CN105886116A - Method for subcritical fluid extraction of wolfberry seed oil - Google Patents
Method for subcritical fluid extraction of wolfberry seed oil Download PDFInfo
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- CN105886116A CN105886116A CN201410499370.4A CN201410499370A CN105886116A CN 105886116 A CN105886116 A CN 105886116A CN 201410499370 A CN201410499370 A CN 201410499370A CN 105886116 A CN105886116 A CN 105886116A
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Abstract
The invention discloses a method for subcritical fluid extraction of wolfberry seed oil. The method comprises 1, sun-drying or baking wolfberry seeds obtained through fresh wolfberry juicing to obtain dry wolfberry seeds, 2, putting the dried wolfberry seeds and an extraction agent into an extraction reactor of a subcritical fluid extraction device according to a material dissolution mass-volume ratio of 1: 1-1: 20 and carrying out continuous extraction 1-20 times, for 10-150min every time, so that extract is obtained, 3, separating the extract in the step 2 through a decompression heating method under separation pressure of 0.10-1.95MPa at a separation temperature of 10-90 DEG C to obtain extract, and 4, standing the extract at the room temperature for 10-90min to obtain wolfberry seed oil. The method effectively reduces a production cost, shortens extraction separation time, reduces solvent consumption and energy consumption in a process, has simple processes, strong operability and high extraction efficiency, is environmentally friendly, has no pollution, has good safety and repeatability and realizes large-scale industrialized continuous production.
Description
Technical field
The present invention relates to a kind of boxthorn seed oil extracting method, a kind of method particularly relating to subcritical fluid extraction boxthorn seed oil.
Background technology
The wolfberry juice obtained after broken by Fructus Lycii, the Fructus Lycii that particularly obtains after broken with new fresh fructus lycii is fresh squeezes the juice, day at home and abroad
Benefit is popular.Existing wolfberry juice in process of production, can obtain the seed of Fructus Lycii containing abundant nutrition composition.Seed of Fructus Lycii through squeezing or
Can obtain boxthorn seed oil after the methods such as extraction are refined, seed of Fructus Lycii oil yield is 17%-20%.In boxthorn seed oil containing substantial amounts of not
Satisfied fatty acid, VE and phospholipid, the most linoleic content is up to 66.5%, and VE content is 42.02mg/100g, content of phospholipid
Being 0.75%, content beta-carotene is 0.73mg/100g, is the vegetable oil of a kind of great health care.Boxthorn seed oil contains
There are substantial amounts of nutritional labeling and biological active substances, in addition to having edibility, also medical care effect, may be used for height
The auxiliary treatment of the cardiovascular and cerebrovascular diseases such as blood pressure, hyperlipidemia, atherosclerosis.
The extraction of boxthorn seed oil at present mainly uses Mechanical Method, organic solvent method and supercritical fluid extraction.Mechanical expression method
Squeezing time length, oil yield is low, impurity content is high, oil quality is poor, and color and luster is deeper;When there is extraction in organic solvent extractionprocess
Between long, inefficient, solvent-oil ratio is big, and easily causes in product a series of drawbacks such as dissolvent residual;And supercritical fluid
Extraction requires height to instrument and equipment, and technological process is complicated, and volume of equipment is little, cost is high, energy consumption is big, is not suitable for extensive
Industrialization continuity produces.
Subcritical fluid extraction technology is to develop the most quick novel extractive technique in the last few years, is also a skill of extraction industry
Art revolution.Subcritical fluid extraction technology is to utilize subcritical fluids to hold as extractant, the pressure in airtight, anaerobic, low pressure
In device, according to the similar principle mixed of Organic substance, by extraction material and extractant molecule diffusion process in immersion process,
Reach in the extractant that the liposoluble constituent in solid material transfers to liquid, then by the process of reduction vaporization by extractant and mesh
Product separate, finally give a kind of novel extraction and the isolation technics of purpose product.Extract with traditional solvent extraction and supercritical
The technology of taking is compared, and subcritical abstraction had both had supercritical extraction extraction efficiency height, the advantage of product no solvent residue, the most again
There is the features such as Conventional solvents extraction equipment cost is low, technological process is simple, production cost is low, and whole extraction process
Carry out under conditions of airtight anoxybiotic, low-temp low-pressure, be particularly suitable for similar boxthorn seed oil etc. rich in unsaturated fatty acids acid lipid
Industrialization continuity produces.
Summary of the invention
A kind of method that it is an object of the invention to provide subcritical fluid extraction boxthorn seed oil, it can be effectively improved boxthorn seed oil
Extraction efficiency, be suitable to industrialized production.
In order to achieve the above object, the technical solution of the present invention is: a kind of method of subcritical fluid extraction boxthorn seed oil,
It comprises the steps:
(1) after being squeezed the juice by medlar fresh fruit, the seed of Fructus Lycii of gained dries or dries, and obtains dried wolfberry seed;
(2) by dried wolfberry seed in step (1) and extractant by expecting that molten mass volume ratio is 1: 1~1: 20 to put into Asia and face
Continuous extraction 1~20 times in the extraction kettle of boundary's fluid extraction device, each 10~150min, it is extracted thing;
(3) utilize decompression temperature-raising method make extract in step (2) separating pressure be 0.10~1.95MPa, separation temperature
Separate under conditions of being 10~90 DEG C, be extracted liquid;
(4) by after the extract left at room temperature 10~90min in step (3), boxthorn seed oil is obtained.
The method of subcritical fluid extraction boxthorn seed oil of the present invention, in wherein said step (2), extractant is propane, butane, different
Any one in butane, dimethyl ether, liquefied petroleum gas, HFA 134a.
The method of subcritical fluid extraction boxthorn seed oil of the present invention, in wherein said step (2) extraction conditions be extraction temperature 5~
85 DEG C, extracting pressure 0.15~2.95MPa, extractant flow 10~200L/h.
After using such scheme, the present invention compared with prior art has the advantage that
1, use the side-product seed of Fructus Lycii in wolfberry juice processing to be raw material due to the present invention, therefore significantly reduce production cost;
2, the present invention uses subcritical fluid extraction and isolation technics, not only significantly reduces production cost, shortens extraction point
From the time, decrease solvent-oil ratio and energy consumption in technical process, and technological process is simple, workable, extraction efficiency
Height, environmental protection, pollution-free, safety and reproducible, heavy industrialization consecutive production can be realized;
3, carry out under conditions of airtight anoxybiotic, low-temp low-pressure due to whole extraction process, therefore, be particularly suitable for similar Fructus Lycii
Seed oil etc. produce rich in the industrialization continuity of unsaturated fatty acids acid lipid;
4, extraction efficiency of the present invention is high, and Extraction solvent can be recycled, with conventional method extract the yield of boxthorn seed oil be 5.7%~
6.4%, and use the inventive method yield up to 8.0%~9.5%;
5, the boxthorn seed oil of gained of the present invention is faint yellow, and clear shape has the fragrance that boxthorn seed oil is special, and quality is preferable.
Detailed description of the invention
The method illustrating subcritical fluid extraction boxthorn seed oil of the present invention below in conjunction with embodiment.
Embodiment 1
The method of subcritical fluid extraction boxthorn seed oil of the present invention, it comprises the steps:
(1) after being squeezed the juice by medlar fresh fruit, the seed of Fructus Lycii of gained dries or dries, and obtains dried wolfberry seed;
(2) seed of Fructus Lycii after processing presses material molten mass volume ratio (the seed of Fructus Lycii quality: extractant of 1: 1 with extractant-propane
Volume ratio) (g/mL) put into subcritical fluid extraction device (this subcritical abstraction device be the extraction of existing market sale
And the subcritical abstraction instrument of segregation apparatus, such as Henan Province subcritical Bioisystech Co., Ltd production and selling) extraction kettle in,
Extraction temperature be 5 DEG C, extracting pressure be 0.15MPa, extractant flow be 10L/h under conditions of continuous extraction 1 time, every time
10min, is extracted thing;
(3) utilize decompression temperature-raising method make extract separating pressure be 0.10MPa, separation temperature be 10 DEG C under conditions of carry out point
From, it is extracted liquid;Wherein subcritical fluid extraction agent is become gaseous state from liquid and is recycled;
(4), after extract left at room temperature 72min, boxthorn seed oil is obtained.
This boxthorn seed oil yield is 18.27%, and GC-MS (gas chromatograph-mass spectrometer (GC-MS)) analyzes, and linoleic acid content is 60.246%.
Embodiment 2
The method of subcritical fluid extraction boxthorn seed oil of the present invention, it comprises the steps:
(1) after being squeezed the juice by medlar fresh fruit, the seed of Fructus Lycii of gained dries or dries, and obtains dried wolfberry seed;
(2) seed of Fructus Lycii after processing presses the material molten mass volume ratio (Chinese holly of 1: 20 with extractant-HFA 134a
Qi seed quality: extractant volume ratio) (g/mL) put in the extraction kettle of subcritical fluid extraction device, in extraction temperature be
85 DEG C, extracting pressure be 2.95MPa, extractant flow be continuous extraction 20 times under conditions of 200L/h, each 150min,
It is extracted thing;
(3) utilize decompression temperature-raising method make extract separating pressure be 1.95MPa, separation temperature be 90 DEG C under conditions of carry out point
From, it is extracted liquid;Wherein subcritical fluid extraction agent is become gaseous state from liquid and is recycled;
(4), after extract left at room temperature 30min, boxthorn seed oil is obtained.
This boxthorn seed oil yield is 18.60%, and GC-MS analyzes, and linoleic acid content is 61.230%.
Embodiment 3
The method of subcritical fluid extraction boxthorn seed oil of the present invention, it comprises the steps:
(1) after being squeezed the juice by medlar fresh fruit, the seed of Fructus Lycii of gained dries or dries, and obtains dried wolfberry seed;
(2) seed of Fructus Lycii after processing presses material molten mass volume ratio (the seed of Fructus Lycii quality: extractant of 1: 5 with extractant-butane
Volume ratio) (g/mL) put in the extraction kettle of subcritical fluid extraction device, extraction temperature be 45 DEG C, extracting pressure be
0.55MPa, extractant flow are continuous extraction 5 times, each 40min under conditions of 80L/h, are extracted thing;
(3) utilize decompression temperature-raising method make extract separating pressure be 0.20MPa, separation temperature be 50 DEG C under conditions of carry out point
From, it is extracted liquid;Wherein subcritical fluid extraction agent is become gaseous state from liquid and is recycled;
(4), after extract left at room temperature 40min, boxthorn seed oil is obtained.
This boxthorn seed oil yield is 19.15%, and GC-MS analyzes, and linoleic acid content is 62.345%.
Embodiment 4
The method of subcritical fluid extraction boxthorn seed oil of the present invention, it comprises the steps:
(1) after being squeezed the juice by medlar fresh fruit, the seed of Fructus Lycii of gained dries or dries, and obtains dried wolfberry seed;
(2) seed of Fructus Lycii after processing presses material molten mass volume ratio (the seed of Fructus Lycii quality: extractant of 1: 3 with extractant-iso-butane
Volume ratio) (g/mL) put in the extraction kettle of subcritical fluid extraction device, extraction temperature be 35 DEG C, extracting pressure be
1.05MPa, extractant flow are continuous extraction 8 times, each 30min under conditions of 100L/h, are extracted thing;
(3) utilize decompression temperature-raising method make extract separating pressure be 0.45MPa, separation temperature be 60 DEG C under conditions of carry out point
From, it is extracted liquid;Wherein subcritical fluid extraction agent is become gaseous state from liquid and is recycled;
(4), after extract left at room temperature 10min, boxthorn seed oil is obtained.
This boxthorn seed oil yield is 18.33%, and GC-MS analyzes, and linoleic acid content is 62.781%.
Embodiment 5
The method of subcritical fluid extraction boxthorn seed oil of the present invention, it comprises the steps:
(1) after being squeezed the juice by medlar fresh fruit, the seed of Fructus Lycii of gained dries or dries, and obtains dried wolfberry seed;
(2) seed of Fructus Lycii after processing and extractant-dimethyl ether press the molten mass volume ratio of material of 1: 10 (seed of Fructus Lycii quality: extraction
Agent volume ratio) (g/mL) put in the extraction kettle of subcritical fluid extraction device, is 45 DEG C, extracting pressure in extraction temperature
It is continuous extraction 10 times, each 90min under conditions of 50L/h for 0.45MPa, extractant flow, is extracted thing;
(3) utilize decompression temperature-raising method make extract separating pressure be 1.05MPa, separation temperature be 30 DEG C under conditions of carry out point
From, it is extracted liquid;Wherein subcritical fluid extraction agent is become gaseous state from liquid and is recycled;
(4), after extract left at room temperature 90min, boxthorn seed oil is obtained.
This boxthorn seed oil yield is 18.52%, and GC-MS analyzes, and linoleic acid content is 61.456%.
Embodiment 6
The method of subcritical fluid extraction boxthorn seed oil of the present invention, it comprises the steps:
(1) after being squeezed the juice by medlar fresh fruit, the seed of Fructus Lycii of gained dries or dries, and obtains dried wolfberry seed;
(2) seed of Fructus Lycii and the extractant-liquefied petroleum gas after processing by 1: 15 the molten mass volume ratio of material (seed of Fructus Lycii quality:
Extractant volume ratio) (g/mL) put in the extraction kettle of subcritical fluid extraction device, is 65 DEG C, extraction in extraction temperature
Pressure is 1.95MPa, extractant flow is continuous extraction 14 times, each 20min under conditions of 120L/h, is extracted thing;
(3) utilize decompression temperature-raising method make extract separating pressure be 1.60MPa, separation temperature be 75 DEG C under conditions of carry out point
From, it is extracted liquid;Wherein subcritical fluid extraction agent is become gaseous state from liquid and is recycled;
(4), after extract left at room temperature 65min, boxthorn seed oil is obtained.
This boxthorn seed oil yield is 18.92%, and GC-MS analyzes, and linoleic acid content is 62.783%.
Embodiment described above is only to be described the preferred embodiment of the present invention, not limits the scope of the present invention
Fixed, on the premise of designing spirit without departing from the present invention, technical scheme is made by this area ordinary skill technical staff
Various deformation and improvement, all should fall in the protection domain that claims of the present invention determines.
Claims (3)
1. the method for a subcritical fluid extraction boxthorn seed oil, it is characterised in that: comprise the steps:
(1) after being squeezed the juice by medlar fresh fruit, the seed of Fructus Lycii of gained dries or dries, and obtains dried wolfberry seed;
(2) by dried wolfberry seed in step (1) and extractant by expecting that molten mass volume ratio is 1: 1~1: 20 to put into Asia and face
Continuous extraction 1~20 times in the extraction kettle of boundary's fluid extraction device, each 10~150min, it is extracted thing;
(3) utilize decompression temperature-raising method make extract in step (2) separating pressure be 0.10~1.95MPa, separation temperature
Separate under conditions of being 10~90 DEG C, be extracted liquid;
(4) by after the extract left at room temperature 10~90min in step (3), boxthorn seed oil is obtained.
2. the method for subcritical fluid extraction boxthorn seed oil as claimed in claim 1, it is characterised in that: described step (2)
Middle extractant is any one in propane, butane, iso-butane, dimethyl ether, liquefied petroleum gas, HFA 134a.
3. the method for subcritical fluid extraction boxthorn seed oil as claimed in claim 1, it is characterised in that: described step (2)
Middle extraction conditions is extraction temperature 5~85 DEG C, extracting pressure 0.15~2.95MPa, extractant flow 10~200L/h.
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Cited By (6)
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CN106281667A (en) * | 2016-11-19 | 2017-01-04 | 青海泰柏特生物科技有限公司 | A kind of method of subcritical fluid extraction Quinoa seed oil |
CN106675774A (en) * | 2017-02-10 | 2017-05-17 | 合肥师范学院 | Method for extracting blueberry seed oil with subcritical extraction method |
CN106995747A (en) * | 2017-06-14 | 2017-08-01 | 中国科学院兰州化学物理研究所 | A kind of air-flow ultramicro grinding and the method for ultrasonic subcritical abstraction combined extracting fructus lycii oil |
CN107474963A (en) * | 2017-09-01 | 2017-12-15 | 云南巴菰生物科技有限公司 | A kind of cordate houttuynia essential oil cigarette is with quick-fried pearl and preparation method thereof |
CN108251218A (en) * | 2018-02-11 | 2018-07-06 | 安阳工学院 | A kind of method of highly selective extraction north Chinese mugwort essential oil |
CN110106025A (en) * | 2019-05-07 | 2019-08-09 | 南宁辰康生物科技有限公司 | Method for extracting citronella oil |
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CN102504941A (en) * | 2011-11-22 | 2012-06-20 | 中国科学院西北高原生物研究所 | Method for extracting chufa bean oil from subcritical fluid |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106281667A (en) * | 2016-11-19 | 2017-01-04 | 青海泰柏特生物科技有限公司 | A kind of method of subcritical fluid extraction Quinoa seed oil |
CN106675774A (en) * | 2017-02-10 | 2017-05-17 | 合肥师范学院 | Method for extracting blueberry seed oil with subcritical extraction method |
CN106995747A (en) * | 2017-06-14 | 2017-08-01 | 中国科学院兰州化学物理研究所 | A kind of air-flow ultramicro grinding and the method for ultrasonic subcritical abstraction combined extracting fructus lycii oil |
CN107474963A (en) * | 2017-09-01 | 2017-12-15 | 云南巴菰生物科技有限公司 | A kind of cordate houttuynia essential oil cigarette is with quick-fried pearl and preparation method thereof |
CN108251218A (en) * | 2018-02-11 | 2018-07-06 | 安阳工学院 | A kind of method of highly selective extraction north Chinese mugwort essential oil |
CN108251218B (en) * | 2018-02-11 | 2021-06-15 | 安阳工学院 | Method for extracting artemisia vulgaris essential oil with high selectivity |
CN110106025A (en) * | 2019-05-07 | 2019-08-09 | 南宁辰康生物科技有限公司 | Method for extracting citronella oil |
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