CN101461424A - Supercritical CO2 extraction method of medlar seed oil - Google Patents
Supercritical CO2 extraction method of medlar seed oil Download PDFInfo
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- CN101461424A CN101461424A CNA2009100291171A CN200910029117A CN101461424A CN 101461424 A CN101461424 A CN 101461424A CN A2009100291171 A CNA2009100291171 A CN A2009100291171A CN 200910029117 A CN200910029117 A CN 200910029117A CN 101461424 A CN101461424 A CN 101461424A
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Abstract
The invention discloses a method for extracting boxthorn seed oil by supercritical CO2. The method comprises the following steps: a, drying and grinding boxthorn seeds and loading in extraction kettle; b, injecting the supercritical CO2 into the extraction kettle, and extracting under the temperature of 40-50 degrees centigrade, pressure of 30-40Mpa and CO2 flow rate of 8-18L/min for 2.5-4 hours; c, inducing the CO2 fluid solved with boxthorn seed oil into a separation kettle, separating out the boxthorn seed oil by adjusting temperature and pressure, compressing the CO2 gas and inducing into the extraction kettle for circulation. The invention has a simple process and convenient operation, avoids the organic solvent residue, shortens the extraction time, increases the boxthorn seed oil extraction efficiency, especially increases the contents of alpha-linolenic acid and gamma-linolenic acid in the boxthorn seed oil greatly.
Description
Technical field
The present invention relates to a kind of extracting process of Boxthorn Seed Oil, particularly a kind of method with the gas extraction Boxthorn Seed Oil belongs to vegetable oil extractive technique scope.
Background technology
The fruit of Chinese wolfberry is traditional rare Chinese medicine, is the fruit of matrimony vine, and the beginning is carried Shennong's Herbal, classifies as top grade.Has effect nourishing liver and kidney, benefiting shrewd head.Ming Dynasty's Li Shizhen (1518-1593 A.D.) is put down in writing in Compendium of Material Medica, " perverse trends in the matrimony vine master five, pine for quenching one's thirst, general arthralgia rheumatism.Obey hard muscles and bones for a long time, it is not old to make light of one's life by commiting suicide.Cold-resistant heat, lower breast side of body gas.The hot headache of visitor is mended internal injury, Da Lao void.Reinforcing yin essence, sharp intestine and small intestine.Mend vital essence deficiency, easy color, bleach, make eye bright and calm the nerves, make us long-lived ".Modern clinically be widely used in antifatigue, improve immunity of organism, anti-ageing, regulate aspects such as blood fat and blood sugar.
The matrimony vine seed is the byproduct in the matrimony vine process, accounts for about 3% of matrimony vine.The oil yield of matrimony vine seed contains a large amount of unrighted acids in the Boxthorn Seed Oil about 17～20%, contain VE, phosphatide, trace element, SOD etc. in addition, is the very high vegetable oil of a kind of nutritive value.The traditional extraction process of Boxthorn Seed Oil has the water distillation to extract, directly squeezing is extracted and organic solvent extractionprocess.Utilizing these three kinds of methods to extract Boxthorn Seed Oil all has drawback, and Boxthorn Seed Oil is a fixed oil, is difficult for steaming with water vapour; The matrimony vine seed is harder, and the milling process oil yield is low, is not suitable for; The Chinese holly seed Qi oil that organic solvent extracts has dissolvent residual and peculiar smell, and the product purity of extracting is low, product quality is relatively poor.
Recently, supercritical CO has appearred using
2The method of extraction Boxthorn Seed Oil is CN1266092A as publication number, and the Chinese invention patent ublic specification of application that open day is on September 13rd, 2000 " is used supercritical CO
2Extraction separates matrimony vine oil from the matrimony vine seed ".This method comprises the steps: a, isolated matrimony vine seed in the fresh matrimony vine berry is packed in the extraction kettle; B, with the CO of supercriticality
2Gas injects extraction kettle, and in temperature be: 36～38 ℃, pressure is: under 25～27MPa condition, extracted 6～7 hours; C, be dissolved with the CO of Boxthorn Seed Oil
2Fluid enters separating still, by regulating temperature and pressure Boxthorn Seed Oil is separated.With this method extraction Boxthorn Seed Oil, though can not produce organic solvent residue, extract overlong time, extraction efficiency is not high.
Granted publication number is CN100400133C, and Granted publication day is the Chinese invention patent " supercritical Chinese wolfberry fruit dregs extract and production method thereof " on July 9th, 2008.This method is that the slag dregs of rice after squeezing the juice with matrimony vine are raw material, through water cleaning, dehydration, drying, pulverizing, supercritical extract, technical process such as separator separation, rectifying column rectifying, technic index is: extracting pressure 30-36MPa, extraction temperature 45-50 ℃, dry back moisture is reduced to below 12%, through supercritical CO
2The weight percentage of alpha-linolenic acid is that the weight percentage of 1-2%, gamma-Linolenic acid is 3-4% in the product after the extraction, and still, the extraction quantity of alpha-linolenic acid and gamma-Linolenic acid is all lower.
Summary of the invention
Technical problem to be solved by this invention provides a kind of supercritical CO
2The method of Boxthorn Seed Oil in the extraction matrimony vine seed, this method technology is simple, easy to operate, avoided organic solvent residue, shorten extraction time, improved the extraction efficiency of Boxthorn Seed Oil, improved the content of alpha-linolenic acid, gamma-Linolenic acid in the Boxthorn Seed Oil especially greatly.
In order to solve the problems of the technologies described above supercritical CO of the present invention
2The method step of extraction Boxthorn Seed Oil is as follows:
A, with in the extraction kettle of packing into after the matrimony vine seed drying and crushing;
B, with the CO of supercriticality
2Injecting extraction kettle, is 40～50 ℃ in temperature, and pressure is 30～40MPa, CO
2Flow velocity is: under the condition of 8～18L/min, extracted 2.5～4 hours;
C, be dissolved with the CO of Boxthorn Seed Oil
2Fluid enters separating still, Boxthorn Seed Oil is separated CO by regulating temperature and pressure
2Gas enters extraction kettle after compression and recycles.
Above-mentioned supercritical CO
2The method of extraction Boxthorn Seed Oil, wherein, described supercritical CO
2The preferred temperature of extraction is 43 ℃, and pressure is 35Mpa, CO
2Flow velocity is 12L/min.
Above-mentioned supercritical CO
2The method of extraction Boxthorn Seed Oil, wherein, described drying is carried out in temperature is lower than 60 ℃ baking oven, and dry 5～7 hours, the matrimony vine seed water content after the drying was lower than 8%.
Above-mentioned supercritical CO
2The method of extraction Boxthorn Seed Oil, wherein, weight percentage 〉=3% of alpha-linolenic acid in the Boxthorn Seed Oil of extraction gained, the weight percentage of gamma-Linolenic acid 〉=4%.
Supercritical CO of the present invention
2The method of extraction Boxthorn Seed Oil earlier with matrimony vine seed drying and crushing, has overcome because matrimony vine seed shell is hard CO before extracting
2Fluid can't penetrate its shell and the incomplete defective of extraction that causes, has increased matrimony vine seed and CO
2The contact area of fluid was pulverized 40 mesh sieves with the matrimony vine seed simultaneously, and its granularity just makes CO
2Fluid is smooth and easy circulation in extraction process, contacts more fully with the matrimony vine seed, thereby has further improved the extraction efficiency of Boxthorn Seed Oil.
Supercritical CO of the present invention
2Used CO in the method for extraction Boxthorn Seed Oil
2Purity is more than or equal to 99%, CO
2Be inert gas, can operate at normal temperatures, can prevent the oxidation and the decomposition of thermal sensitivity composition and chemically unstable composition effectively, utilize CO
2Be in the big character of the high density, low viscosity and the diffusion coefficient that have under the supercriticality and extract active ingredient in the matrimony vine seed, and then the method that heats up with step-down will be dissolved in CO
2Solute in the fluid separates, and plays the double action of extracting with distillation, can finish a leaching process in 2.5～4 hours.This method operation cycle is short, extraction efficiency is high, can avoid organic solvent residue simultaneously, in addition, because CO
2Cheap and easy to get, general recyclable about 80%, saved the energy, simultaneously because CO
2No flammability, safe in utilization and environmentally safe.
Supercritical CO of the present invention
2The method technology of extraction Boxthorn Seed Oil is simple, easy to operate, has greatly improved production efficiency, with the Boxthorn Seed Oil of this method extraction, the weight percentage of alpha-linolenic acid 〉=3% wherein, the weight percentage of gamma-Linolenic acid 〉=4% is 43 ℃ in temperature especially, pressure is 35Mpa, CO
2Flow velocity is that the weight percentage of alpha-linolenic acid in the Boxthorn Seed Oil that extracts under the condition of 12L/min is 4.3%, and the weight percentage of gamma-Linolenic acid is 5.2%, and effect of extracting is remarkable.Alpha-linolenic acid is to constitute the necessary aliphatic acid of human body, can not synthesize in vivo, must provide by meals, alpha-linolenic acid is synthetic DHA and EPA in human body, and that DHA plays a part growing of the division of brain cell, propagation, nerve conduction, cynapse, dendron is very important, is the essential material that brain forms and IQ is developed.Gamma-Linolenic acid has tangible anti peroxidation of lipid, reduces T-CHOL, improves HDL, suppresses platelet aggregation and thromboxane A
2Synthesize, bring high blood pressure down, suppress effects such as ulcer and gastrorrhagia, increase insulin secretion, fat-reducing.
The specific embodiment
Below in conjunction with example the present invention is described in detail.
In order to solve the problems of the technologies described above the present invention's supercritical CO
2The method of extraction Boxthorn Seed Oil, wherein, the step of described method is as follows:
A, with in the extraction kettle of packing into after the matrimony vine seed drying and crushing;
B, with the CO of supercriticality
2Injecting extraction kettle, is 40～50 ℃ in temperature, and pressure is 30～40MPa, CO
2Flow velocity is: under the condition of 8～18L/min, extracted 2.5～4 hours;
C, be dissolved with the CO of Boxthorn Seed Oil
2Fluid enters separating still, Boxthorn Seed Oil is separated CO by regulating temperature and pressure
2Gas enters extraction kettle after compression and recycles.
Example one
The matrimony vine seed was dried by the fire 6 hours in 55 ℃ baking oven, and the matrimony vine seed water content after the drying is 5%, and dried matrimony vine seed was pulverized 40 mesh sieves, and the matrimony vine seed after will sieving is then put into supercritical extraction reactor and extracted.In temperature is 43 ℃, and pressure is 35Mpa, CO
2Flow velocity is under the condition of 12L/min, extracts 3 hours, and Boxthorn Seed Oil is dissolved in supercritical CO
2In the fluid, enter in the separating still, be dissolved in supercritical CO through overregulating temperature and pressure, making
2Boxthorn Seed Oil in the fluid is separated, CO
2Recycle.
Detect the active ingredient in the Boxthorn Seed Oil, wherein the weight percentage of alpha-linolenic acid is 4.3%, and the weight percentage of gamma-Linolenic acid is 5.2%.
Example two:
The matrimony vine seed was dried by the fire 5 hours in 50 ℃ baking oven, and the matrimony vine seed water content after the drying is 7%, and dried matrimony vine seed was pulverized 40 mesh sieves, and the matrimony vine seed after will sieving is then put into supercritical extraction reactor and extracted.In temperature is 40 ℃, and pressure is 40Mpa, CO
2Flow velocity is under the condition of 8L/min, extracts 4 hours, and Boxthorn Seed Oil is dissolved in supercritical CO
2In the fluid, enter in the separating still, be dissolved in supercritical CO through overregulating temperature and pressure, making
2Boxthorn Seed Oil in the fluid is separated, CO
2Recycle.
Detect the active ingredient in the Boxthorn Seed Oil, wherein the weight percentage of alpha-linolenic acid is 3.7%, and the weight percentage of gamma-Linolenic acid is 4.7%.
Example three:
The matrimony vine seed was dried by the fire 7 hours in 45 ℃ baking oven, and the matrimony vine seed water content after the drying is 6%, and dried matrimony vine seed was pulverized 40 mesh sieves, and the matrimony vine seed after will sieving is then put into supercritical extraction reactor and extracted.In temperature is 50 ℃, and pressure is 30Mpa, CO
2Flow velocity is under the condition of 18L/min, extracts 2.5 hours, and Boxthorn Seed Oil is dissolved in supercritical CO
2In the fluid, enter in the separating still, be dissolved in supercritical CO through overregulating temperature and pressure, making
2Boxthorn Seed Oil in the fluid is separated, CO
2Recycle.
Detect the active ingredient in the Boxthorn Seed Oil, wherein the weight percentage of alpha-linolenic acid is 3.2%, and the weight percentage of gamma-Linolenic acid is 4.3%.
Here description of the invention and application is illustrative, is not to want that therefore, the present invention is not subjected to the restriction of present embodiment with scope restriction of the present invention in the above-described embodiments, and the technical scheme that any employing equivalence replacement obtains is all in the scope of protection of the invention.
Claims (4)
1, supercritical CO
2The method of extraction Boxthorn Seed Oil is characterized in that described method step is as follows:
A, with in the extraction kettle of packing into after the matrimony vine seed drying and crushing;
B, with the CO of supercriticality
2Injecting extraction kettle, is 40～50 ℃ in temperature, and pressure is 30～40MPa, CO
2Flow velocity is: under the condition of 8～18L/min, extracted 2.5～4 hours;
C, be dissolved with the CO of Boxthorn Seed Oil
2Fluid enters separating still, Boxthorn Seed Oil is separated CO by regulating temperature and pressure
2Gas enters extraction kettle after compression and recycles.
2, supercritical CO as claimed in claim 1
2The method of extraction Boxthorn Seed Oil is characterized in that described supercritical CO
2The preferred temperature of extraction is 43 ℃, and pressure is 35Mpa, CO
2Flow velocity is 12L/min.
3, supercritical CO as claimed in claim 1 or 2
2The method of extraction Boxthorn Seed Oil is characterized in that described drying is carried out in temperature is lower than 60 ℃ baking oven, dry 5～7 hours, the matrimony vine seed water content after the drying was lower than 8%.
4, supercritical CO as claimed in claim 3
2The method of extraction Boxthorn Seed Oil is characterized in that, weight percentage 〉=3% of alpha-linolenic acid in the Boxthorn Seed Oil of extraction gained, the weight percentage of gamma-Linolenic acid 〉=4%.
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| CNA2009100291171A CN101461424A (en) | 2009-01-13 | 2009-01-13 | Supercritical CO2 extraction method of medlar seed oil |
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| CNA2009100291171A CN101461424A (en) | 2009-01-13 | 2009-01-13 | Supercritical CO2 extraction method of medlar seed oil |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102071099A (en) * | 2011-01-07 | 2011-05-25 | 中国科学院西北高原生物研究所 | Process for quickly breaking cell walls of Chinese wolfberry seeds and extracting seed oil |
| CN103082291A (en) * | 2013-02-28 | 2013-05-08 | 上海基赛生物医药科技有限公司 | Industrial application technology of lycium ruthenicum fruit |
| CN103710135A (en) * | 2013-12-13 | 2014-04-09 | 广西科技大学 | Pure plant modifier used before supercritical CO2 extraction of Lycium seed oil |
| CN103710136A (en) * | 2013-12-13 | 2014-04-09 | 广西科技大学 | Pretreatment agent for supercritical CO2 extraction of wolfberry fruit oil |
| CN103725415A (en) * | 2013-12-13 | 2014-04-16 | 广西科技大学 | Additive for supercritical CO2 extraction of medlar seed oil |
| CN103789085A (en) * | 2014-02-20 | 2014-05-14 | 陕西师范大学 | Method for extracting gynostemma pentaphylla seed oil by using supercritical carbon dioxide |
| CN105132119A (en) * | 2015-10-09 | 2015-12-09 | 青海泰柏特生物科技有限公司 | Method for preparing boxthorn seed oil through enzymolysis |
| CN105341569A (en) * | 2015-10-11 | 2016-02-24 | 青海泰柏特生物科技有限公司 | Whole lycium ruthenicum juice and preparation method thereof |
| CN108611182A (en) * | 2018-06-29 | 2018-10-02 | 成都纺织高等专科学校 | A kind of supercritical CO2Extract the method and system of Boxthorn Seed Oil |
| CN108704034A (en) * | 2018-08-24 | 2018-10-26 | 宁夏医科大学 | Application of the Boxthorn Seed Oil in preparing testicular function damage disease prevention product |
| CN111154547A (en) * | 2020-01-10 | 2020-05-15 | 中国科学院西北高原生物研究所 | Supercritical fluid extraction method of Chinese iris seed oil and application thereof |
-
2009
- 2009-01-13 CN CNA2009100291171A patent/CN101461424A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102071099B (en) * | 2011-01-07 | 2013-06-19 | 中国科学院西北高原生物研究所 | Process for quickly breaking cell walls of Chinese wolfberry seeds and extracting seed oil |
| CN102071099A (en) * | 2011-01-07 | 2011-05-25 | 中国科学院西北高原生物研究所 | Process for quickly breaking cell walls of Chinese wolfberry seeds and extracting seed oil |
| CN103082291A (en) * | 2013-02-28 | 2013-05-08 | 上海基赛生物医药科技有限公司 | Industrial application technology of lycium ruthenicum fruit |
| CN103710136B (en) * | 2013-12-13 | 2016-03-02 | 广西科技大学 | A kind of SCF-CO 2 Boxthorn Seed Oil pretreating reagent |
| CN103710135A (en) * | 2013-12-13 | 2014-04-09 | 广西科技大学 | Pure plant modifier used before supercritical CO2 extraction of Lycium seed oil |
| CN103710136A (en) * | 2013-12-13 | 2014-04-09 | 广西科技大学 | Pretreatment agent for supercritical CO2 extraction of wolfberry fruit oil |
| CN103725415A (en) * | 2013-12-13 | 2014-04-16 | 广西科技大学 | Additive for supercritical CO2 extraction of medlar seed oil |
| CN103725415B (en) * | 2013-12-13 | 2015-10-07 | 广西科技大学 | A kind of supercritical CO 2extraction Boxthorn Seed Oil additive |
| CN103789085A (en) * | 2014-02-20 | 2014-05-14 | 陕西师范大学 | Method for extracting gynostemma pentaphylla seed oil by using supercritical carbon dioxide |
| CN105132119A (en) * | 2015-10-09 | 2015-12-09 | 青海泰柏特生物科技有限公司 | Method for preparing boxthorn seed oil through enzymolysis |
| CN105341569A (en) * | 2015-10-11 | 2016-02-24 | 青海泰柏特生物科技有限公司 | Whole lycium ruthenicum juice and preparation method thereof |
| CN108611182A (en) * | 2018-06-29 | 2018-10-02 | 成都纺织高等专科学校 | A kind of supercritical CO2Extract the method and system of Boxthorn Seed Oil |
| CN108704034A (en) * | 2018-08-24 | 2018-10-26 | 宁夏医科大学 | Application of the Boxthorn Seed Oil in preparing testicular function damage disease prevention product |
| CN111154547A (en) * | 2020-01-10 | 2020-05-15 | 中国科学院西北高原生物研究所 | Supercritical fluid extraction method of Chinese iris seed oil and application thereof |
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Open date: 20090624 |