CN112457154A - R-linolenic acid extraction and pinolenic acid preparation method based on Yunnan pine nuts - Google Patents
R-linolenic acid extraction and pinolenic acid preparation method based on Yunnan pine nuts Download PDFInfo
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Abstract
The invention discloses a r-linolenic acid extraction and pinolenic acid preparation method based on Yunnan pine nuts, belonging to the technical field of preparation of cathode material pole pieces of ultralow temperature batteries, and the method comprises the following specific steps: the method adopts a multi-element extraction solvent and solution to match and mix for use, has simple operation, high production efficiency, high purity of the r-linolenic acid obtained by extraction, and the finally obtained r-linolenic acid reaches more than 99 percent, wherein the pinolenic acid reaches more than 78 percent, and the used extraction agent is easy to prepare, has low energy consumption of equipment and low cost, and is suitable for extracting the r-linolenic acid in the pine seed oil and preparing the pinolenic acid in industrial scale.
Description
Technical Field
The invention relates to the technical field of r-linolenic acid extraction and pinolenic acid preparation, in particular to a r-linolenic acid extraction and pinolenic acid preparation method based on Yunnan pine nuts.
Background
Yunnan pine (Pinus yunnanensis), also known as Feiyong, Qingsong and Chang Mao pine, is an evergreen arbor of Pinus of Pinaceae. The bark is brown gray, and breaks into irregular scales and falls off, the needle leaves are usually bundled by 3 needles (diluted 2 needles), the cone-shaped egg is cone-shaped, the cone is opened when the cone is mature, and the seeds are brown.
Gamma-linolenic Acid (Gamma-linolenic Acid), which is an intermediate for converting linoleic Acid in foods to Prostaglandin (PG) in the human body, has been gaining attention as a fatty Acid (vitamin-F) essential to the human body. The liquid of the r-linolenic acid is colorless or light yellow oil. The solid is white powder, and is commonly named as isolinolenic acid. Linolenic acid is an essential fatty acid component which cannot be lacked by a human body and cannot be synthesized by the human body, and belongs to a vitamin F-like substance. In the absence of the body, the immune, cardiovascular, cerebrovascular and reproductive endocrine systems become abnormal. The gamma-linolenic acid can be converted into prostaglandin E1 in a human body, can inhibit the aggregation of blood platelets and the formation of thromboxane A2, has obvious functions of resisting thrombus and atheromatous plaque, can obviously reduce hyperlipidemia, cholesterol and blood sugar, reduce density lipoprotein and the like, and has obvious curative effects of delaying senility and female premenstrual symptoms. On the other hand, gamma-linolenic acid is an excellent conditioner and nutritional supplement for external use, and can improve blood circulation and cell metabolism. The liposome prepared with phospholipid can be used for smoothing epidermal blood vessels and treating acne and exanthema.
Pinolenic acid (Pinolenic acid): norwegian scientists in 1997 have disclosed for the first time that pine nuts contain an unsaturated fatty acid, which is different from the unsaturated fatty acids in all plants on the earth, and which is only present in pine nut oil, not only can reduce cholesterol (TC), Triglyceride (TG) and increase High Density Lipoprotein (HDL), but also can inhibit and eliminate the adverse effects of other unsaturated fatty acids on the body. The structure of the method is unsaturated fatty acid containing three unsaturated bonds, most of pine nut oil is saturated fatty acid, how to separate saturated fatty acid and unsaturated fatty acid from fatty acid is always a difficult point for research, linoleic acid and linolenic acid are difficult to separate by general non-high-pressure preparation type liquid chromatography, and the existing method has the defects of low yield, difficult urea recovery and the like, needs special molecular distillation equipment, and has high energy consumption, high investment cost and the like.
Therefore, a method for extracting r-linolenic acid and preparing pinolenic acid based on Yunnan pine seeds is provided.
Disclosure of Invention
The invention aims to provide a r-linolenic acid extraction and pinolenic acid preparation method based on Yunnan pine nuts, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a method for extracting r-linolenic acid based on Yunnan pine nuts comprises the following specific steps:
(1) obtaining pine seed oil: mechanically cold pressing Yunnan pine nuts, refining and dewaxing to obtain pine nut oil;
(2) saponification and acidolysis: adding the pine nut oil into an ethanol solution for complete dissolution, slowly adding a sodium hydroxide solution with the mass fraction of 10-20% while stirring for reaction, adjusting the pH value with hydrochloric acid after the reaction is finished, separating an upper oil layer, washing the upper oil layer with water until the water is neutral, and obtaining the separated upper oil layer which is the mixed fatty acid;
(3) urea inclusion: mixing and refluxing urea and ethanol, adding the urea and the ethanol into the mixed fatty acid obtained in the step (2), stirring, standing, filtering, washing with ethanol, collecting filtrate, and evaporating to remove ethanol, wherein an oil layer in the filtrate is the mixed fatty acid enriched with the r-linolenic acid;
(4) complexing with silver nitrate: mixing and stirring the mixed fatty acid coated by urea and a silver nitrate solution at 0 +/-2 ℃, taking a water phase by a separating funnel, extracting the water phase by petroleum ether, collecting an ether layer, repeatedly complexing for 3 times, combining the ether layers, and recovering the petroleum ether by a distillation flask to obtain the r-linolenic acid.
Preferably, the weight ratio of the sodium hydroxide solution to the ethanol in the step (1) is 0.02-0.04: 1.
Preferably, hydrochloric acid with the concentration of 20-50% is added in the step (2), and the pH value is adjusted to 2-3.
Preferably, the ratio of the mixed fatty acid, urea and ethanol in the step (3) is 1: 3: 9.
a preparation method of pinolenic acid based on Yunnan pine nut comprises the following specific steps:
A. preparing an extraction liquid: preparing inorganic ion water solution of copper sulfate 2-4 mol/l, and adding methanol with the volume ratio of 1/8-1/3; the organic phase is petroleum ether containing pentaerythritol tetraoleate with the mass fraction of 10-30%.
B. Saponification treatment: putting the pine nut oil in the step (1) into 60-100% ethanol solution with the volume 4-8 times that of the pine nut oil, adding 10-30% of sodium hydroxide or potassium hydroxide by mass fraction, stirring for 24-48h at room temperature or heating and refluxing for 0.5-2h, recovering the ethanol solution to 1/5-1/2 with the original volume under reduced pressure, adding distilled water to 0.5-2 times of the original volume, adjusting the pH to 2-3, adding n-hexane or petroleum ether with the same volume for extraction for 2-3 times, and recovering an organic solvent under reduced pressure to obtain saponified pine nut oil fatty acid;
C. carrying out pinolenic acid complexation: dissolving saponified oleum Pini koraiensis fatty acid with n-hexane or petroleum ether to obtain 0.2-1.0g/ml organic solution, and mixing at a ratio of 1: 1-1:3, adding the inorganic ion water solution prepared in the step A and petroleum ether containing pentaerythritol tetraoleate with the mass fraction of 10-30%, uniformly stirring, placing the mixture in a reaction kettle at the temperature of zero to 15 ℃, and stirring and extracting;
D. dissociation of pinolenic acid: pouring the extract into a separating funnel, standing for 30-60 minutes, pouring out lower-layer water liquid after the liquid is completely stood and layered, transferring to a reaction kettle, adding equal amount of normal hexane, heating, and stirring and extracting;
E. pinolenic acid elution: and D, standing the extract liquor obtained in the step D, layering, discharging the n-hexane part, adding a saturated sodium chloride solution with the volume being 2-5 times that of the n-hexane, layering and reserving the n-hexane part, eluting with distilled water with the volume being 10-20 times that of the n-hexane, adding anhydrous sodium sulfate into the layered n-hexane part, standing overnight for dewatering, and carrying out reduced pressure distillation to remove the n-hexane to obtain the product.
Preferably, the stirring extraction time in the step B is 25 to 45 minutes.
Preferably, the stirring extraction time in the step C is 25-45 minutes, and the heating temperature in the step C is 50-70 ℃.
Compared with the prior art, the invention has the beneficial effects that:
the method adopts the multi-element mixed solvent and the solution to be matched and mixed for use, has simple operation and high production efficiency, the purity of the r-linolenic acid obtained by extraction is high, the finally obtained r-linolenic acid reaches more than 99 percent, wherein the pinolenic acid reaches more than 78 percent, and the used extractant is easy to prepare and has low cost, thereby being suitable for industrial large-scale production of the pinolenic acid in the pine seed oil.
Detailed Description
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 only a part of the embodiments of the present invention, and not all of the 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.
Example one
A method for extracting r-linolenic acid based on Yunnan pine nuts comprises the following specific steps:
(1) obtaining pine seed oil: mechanically cold pressing Yunnan pine nuts, refining and dewaxing to obtain pine nut oil;
(2) saponification and acidolysis: adding the pine nut oil into an ethanol solution for complete dissolution, slowly adding a sodium hydroxide solution with the mass fraction of 10% while stirring for reaction, adjusting the pH value with hydrochloric acid after the reaction is finished, separating an upper oil layer, washing the upper oil layer with water until the water is neutral, and obtaining the separated upper oil layer which is the mixed fatty acid;
(3) urea inclusion: mixing and refluxing urea and ethanol, adding the urea and the ethanol into the mixed fatty acid obtained in the step (2), stirring, standing, filtering, washing with ethanol, collecting filtrate, and evaporating to remove ethanol, wherein an oil layer in the filtrate is the mixed fatty acid enriched with the r-linolenic acid;
(4) complexing with silver nitrate: mixing and stirring the mixed fatty acid coated by urea and a silver nitrate solution at 0 +/-2 ℃, taking a water phase by a separating funnel, extracting the water phase by petroleum ether, collecting an ether layer, repeatedly complexing for 3 times, combining the ether layers, and recovering the petroleum ether by a distillation flask to obtain the r-linolenic acid.
In this embodiment, the weight ratio of the sodium hydroxide solution to the ethanol in the step (1) is preferably 0.02: 1.
In this embodiment, preferably, hydrochloric acid with a concentration of 20-50% is added in the step (2), and the PH is adjusted to 2.
In this embodiment, preferably, the ratio of the mixed fatty acid, urea, and ethanol in step (3) is 1: 3: 9.
a preparation method of pinolenic acid based on Yunnan pine nut comprises the following specific steps:
A. preparing an extraction liquid: preparing inorganic ionic water solution of copper sulfate 2mol/l, and adding methanol with the volume ratio of 1/8; the organic phase is petroleum ether containing pentaerythritol tetraoleate with the mass fraction of 10-30%.
B. Saponification treatment: putting the pine nut oil in the step (1) into 60% ethanol solution with the volume 4-8 times that of the pine nut oil, adding 10-30% of sodium hydroxide or potassium hydroxide by mass fraction, stirring for 24-48h at room temperature or heating and refluxing for 0.5, recovering the ethanol solution to 1/5 of the original volume under reduced pressure, adding distilled water to 0.5 time of the original volume, adjusting the pH to 2, adding n-hexane or petroleum ether with the same volume for extraction for 2 times, and recovering an organic solvent under reduced pressure to obtain saponified pine nut oil fatty acid;
C. carrying out pinolenic acid complexation: dissolving saponified oleum Pini koraiensis fatty acid with n-hexane or petroleum ether to obtain 0.2g/ml organic solution, and mixing at a ratio of 1: 1, adding the inorganic ion water solution prepared in the step A and petroleum ether containing pentaerythritol tetraoleate with the mass fraction of 10-30% in proportion, uniformly stirring, placing the mixture in a reaction kettle at the temperature of zero to 15 ℃ below zero, and stirring and extracting;
D. dissociation of pinolenic acid: pouring the extract into a separating funnel, standing for 30 minutes, pouring out lower-layer water liquid after the liquid is completely stood and layered, transferring to a reaction kettle, adding equal amount of normal hexane, heating, and stirring and extracting;
E. pinolenic acid elution: and D, standing the extract liquor obtained in the step D, layering, discharging the n-hexane part, adding a saturated sodium chloride solution with the volume being 2 times that of the n-hexane, layering and reserving the n-hexane part, eluting with distilled water with the volume being 10 times that of the n-hexane, adding anhydrous sodium sulfate into the layered n-hexane part, standing overnight for dewatering, and distilling under reduced pressure to remove the n-hexane to obtain the product.
In this embodiment, the stirring extraction time in step B is preferably 25 minutes.
In this embodiment, preferably, the stirring extraction time in step C is 25 minutes, and the heating temperature in step C is 50 ℃.
Example two
A method for extracting r-linolenic acid based on Yunnan pine nuts comprises the following specific steps:
(1) obtaining pine seed oil: mechanically cold pressing Yunnan pine nuts, refining and dewaxing to obtain pine nut oil;
(2) saponification and acidolysis: adding the pine nut oil into an ethanol solution for complete dissolution, slowly adding a sodium hydroxide solution with the mass fraction of 10% while stirring for reaction, adjusting the pH value with hydrochloric acid after the reaction is finished, separating an upper oil layer, washing the upper oil layer with water until the water is neutral, and obtaining the separated upper oil layer which is the mixed fatty acid;
(3) urea inclusion: mixing and refluxing urea and ethanol, adding the urea and the ethanol into the mixed fatty acid obtained in the step (2), stirring, standing, filtering, washing with ethanol, collecting filtrate, and evaporating to remove ethanol, wherein an oil layer in the filtrate is the mixed fatty acid enriched with the r-linolenic acid;
(4) complexing with silver nitrate: mixing and stirring the mixed fatty acid coated by urea and a silver nitrate solution at 0 +/-2 ℃, taking a water phase by a separating funnel, extracting the water phase by petroleum ether, collecting an ether layer, repeatedly complexing for 3 times, combining the ether layers, and recovering the petroleum ether by a distillation flask to obtain the r-linolenic acid.
In this embodiment, the weight ratio of the sodium hydroxide solution to the ethanol in the step (1) is preferably 0.02-0.04: 1.
In this embodiment, preferably, hydrochloric acid with a concentration of 20-50% is added in the step (2), and the PH is adjusted to 2.
In this embodiment, preferably, the ratio of the mixed fatty acid, urea, and ethanol in step (3) is 1: 3: 9.
a preparation method of pinolenic acid based on Yunnan pine nut comprises the following specific steps:
A. preparing an extraction liquid: preparing inorganic ionic water solution of copper sulfate 2mol/l, and adding methanol with the volume ratio of 1/8; the organic phase is petroleum ether containing pentaerythritol tetraoleate with the mass fraction of 20%.
B. Saponification treatment: putting the pine nut oil in the step (1) into 60% ethanol solution with the volume 4 times that of the pine nut oil, adding sodium hydroxide or potassium hydroxide with the mass fraction of 10%, stirring for 24 hours at room temperature or heating and refluxing for 0.5, recovering the ethanol solution to 1/5 of the original volume under reduced pressure, adding distilled water to 0.5 time of the original volume, adjusting the pH to 3, adding n-hexane or petroleum ether with the same volume for extraction for 3 times, and recovering an organic solvent under reduced pressure to obtain saponified pine nut oil fatty acid;
C. carrying out pinolenic acid complexation: dissolving saponified oleum Pini with n-hexane or petroleum ether to obtain 1.0g/ml organic solution, adding the inorganic ion water solution prepared in step A and petroleum ether containing pentaerythritol tetraoleate 10-30% by mass at a ratio of 1:3, stirring, placing in a reaction kettle at-5 deg.C, and stirring for extraction;
D. dissociation of pinolenic acid: pouring the extract into a separating funnel, standing for 60 minutes, pouring out lower-layer water liquid after the liquid is completely stood and layered, transferring to a reaction kettle, adding equal amount of normal hexane, heating, and stirring and extracting;
E. pinolenic acid elution: and D, standing the extract liquor obtained in the step D, layering, discharging the n-hexane part, adding a saturated sodium chloride solution, wherein the volume of the saturated sodium chloride solution is 5 times that of the n-hexane, layering and reserving the n-hexane part, eluting with distilled water, wherein the volume of the saturated sodium chloride solution is 20 times that of the n-hexane, adding anhydrous sodium sulfate to the layered n-hexane part, standing overnight for dewatering, and distilling under reduced pressure to remove the n-hexane to obtain the product.
In this embodiment, the stirring extraction time in step B is preferably 45 minutes.
In this embodiment, preferably, the stirring extraction time in step C is 45 minutes, and the heating temperature in step C is 70 ℃.
EXAMPLE III
A method for extracting r-linolenic acid based on Yunnan pine nuts comprises the following specific steps:
(1) obtaining pine seed oil: mechanically cold pressing Yunnan pine nuts, refining and dewaxing to obtain pine nut oil;
(2) saponification and acidolysis: adding the pine nut oil into an ethanol solution for complete dissolution, slowly adding a sodium hydroxide solution with the mass fraction of 10% while stirring for reaction, adjusting the pH value with hydrochloric acid after the reaction is finished, separating an upper oil layer, washing the upper oil layer with water until the water is neutral, and obtaining the separated upper oil layer which is the mixed fatty acid;
(3) urea inclusion: mixing and refluxing urea and ethanol, adding the urea and the ethanol into the mixed fatty acid obtained in the step (2), stirring, standing, filtering, washing with ethanol, collecting filtrate, and evaporating to remove ethanol, wherein an oil layer in the filtrate is the mixed fatty acid enriched with the r-linolenic acid;
(4) complexing with silver nitrate: mixing and stirring the mixed fatty acid coated by urea and a silver nitrate solution at 0 +/-2 ℃, taking a water phase by a separating funnel, extracting the water phase by petroleum ether, collecting an ether layer, repeatedly complexing for 3 times, combining the ether layers, and recovering the petroleum ether by a distillation flask to obtain the r-linolenic acid.
In this embodiment, the weight ratio of the sodium hydroxide solution to the ethanol in the step (1) is preferably 0.04: 1.
In this embodiment, preferably, hydrochloric acid with a concentration of 30% is added in the step (2), and the PH is adjusted to 3.
In this embodiment, preferably, the ratio of the mixed fatty acid, urea, and ethanol in step (3) is 1: 3: 9.
a preparation method of pinolenic acid based on Yunnan pine nut comprises the following specific steps:
A. preparing an extraction liquid: preparing inorganic ionic water solution of copper sulfate 2mol/l, and adding methanol with the volume ratio of 1/8; the organic phase is petroleum ether containing pentaerythritol tetraoleate with a mass fraction of 10-%.
B. Saponification treatment: putting the pine nut oil in the step (1) into 60% ethanol solution with the volume 4 times that of the pine nut oil, adding sodium hydroxide or potassium hydroxide with the mass fraction of 10%, stirring for 24 hours at room temperature or heating and refluxing for 0.5, recovering the ethanol solution to 1/4 of the original volume under reduced pressure, adding distilled water to 1 time of the original volume, adjusting the pH to 3, adding n-hexane or petroleum ether with the same volume for extraction for 3 times, and recovering an organic solvent under reduced pressure to obtain saponified pine nut oil fatty acid;
C. carrying out pinolenic acid complexation: dissolving saponified oleum Pini with n-hexane or petroleum ether to obtain 1.0g/ml organic solution, adding the inorganic ion water solution prepared in step A and petroleum ether containing pentaerythritol tetraoleate 10-30% by mass at a ratio of 1:3, stirring, placing in a reaction kettle at-5 deg.C, and stirring for extraction;
D. dissociation of pinolenic acid: pouring the extract into a separating funnel, standing for 60 minutes, pouring out lower-layer water liquid after the liquid is completely stood and layered, transferring to a reaction kettle, adding equal amount of normal hexane, heating, and stirring and extracting;
E. pinolenic acid elution: and D, standing the extract liquor obtained in the step D, layering, discharging the n-hexane part, adding a saturated sodium chloride solution, wherein the volume of the saturated sodium chloride solution is 5 times that of the n-hexane, layering and reserving the n-hexane part, eluting with distilled water, wherein the volume of the saturated sodium chloride solution is 20 times that of the n-hexane, adding anhydrous sodium sulfate to the layered n-hexane part, standing overnight for dewatering, and distilling under reduced pressure to remove the n-hexane to obtain the product.
In this embodiment, the stirring extraction time in step B is preferably 35 minutes.
In this embodiment, preferably, the stirring extraction time in step C is 35 minutes, and the heating temperature in step C is 70 ℃.
The method adopts the multi-element mixed solvent and the solution to be matched and mixed for use, has simple operation and high production efficiency, the purity of the r-linolenic acid obtained by extraction is high, the finally obtained r-linolenic acid reaches more than 99 percent, wherein the pinolenic acid reaches more than 78 percent, and the used extractant is easy to prepare and has low cost, thereby being suitable for industrial large-scale production of the pinolenic acid in the pine seed oil.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A method for extracting r-linolenic acid based on Yunnan pine nuts is characterized by comprising the following steps: the method comprises the following specific steps:
(1) obtaining pine seed oil: mechanically cold pressing Yunnan pine nuts, refining and dewaxing to obtain pine nut oil;
(2) saponification and acidolysis: adding the pine nut oil into an ethanol solution for complete dissolution, slowly adding a sodium hydroxide solution with the mass fraction of 10-20% while stirring for reaction, adjusting the pH value with hydrochloric acid after the reaction is finished, separating an upper oil layer, washing the upper oil layer with water until the water is neutral, and obtaining the separated upper oil layer which is the mixed fatty acid;
(3) urea inclusion: mixing and refluxing urea and ethanol, adding the urea and the ethanol into the mixed fatty acid obtained in the step (2), stirring, standing, filtering, washing with ethanol, collecting filtrate, and evaporating to remove ethanol, wherein an oil layer in the filtrate is the mixed fatty acid enriched with the r-linolenic acid;
(4) complexing with silver nitrate: mixing and stirring the mixed fatty acid coated by urea and a silver nitrate solution at 0 +/-2 ℃, taking a water phase by a separating funnel, extracting the water phase by petroleum ether, collecting an ether layer, repeatedly complexing for 3 times, combining the ether layers, and recovering the petroleum ether by a distillation flask to obtain the r-linolenic acid.
2. The method for r-linolenic acid extraction and pinolenic acid preparation based on Yunnan pine nuts as claimed in claim 1, which is characterized in that: the weight ratio of the sodium hydroxide solution to the ethanol in the step (1) is 0.02-0.04: 1.
3. The method for r-linolenic acid extraction and pinolenic acid preparation based on Yunnan pine nuts as claimed in claim 1, which is characterized in that: adding hydrochloric acid with the concentration of 20-50% in the step (2), and adjusting the pH value to 2-3.
4. The method for r-linolenic acid extraction and pinolenic acid preparation based on Yunnan pine nuts as claimed in claim 1, which is characterized in that: the proportion of the mixed fatty acid, the urea and the ethanol in the step (3) is 1: 3: 9.
5. a pinolenic acid preparation method based on Yunnan pine seeds is characterized in that: the method comprises the following specific steps:
A. preparing an extraction liquid: preparing inorganic ion water solution of copper sulfate 2-4 mol/l, and adding methanol with the volume ratio of 1/8-1/3; the organic phase is petroleum ether containing pentaerythritol tetraoleate with the mass fraction of 10-30%.
B. Saponification treatment: putting the pine nut oil in the step (1) into 60-100% ethanol solution with the volume 4-8 times that of the pine nut oil, adding 10-30% of sodium hydroxide or potassium hydroxide by mass fraction, stirring for 24-48h at room temperature or heating and refluxing for 0.5-2h, recovering the ethanol solution to 1/5-1/2 with the original volume under reduced pressure, adding distilled water to 0.5-2 times of the original volume, adjusting the pH to 2-3, adding n-hexane or petroleum ether with the same volume for extraction for 2-3 times, and recovering an organic solvent under reduced pressure to obtain saponified pine nut oil fatty acid;
C. carrying out pinolenic acid complexation: dissolving saponified oleum Pini koraiensis fatty acid with n-hexane or petroleum ether to obtain 0.2-1.0g/ml organic solution, and mixing at a ratio of 1: 1-1:3, adding the inorganic ion water solution prepared in the step A and petroleum ether containing pentaerythritol tetraoleate with the mass fraction of 10-30%, uniformly stirring, placing the mixture in a reaction kettle at the temperature of zero to 15 ℃, and stirring and extracting;
D. dissociation of pinolenic acid: pouring the extract into a separating funnel, standing for 30-60 minutes, pouring out lower-layer water liquid after the liquid is completely stood and layered, transferring to a reaction kettle, adding equal amount of normal hexane, heating, and stirring and extracting;
E. pinolenic acid elution: and D, standing the extract liquor obtained in the step D, layering, discharging the n-hexane part, adding a saturated sodium chloride solution with the volume being 2-5 times that of the n-hexane, layering and reserving the n-hexane part, eluting with distilled water with the volume being 10-20 times that of the n-hexane, adding anhydrous sodium sulfate into the layered n-hexane part, standing overnight for dewatering, and carrying out reduced pressure distillation to remove the n-hexane to obtain the product.
6. The method for preparing pinolenic acid based on Yunnan pine nut as claimed in claim 5, wherein: and the stirring extraction time in the step B is 25-45 minutes.
7. The method for preparing pinolenic acid based on Yunnan pine nut as claimed in claim 5, wherein: and C, stirring and extracting for 25-45 minutes, wherein the heating temperature in the step C is 50-70 ℃.
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| CN1333047A (en) * | 2001-06-21 | 2002-01-30 | 昆明生宝生物技术有限公司 | Yunnan pine nut extract and preparation process and use thereof |
| CN102041159A (en) * | 2010-12-18 | 2011-05-04 | 胡保军 | Method for refining pine nut kernel essential oil |
| CN102150711A (en) * | 2011-02-22 | 2011-08-17 | 云南恩典科技产业发展有限公司 | Health product with efficacy of assisting in blood fat reduction and preparation method thereof |
| CN104418726A (en) * | 2013-08-20 | 2015-03-18 | 陕西中鼎华盛农业发展有限公司 | Extraction method of [alpha]-linolenic acid |
| CN105925363A (en) * | 2016-04-17 | 2016-09-07 | 吉林派诺生物技术股份有限公司 | Extracting method of pine seed oil with low acid value and pinolenic acid |
| CN106433949A (en) * | 2016-09-09 | 2017-02-22 | 王俊人 | Low-acid-value Yunnan pine seed oil, preparation method and application thereof |
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