阅读说明：本技术 一种稻米油中谷维素提取方法 (Method for extracting oryzanol from rice oil ) 是由 姚莎莎 姚行权 李兵 于 2021-08-31 设计创作，主要内容包括：本发明公开了一种稻米油中谷维素提取方法。本发明中,对制得的粗谷维素进行初步冲洗,先以含水热甲醇洗一次清洗结束之后,再以石油醚进行清洗,以除去类脂物和色素,然后以加入20％浓度的HCL溶液和甲醇调节PH为5.0之后,浸泡3小时以洗去碱性结合物；取来蒸馏水,对步骤S12中得到的碱性结合物进行水洗,最后真空干燥就可以得到成品谷维素,从而结束整个制备过程,利用NAOH溶液对稻米油中的谷维素进行了两次提取精炼,从而使得后续的利用甲醇提取谷维素的生产过程更加简便快捷,同时提取生产得到的谷维素的纯度更高,从而也提高了后续的谷维素制品的生产加工精度,为人们带来了更多的便利。(The invention discloses a method for extracting oryzanol from rice oil. In the invention, the prepared crude oryzanol is preliminarily washed, firstly washed by hot aqueous methanol, then washed by petroleum ether to remove lipoid and pigment, and then soaked for 3 hours to wash off alkaline conjugate after the pH is adjusted to 5.0 by adding 20% HCL solution and methanol; and (2) taking distilled water, washing the alkaline combination obtained in the step (S12), and finally carrying out vacuum drying to obtain the finished product of oryzanol, so that the whole preparation process is finished, and extracting and refining the oryzanol in the rice oil twice by using the NAOH solution, so that the subsequent production process of extracting the oryzanol by using methanol is simpler, more convenient and faster, and the purity of the oryzanol obtained by extraction and production is higher, thereby improving the production and processing precision of the subsequent oryzanol product and bringing more convenience to people.)

1. A method for extracting oryzanol from rice oil is characterized by comprising the following steps: the method comprises the following steps:

s1, taking the rice oil, using a 800-mesh filter sieve to carry out primary filtering treatment on the rice oil, and storing the filtered rice oil for subsequent use;

s2, fully mixing the filtered rice oil and n-hexane according to 20-30L of rice oil and 40-60L of n-hexane, and then adding 10-15L of NAOH solution;

s3, adding the NAOH solution, and fully stirring to obtain a rice oil mixed solution;

s4, adding the rice oil mixed solution into a centrifuge, beginning to centrifuge the rice oil mixed solution, taking out soapstock in the centrifugate after the centrifugation process is finished, and discarding the soapstock; obtaining primary rice oil;

s5, adding 3-5L of NAOH solution into the primary rice oil obtained in the step S4, fully stirring and mixing, and then starting a reflux reaction;

s6, after the reaction of the step S5 is finished, keeping the temperature of the solution at 40 ℃ for 2 hours, taking a centrifuge and the rice oil mixed solution which is kept warm, adding the rice oil mixed solution into the centrifuge, and beginning to centrifuge the rice oil mixed solution;

s7, after the centrifugation process is finished, taking out soapstock in the centrifugate, and storing the saponin for the subsequent extraction of the oryzanol;

s8, taking 8-10L of methanol from the soapstock obtained in the step S7, dissolving the soapstock obtained in the step S7 in the methanol, filtering and removing unsaponifiable matters;

s9, heating the solution prepared in the step S8 to 40 ℃, adding a citric acid solution with the concentration of 80%, adjusting the pH value to 5, stopping adding the citric acid solution, and performing acid precipitation on the oryzanol;

s10, adjusting the temperature to 10 ℃, cooling and crystallizing the solution prepared in the step S9, and then performing suction filtration in a vacuum environment with constant temperature of 10 ℃ to obtain coarse cereal;

s11, taking hot water, carrying out primary washing on the crude oryzanol prepared in the step S10, and firstly washing once with hot methanol containing water;

s12, after the washing in the step S11 is finished, washing with petroleum ether to remove lipid and pigment, then adding 20% HCL solution and methanol to adjust the pH to 5.0, and soaking for 3 hours to wash off alkaline conjugate;

s13, washing the alkaline combination obtained in the step S12 with water, and finally drying in vacuum to obtain the finished product of oryzanol.

2. The method for extracting oryzanol from rice oil as claimed in claim 1, wherein the method comprises the following steps: in the step S2, the concentration of the added NAOH solution is 45%, and the solution is continuously stirred by a stirring rod during the adding process.

3. The method for extracting oryzanol from rice oil as claimed in claim 1, wherein the method comprises the following steps: in the step S3, the stirring time is 45min after adding the NAOH solution, and the stirring temperature is controlled at 35 ℃ during the stirring process.

4. The method for extracting oryzanol from rice oil as claimed in claim 1, wherein the method comprises the following steps: in step S4, the speed of centrifugation is controlled to 1000Xg, and the time of centrifugation is controlled to 35 min.

5. The method for extracting oryzanol from rice oil as claimed in claim 1, wherein the method comprises the following steps: in the step S5, the reaction temperature of the reflux reaction is controlled at 40 ℃, and the reaction time of the reflux reaction is controlled at 30 min.

6. The method for extracting oryzanol from rice oil as claimed in claim 1, wherein the method comprises the following steps: in the step S9, the time of acid precipitation is 35-45 min.

7. The method for extracting oryzanol from rice oil as claimed in claim 1, wherein the method comprises the following steps: in step S11, the time for performing the preliminary rinsing on the oryzanol is controlled to be 38min, and the time for rinsing is 35 min.

8. The method for extracting oryzanol from rice oil as claimed in claim 1, wherein the method comprises the following steps: in step S12, after adjusting the PH to 5.0, the solution needs to be soaked for 3 hours, and then the alkaline conjugate is washed away.

Technical Field

The invention belongs to the technical field of oryzanol production, and particularly relates to a method for extracting oryzanol from rice oil.

Background

Oryzanol is present in rice oil (rice bran oil) and is a mixture of ferulic acid esters mainly comprising triterpene (alkene) alcohol. Mainly acts on autonomic nervous system and endocrine center of diencephalon, and can regulate autonomic nervous function, reduce endocrine balance disorder, and improve mental disorder symptoms. Meanwhile, the health-care food also has various physiological functions of reducing blood fat, reducing liver lipid, preventing lipid oxidation, resisting oxidation and the like. In addition, it has effect in resisting arrhythmia, and can reduce myocardial excitability by regulating autonomic nerve function. Oryzanol (used for autonomic nerve dysfunction, premenstrual tension, climacteric syndrome, primary dysmenorrhea, periodic psychosis, vascular headache, and head trauma syndrome).

However, the precision of oryzanol obtained by a common oryzanol extraction method is not high enough, so that the purity of a product prepared by subsequently utilizing the oryzanol is low.

Disclosure of Invention

The invention aims to: in order to solve the problems, a method for extracting oryzanol from rice oil is provided.

The technical scheme adopted by the invention is as follows: a method for extracting oryzanol from rice oil comprises the following steps:

s1, taking the rice oil, using a 800-mesh filter sieve to carry out primary filtering treatment on the rice oil, and storing the filtered rice oil for subsequent use;

s2, fully mixing the filtered rice oil and n-hexane according to 20-30L of rice oil and 40-60L of n-hexane, and then adding 10-15L of NAOH solution;

s3, adding the NAOH solution, and fully stirring to obtain a rice oil mixed solution;

s4, adding the rice oil mixed solution into a centrifuge, beginning to centrifuge the rice oil mixed solution, taking out soapstock in the centrifugate after the centrifugation process is finished, and discarding the soapstock; obtaining primary rice oil;

s5, adding 3-5L of NAOH solution into the primary rice oil obtained in the step S4, fully stirring and mixing, and then starting a reflux reaction;

s6, after the reaction of the step S5 is finished, keeping the temperature of the solution at 40 ℃ for 2 hours, taking a centrifuge and the rice oil mixed solution which is kept warm, adding the rice oil mixed solution into the centrifuge, and beginning to centrifuge the rice oil mixed solution;

s7, after the centrifugation process is finished, taking out soapstock in the centrifugate, and storing the saponin for the subsequent extraction of the oryzanol;

s8, taking 8-10L of methanol from the soapstock obtained in the step S7, dissolving the soapstock obtained in the step S7 in the methanol, filtering and removing unsaponifiable matters;

s9, heating the solution prepared in the step S8 to 40 ℃, adding a citric acid solution with the concentration of 80%, adjusting the pH value to 5, stopping adding the citric acid solution, and performing acid precipitation on the oryzanol;

s10, adjusting the temperature to 10 ℃, cooling and crystallizing the solution prepared in the step S9, and then performing suction filtration in a vacuum environment with constant temperature of 10 ℃ to obtain coarse cereal;

s11, taking hot water, carrying out primary washing on the crude oryzanol prepared in the step S10, and firstly washing once with hot methanol containing water;

s12, after the washing in the step S11 is finished, washing with petroleum ether to remove lipid and pigment, then adding 20% HCL solution and methanol to adjust the pH to 5.0, and soaking for 3 hours to wash off alkaline conjugate;

s13, washing the alkaline combination obtained in the step S12 with water, and finally drying in vacuum to obtain the finished product of oryzanol.

In a preferred embodiment, in step S2, the concentration of the NAOH solution added is 45%, and the solution is continuously stirred by a stirring rod during the addition.

In a preferred embodiment, in the step S3, the stirring time is 45min after adding the NAOH solution, and the stirring temperature is controlled at 35 ℃ during the stirring process.

In a preferred embodiment, in step S4, the centrifugation speed is controlled to be 1000xg, and the centrifugation time is controlled to be 35 min.

In a preferred embodiment, in step S5, the reaction temperature of the reflux reaction is controlled at 40 ℃, and the reaction time of the reflux reaction is controlled at 30 min.

In a preferred embodiment, the time for the acid precipitation in step S9 is 35 to 45 min.

In a preferred embodiment, in step S11, the time for performing the preliminary rinsing on the oryzanol is controlled to be 38min, and the time for rinsing is 35 min.

In a preferred embodiment, in step S12, after adjusting the PH to 5.0, the solution is soaked for 3 hours, and then the alkaline conjugate is washed away.

In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:

in the invention, the oryzanol in the rice oil is extracted and refined twice by using the NAOH solution, so that the subsequent production process of extracting the oryzanol by using methanol is simpler, more convenient and faster, and the purity of the oryzanol obtained by extraction and production is higher, thereby improving the subsequent production and processing precision of oryzanol products and bringing more convenience to people.

Detailed Description

In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

The first embodiment is as follows:

a method for extracting oryzanol from rice oil comprises the following steps:

s1, taking the rice oil, using a 800-mesh filter sieve to carry out primary filtering treatment on the rice oil, and storing the filtered rice oil for subsequent use;

s2, fully mixing the filtered rice oil and n-hexane according to 20L rice oil and 40L n-hexane, then adding 10L of NAOH solution, wherein in the step S2, the concentration of the added NAOH solution is 45%, and stirring the solution by using a stirring rod continuously in the adding process;

s3, adding the NAOH solution, fully stirring, in step S3, adding the NAOH solution, stirring for 45min, and controlling the stirring temperature to be 35 ℃ in the stirring process;

s4, in step S3, after the reaction is finished, taking the mixed solution of the centrifuge and the rice oil prepared in the step S3, adding the mixed solution of the rice oil into the centrifuge, starting the centrifugal operation of the mixed solution of the rice oil, and after the centrifugal process is finished, taking out soapstock in the centrifugal liquid and abandoning the soapstock; obtaining primary rice oil; in step S4, the speed of centrifugation is controlled to be 1000xg, and the time of centrifugation is controlled to be 35 min;

s5, taking the primary rice oil obtained in the step S4, adding 3-5L of NAOH solution into the primary rice oil, fully stirring and mixing the mixture, and then starting a reflux reaction; in step S5, the reaction temperature of the reflux reaction is controlled at 40 ℃, and the reaction time of the reflux reaction is controlled at 30 min;

s6, after the reaction of the step S5 is finished, keeping the temperature of the solution at 40 ℃ for 2 hours, taking a centrifuge and the rice oil mixed solution which is kept warm, adding the rice oil mixed solution into the centrifuge, and beginning to centrifuge the rice oil mixed solution;

s7, after the centrifugation process is finished, taking out soapstock in the centrifugate, and storing the saponin for the subsequent extraction of the oryzanol;

s8, taking 8-10L of methanol from the soapstock obtained in the step S7, dissolving the soapstock obtained in the step S7 in the methanol, filtering and removing unsaponifiable matters;

s9, heating the solution prepared in the step S8 to 40 ℃, adding a citric acid solution with the concentration of 80%, adjusting the pH value to 5, stopping adding the citric acid solution, and performing acid precipitation on the oryzanol; in step S9, the time of acid precipitation is 35-45 min;

s10, adjusting the temperature to 10 ℃, starting the solution prepared in the step S9, cooling and crystallizing, and performing suction filtration in a vacuum environment at constant temperature of 10 ℃ to obtain the crude oryzanol; s11, taking hot water, carrying out primary washing on the crude oryzanol prepared in the step S10, and firstly washing once with hot methanol containing water; in step S11, the time for performing the preliminary washing on the coarse oryzanol is controlled to be 38min, and the washing time is 35 min;

s12, after the washing in the step S11 is finished, washing with petroleum ether to remove lipid and pigment, then adding 20% HCL solution and methanol to adjust the pH to 5.0, and soaking for 3 hours to wash off alkaline conjugate; in step S12, after adjusting the PH to 5.0, the solution needs to be soaked for 3 hours, and then the alkaline conjugate is washed away;

and S13, taking distilled water, washing the alkaline combination obtained in the step S12 with water, and finally drying in vacuum to obtain oryzanol refined powder.

Example two:

a method for extracting oryzanol from rice oil comprises the following steps:

s1, taking the rice oil, using a 800-mesh filter sieve to carry out primary filtering treatment on the rice oil, and storing the filtered rice oil for subsequent use;

s2, mixing the filtered rice oil and n-hexane fully according to the ratio of 30L rice oil to 60L n-hexane, then adding 15L of NAOH solution, wherein in the step S2, the concentration of the added NAOH solution is 45%, and stirring the solution by a stirring rod continuously in the adding process;

s3, adding the NAOH solution, fully stirring, in step S3, adding the NAOH solution, stirring for 45min, and controlling the stirring temperature to be 35 ℃ in the stirring process;

s4, in step S3, after the reaction is finished, taking the mixed solution of the centrifuge and the rice oil prepared in the step S3, adding the mixed solution of the rice oil into the centrifuge, starting the centrifugal operation of the mixed solution of the rice oil, and after the centrifugal process is finished, taking out soapstock in the centrifugal liquid and abandoning the soapstock; obtaining primary rice oil; in step S4, the speed of centrifugation is controlled to be 1000xg, and the time of centrifugation is controlled to be 35 min;

s5, taking the primary rice oil obtained in the step S4, adding 3-5L of NAOH solution into the primary rice oil, fully stirring and mixing the mixture, and then starting a reflux reaction; in step S5, the reaction temperature of the reflux reaction is controlled at 40 ℃, and the reaction time of the reflux reaction is controlled at 30 min;

s6, after the reaction of the step S5 is finished, keeping the temperature of the solution at 40 ℃ for 2 hours, taking a centrifuge and the rice oil mixed solution which is kept warm, adding the rice oil mixed solution into the centrifuge, and beginning to centrifuge the rice oil mixed solution;

s7, after the centrifugation process is finished, taking out soapstock in the centrifugate, and storing the saponin for the subsequent extraction of the oryzanol;

s8, taking 8-10L of methanol from the soapstock obtained in the step S7, dissolving the soapstock obtained in the step S7 in the methanol, filtering and removing unsaponifiable matters;

s9, heating the solution prepared in the step S8 to 40 ℃, adding a citric acid solution with the concentration of 80%, adjusting the pH value to 5, stopping adding the citric acid solution, and performing acid precipitation on the oryzanol; in step S9, the time of acid precipitation is 35-45 min;

s10, adjusting the temperature to 10 ℃, starting the solution prepared in the step S9, cooling and crystallizing, and performing suction filtration in a vacuum environment at constant temperature of 10 ℃ to obtain the crude oryzanol; s11, taking hot water, carrying out primary washing on the crude oryzanol prepared in the step S10, and firstly washing once with hot methanol containing water; in step S11, the time for performing the preliminary washing on the coarse oryzanol is controlled to be 38min, and the washing time is 35 min;

s12, after the washing in the step S11 is finished, washing with petroleum ether to remove lipid and pigment, then adding 20% HCL solution and methanol to adjust the pH to 5.0, and soaking for 3 hours to wash off alkaline conjugate; in step S12, after adjusting the PH to 5.0, the solution needs to be soaked for 3 hours, and then the alkaline conjugate is washed away;

and S13, taking distilled water, washing the alkaline combination obtained in the step S12 with water, and finally drying in vacuum to obtain oryzanol refined powder.

It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.

The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.