice oil phytosterol is characterized in that rice oil and an adsorbent are put into a ball mill together for ball milling, the obtained ball milling liquid is filtered, a filter cake is eluted by a solvent to obtain a phytosterol crude product solution, the phytosterol crude product is obtained by concentration, and then the rice oil phytosterol product is obtained by ethanol recrystallization, wherein the adsorbent is one or more of attapulgite, silica gel, activated carbon, β -cyclodextrin, hydroxypropyl- β -cyclodextrin, sepiolite and basic alumina;
the ball milling medium adopted by the ball mill is one or two of stainless steel ball milling beads, alumina ball milling beads and zirconia ball milling beads, and the diameter of the ball milling medium is between 5 and 40 mm;
the solvent is n-hexane, ethyl acetate or isopropanol.
2. The method for extracting rice oil phytosterol as claimed in claim 1, wherein the ratio of the mass of said adsorbent to the volume of said rice oil is 1-15: 100, the unit of mass is g, and the unit of volume is mL.
3. The method for extracting rice oil phytosterol according to claim 1, wherein the ball mill is a high-energy planetary ball mill or a high-energy oscillating ball mill.
4. The method for extracting rice oil phytosterol as claimed in claim 3, wherein the ball mill is a high-energy planetary ball mill, and the rotation speed of the ball mill is 100-500 rpm.
5. The method for extracting rice oil phytosterol as claimed in claim 4, wherein the time for ball milling is 0.5-14 h; the mass sum of the rice oil and the adsorbent is recorded as the mass of the feed liquid, and the mass ratio of the feed liquid to the ball milling medium adopted by the ball mill is 1: 3-15.
6. The method for extracting rice oil phytosterol according to claim 3, wherein the ball mill is a high-energy oscillating ball mill, and the ball milling frequency of the ball mill is 10-30 Hz.
7. The method for extracting rice oil phytosterol as claimed in claim 6, wherein the time for ball milling is 0.5-5 h; the mass sum of the rice oil and the adsorbent is recorded as the mass of the feed liquid, and the mass ratio of the feed liquid to the ball milling medium adopted by the ball mill is 1: 5-20.
8. The method for extracting rice oil phytosterol according to claim 1, wherein the adsorbent is one or two of β -cyclodextrin, silica gel and attapulgite.
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| CN110615824B (en) * | 2019-08-07 | 2020-12-22 | 厦门大学 | Method for separating triterpene alcohol and sterol from crude sterol of rice bran |
| CN111187329A (en) * | 2020-03-04 | 2020-05-22 | 南京诺齐生物科技有限公司 | Preparation technology of high-absorptivity phytosterol |
| WO2022151575A1 (en) * | 2021-01-18 | 2022-07-21 | 芦书峰 | Flower classifying and processing process and flower product |
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| CN101225082B (en) * | 2008-01-31 | 2010-12-01 | 浙江工业大学 | Method for extracting tea-polyphenol and separating monomer EGCG from tea |
| CN101508709B (en) * | 2009-03-23 | 2011-02-02 | 浙江工业大学 | Method for auxiliary extraction of aloin with mechanical force |
| CN101942007B (en) * | 2010-08-23 | 2012-07-25 | 领先生物农业股份有限公司 | Method for extracting phytosterol from waste residues generated in biodiesel production and product thereof |
| CN102344692B (en) * | 2011-08-10 | 2013-11-13 | 浙江工业大学 | Method for extracting gardenia yellow pigment from gardeniae longicarpae fruit |
| CN102898491A (en) * | 2012-09-20 | 2013-01-30 | 浙江银河药业有限公司 | Preparation technology for extracting phytosterols from rice bran crude oil |
| CN106167738B (en) * | 2016-09-21 | 2019-07-19 | 山东健源油脂科技有限公司 | The rice essential smelting method of high phytosterol |
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