CN106995747A - A kind of air-flow ultramicro grinding and the method for ultrasonic subcritical abstraction combined extracting fructus lycii oil - Google Patents
A kind of air-flow ultramicro grinding and the method for ultrasonic subcritical abstraction combined extracting fructus lycii oil Download PDFInfo
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- CN106995747A CN106995747A CN201710449498.3A CN201710449498A CN106995747A CN 106995747 A CN106995747 A CN 106995747A CN 201710449498 A CN201710449498 A CN 201710449498A CN 106995747 A CN106995747 A CN 106995747A
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- fructus lycii
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/106—Production of fats or fatty oils from raw materials by extracting using ultra-sounds
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/108—Production of fats or fatty oils from raw materials by extracting after-treatment, e.g. of miscellae
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/008—Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
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- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The present invention is a kind of air-flow ultramicro grinding and the method for ultrasonic subcritical abstraction combined extracting fructus lycii oil, belongs to matrimony vine field of deep.The present invention is with the dry fruit of the full fruit of matrimony vine（Including matrimony vine seed）For raw material, first after ultramicro grinding, then through ultrasonic subcritical abstraction, the fat-soluble effective active composition in the full fruit of matrimony vine is efficiently extracted, the fat-soluble active ingredient of matrimony vine Central Plains ecological material is maintained to the full extent；The oily yield of fructus lycii is also significantly increased simultaneously；Obtained fructus lycii oil is not only comprising the liposoluble constituent in the matrimony vines such as linoleic acid, alpha linolenic acid, the acid and gamma-linolenic beneficial to human body, also comprising the wolfberry pigment with improving eyesight effect；The aliphatic acid based on linoleic acid can also play a part of protecting wolfberry pigment not oxidized and inactivating simultaneously.In addition, simple production process of the present invention, and can continuously produce, green pollution-free, solvent is recyclable, and production cost is low, is adapted to scale industrial production.
Description
Technical field
The present invention relates to a kind of fructus lycii oil extracting method, more particularly to a kind of air-flow ultramicro grinding and ultrasound it is subcritical
The method for extracting combined extracting fructus lycii oil, belongs to matrimony vine field of deep.
Background technology
Matrimony vine possesses vast cultivated area and extensive consumer groups as one of kind of integration of drinking and medicinal herbs in China,
But in addition to Chinese medicine is made, the use of matrimony vine is generally that dry fruit is directly eaten, and its added value of product is relatively low, and matrimony vine deep process technology is system
The bottleneck factor that about wolfberry industry develops.
Fructus lycii oil is the liposoluble active position in matrimony vine, containing a variety of active materials beneficial to human body, is mainly had
A variety of aliphatic acid such as linoleic acid, alpha-linolenic acid, gamma-Linolenic acid, oleic acid, palmitic acid, and carotenoidses wolfberry pigment.Mesh
Before, the preparation method of fructus lycii oil is generally traditional solvent extraction method, and temperature is high, the time is long, the thermal activity in fructus lycii oil
Material is vulnerable to destruction, and production cost is higher, easily pollutes environment, it is more crucial be fructus lycii oil extraction efficiency it is not high, yield and
The content of active material is relatively low, have impact on the availability of matrimony vine, and extraction effect is poor with expense.
CN105886116A discloses the method using subcritical fluid extraction Boxthorn Seed Oil, be using matrimony vine seed as raw material,
Boxthorn Seed Oil is obtained using subcritical abstraction technology, its active site is the aliphatic acid in the aliphatic acid in matrimony vine seed, fructus lycii
It can not be extracted with wolfberry pigment active component.
CN104774690A discloses the production technology of a kind of fruit of Chinese wolfberry essential oil and edible dregs of rice powder, is by the fruit of Chinese wolfberry or its kind
Son is pressed into after base through subcritical abstraction, separation of solid and liquid, obtains the solid wet dregs of rice and mixed solution；Mixed solution is de- through parsing evaporation
Extractant is removed, crude oil is obtained；Crude oil is further refined through molecular distillation, obtains matrimony vine sub-functionality essential oil；The solid wet dregs of rice take off
It is residual it is molten after, low temperature drying, powder expanded, processed cross 100-180 mesh sieves, that is, obtain the fruit of Chinese wolfberry and eat dregs of rice powder.Pressed in this method obtained by embryo
Material thickness be generally sheet material, thickness is between 0.2 ~ 0.4mm, and its material table area is still smaller, to the Chinese holly in matrimony vine
Qi seed can not be accomplished to crush, and effectively can not be extracted Boxthorn Seed Oil in subcritical abstraction, several in gained matrimony vine essential oil
Boxthorn Seed Oil is free of, therefore the availability extracted to matrimony vine is not high, the yield and activity substance content of matrimony vine essential oil are also failed to understand
Really.
The method that CN105130867B discloses zeaxanthin in a kind of Extraction and enrichment fruit of Chinese wolfberry, is by dried wolfberry
Put into continuous extraction in the extraction kettle of subcritical fluid extraction device by a certain percentage with extractant and obtain extract；Again one
Constant-pressure is with a temperature of to the isolated extract of extract；Then it is extracted with ethyl acetate after extract is stood at room temperature,
Medicinal extract is concentrated into after reclaiming organic phase；Finally dilute medicinal extract, upper large pore resin absorption column, with ethanol elution, gained eluent time
Receive after ethanol, zeaxanthin is obtained with alcohol crystal.Because the target product of this method is zeaxanthin, the patent is not to matrimony vine
Raw material is pre-processed, and other active materials in Boxthorn Seed Oil and matrimony vine are practically free of in its subcritical abstraction thing, into
Divide single, the availability extracted to matrimony vine is not high, have impact on the comprehensive utilization of matrimony vine.
The content of the invention
The purpose of the present invention is high, biological there is provided a kind of yield the problem of presence for prior art extraction fructus lycii oil
Activity substance content is high, cost is low, the method for extracting fructus lycii oil of environmental protection.
The method that the present invention extracts fructus lycii oil, is comprised the following steps that：
（1）Air-flow ultramicro grinding：The full dried fruit fruit of matrimony vine（Including matrimony vine seed）Powder of the air-flow ultramicro grinding into 10 ~ 100 μm of particle diameter；
（2）The subcritical combined extraction of ultrasound：The molten ratio of material of matrimony vine powder and extractant is controlled 1:1.2~1:3kg/L, extraction
Ultrasonic subcritical combined extraction is carried out under the conditions of 20 DEG C ~ 50 DEG C of temperature, 0.2 MPa of extracting pressure ~ 0.5Mpa, lucifuge.
Extractant is LPG, butane, high-purity isobutane（R600a）, 1,1,1,2- HFC-134as（R134a）、
Dimethyl ether etc.（Purity 100%）.
Supersonic frequency is 10KHz ~ 30KHz, and extraction time is 15min ~ 60min.
Extract as continuous extraction, extraction times are 1 ~ 5 time.
（3）Precipitation：After ultrasonic subcritical abstraction terminates, extractant is extracted out, and extraction material and extractant are distinguished
It is evaporated after precipitation, extractant precipitation and produces fructus lycii oil.Precipitation temperature control at 10 DEG C ~ 40 DEG C, pressure is -0.09 ~ -
0.05MPa。
（4）Solvent recovery：The gas-solvent evaporated from material and extractant, is compressed and liquefied by diaphragm type compressor
After reclaim.
After testing, the yield that the present invention extracts fructus lycii oil is 5.2% ~ 13.9%.In fructus lycii oil product, linoleic acid content
For 61.3% ~ 72.8%, alpha-linolenic acid content is 0.8% ~ 1.6%, gamma-Linolenic acid 2.4% ~ 3.7%, wolfberry pigment content is 1.5% ~
3.9%。
The present invention has the advantages that compared with prior art：
1st, the present invention is using normal temperature extraction, and low temperature desolventizing overcomes traditional solvent extraction method and needs to heat in separation process and steams
Evaporate, destroy the shortcomings of easily there is dissolvent residual in the active material of thermal sensitivity and easy oxidized, wolfberry fruit extract in matrimony vine, make Chinese holly
Active component in Qi is preserved in ecosystem form；
2nd, air-flow superfine communication technique both solved matrimony vine become it is glutinous be difficult to crush, the broken effect of matrimony vine seed powder is bad, matrimony vine powder grain
Footpath is bigger than normal to wait the unfavorable factor of influence extraction efficiency, and avoid crush or pressure embryo during matrimony vine heat-sensitive active material
Loss, retains the bioactivity and various nutritional ingredients of powder to greatest extent, and the structure for reducing nutrition and active material changes
Become and lose；
3rd, using air-flow ultramicro grinding and ultrasonic subcritical abstraction GC-MS, the infiltration of the fat-soluble active ingredient in matrimony vine is made
Property and solvability significantly improve, while it is high to also significantly increase the oily yield of fructus lycii；Obtain fructus lycii oil not only comprising pair
Liposoluble constituent in the matrimony vines such as the beneficial linoleic acid of human body, alpha-linolenic acid, gamma-Linolenic acid, also comprising with improving eyesight effect
Wolfberry pigment；The aliphatic acid based on linoleic acid can also play a part of protecting wolfberry pigment not oxidized and inactivating simultaneously；
4th, simple production process of the present invention, and can continuously produce, green pollution-free；Solvent is recyclable, subtracts
Few solvent loss, it is cost-effective, it is adapted to scale industrial production actual.
Embodiment
The method that fructus lycii oil is extracted to the present invention below by specific embodiment is further described.
Embodiment 1
The full dried fruit fruit of matrimony vine（Including matrimony vine seed）Air-flow ultramicro grinding, particle diameter is 80 μm.Weigh 30.2kg and be positioned over subcritical extraction
In the closed extractor of taking equipment, feeding-passage is closed, -0.075MPa is evacuated to, by solid-liquid ratio 1:1.3 kg/L inject liquid
State butane solvent 39.3L, is heated to 35 DEG C, extracting pressure is 0.3MPa, supersonic frequency is 15KHz, and lucifuge is extracted 4 times, extraction
Time 30min/ times.After the completion of extraction, extraction solution is drawn in knockout drum.Vavuum pump is opened, by the pressure drop of knockout drum
To -0.06MPa, temperature is maintained at the butane in 35 DEG C, evaporation material, while the butane of gasification is compressed into through diaphragm type compressor
Liquid, is back in solvent tank, in case recycling.Vavuum pump is closed, the air pressure valve of knockout drum is opened, makes the pressure of knockout drum
0MPa is reached, discharge fructus lycii oil imports plate filter filtering, obtains fructus lycii oil product 1.58kg, its Linoleic acid contains
Measure as 70.6%, alpha-linolenic acid content is 1.5%, gamma-Linolenic acid 3.6%, wolfberry pigment content is 3.4%.
Embodiment 2
The full dried fruit fruit of matrimony vine（Including matrimony vine seed）Air-flow ultramicro grinding, particle diameter is 20 μm.Weigh 40.6kg and be positioned over subcritical extraction
In the closed extractor of taking equipment, feeding-passage is closed, -0.075MPa is evacuated to, by solid-liquid ratio 1:1.5 kg/L inject liquid
State diformazan ether solvents 60.9L, is heated to 30 DEG C, extracting pressure is 0.35MPa, supersonic frequency is 25KHz, and lucifuge is extracted 3 times, extraction
It is 50min/ times to take the time.After the completion of extraction, extraction solution is drawn in knockout drum.Vavuum pump is opened, by the pressure of knockout drum
Power is down to -0.06MPa, and temperature is maintained at the dimethyl ether in 30 DEG C, evaporation material, while the dimethyl ether of gasification is compressed into liquid
State, is back in solvent tank, in case recycling.Vavuum pump is closed, the air pressure valve of knockout drum is opened, reaches the pressure of knockout drum
To 0MPa, discharge fructus lycii oil imports plate filter filtering, obtains fructus lycii oil product 5.6kg, wherein linoleic acid content is
61.7%, alpha-linolenic acid content is 0.9%, gamma-Linolenic acid 1.5%, and wolfberry pigment content is 2.1%.
Embodiment 3
The full dried fruit fruit of matrimony vine（Including matrimony vine seed）Air-flow ultramicro grinding, particle diameter is 40 μm.Weigh 40.3kg and be positioned over subcritical extraction
In the closed extractor of taking equipment, feeding-passage is closed, -0.075MPa is evacuated to, by solid-liquid ratio 1:1.6kg/L injects liquid
Butane solvent 64.5L, is heated to 35 DEG C, extracting pressure is 0.3MPa, supersonic frequency is 25KHz, and lucifuge is extracted 3 times, during extraction
Between be 40min/ times.After the completion of extraction, extraction solution is drawn in knockout drum.Vavuum pump is opened, by the pressure drop of knockout drum
To -0.08MPa, temperature is maintained at the butane in 35 DEG C, evaporation material, while the butane of gasification is compressed into through diaphragm type compressor
Liquid, is back in solvent tank, in case recycling.Vavuum pump is closed, the air pressure valve of knockout drum is opened, makes the pressure of knockout drum
0MPa is reached, discharge fructus lycii oil imports plate filter filtering, obtains fructus lycii oil product 4.6kg, wherein linoleic acid content
For 71.1%, alpha-linolenic acid content is 1.4%, gamma-Linolenic acid 3.5%, and wolfberry pigment content is 3.5%.
Embodiment 4
The full dried fruit fruit of matrimony vine（Including matrimony vine seed）Air-flow ultramicro grinding, particle diameter is 20 μm.Weigh 100.6kg and be positioned over subcritical extraction
In the closed extractor of taking equipment, feeding-passage is closed, -0.075MPa is evacuated to, by solid-liquid ratio 1:1.8kg/L injects liquid
Butane solvent 181L, is heated to 40 DEG C, extracting pressure is 0.4MPa, supersonic frequency is 28KHz, and lucifuge is extracted 4 times, extraction time
For 40min/ times.After the completion of extraction, extraction solution is drawn in knockout drum.Vavuum pump is opened, the pressure of knockout drum is down to-
0.08MPa, temperature is maintained at the butane in 40 DEG C, evaporation material, while the butane of gasification is compressed into liquid, is back to solvent
In tank, in case recycling.Vavuum pump is closed, the air pressure valve of knockout drum is opened, the pressure of knockout drum is reached 0MPa, discharges Chinese holly
Fructus lycii oil, imports plate filter filtering, obtains fructus lycii oil product 12.4kg, wherein linoleic acid content is 70.3%, α-flax
Acid content is 1.2%, gamma-Linolenic acid 2.9%, and wolfberry pigment content is 3.7%.
Claims (6)
1. a kind of air-flow ultramicro grinding and the method for ultrasonic subcritical abstraction combined extracting fructus lycii oil, including following technique step
Suddenly：
（1）Air-flow ultramicro grinding：Powder of the full dried fruit fruit air-flow ultramicro grinding of matrimony vine into 10 ~ 100 μm of particle diameter；The full fruit of matrimony vine
Dry fruit includes matrimony vine seed and fructus lycii；
（2）Ultrasonic subcritical abstraction：The molten ratio of material of matrimony vine powder and extractant is controlled 1:1.2~1:3kg/L, extraction temperature
20 DEG C ~ 50 DEG C, 0.2 MPa of extracting pressure ~ 0.5Mpa carries out ultrasonic subcritical combined extraction under the conditions of lucifuge；
（3）Precipitation：After ultrasonic subcritical abstraction terminates, extractant is extracted out, and extraction material and extractant are carried out respectively
Evaporate and fructus lycii oil is produced after precipitation, extractant precipitation；
（4）Solvent recovery：The gas-solvent evaporated from material and extractant, is returned after diaphragm type compressor is compressed and liquefied
Receive.
2. air-flow ultramicro grinding as claimed in claim 1 and the method for ultrasonic subcritical abstraction combined extracting fructus lycii oil, it is special
Levy and be：Step（2）Extractant be LPG, butane, high-purity isobutane, 1,1,1,2- HFC-134as or diformazan
Ether.
3. air-flow ultramicro grinding as claimed in claim 1 and the method for ultrasonic subcritical abstraction combined extracting fructus lycii oil, it is special
Levy and be：Step（2）Supersonic frequency be 10KHz ~ 30KHz.
4. air-flow ultramicro grinding as claimed in claim 1 and the method for ultrasonic subcritical abstraction combined extracting fructus lycii oil, it is special
Levy and be：Step（2）Extraction time be 15min ~ 60min.
5. air-flow ultramicro grinding as claimed in claim 1 and the method for ultrasonic subcritical abstraction combined extracting fructus lycii oil, it is special
Levy and be：Step（2）Extraction be continuous extraction, extraction times be 1 ~ 5 time.
6. air-flow ultramicro grinding as claimed in claim 1 and the method for ultrasonic subcritical abstraction combined extracting fructus lycii oil, it is special
Levy and be：Precipitation temperature control is at 10 DEG C ~ 40 DEG C, and pressure is -0.09 ~ -0.05MPa.
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Cited By (5)
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| 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 |
| CN107674758A (en) * | 2017-11-22 | 2018-02-09 | 中国科学院兰州化学物理研究所 | The method for extracting coffee grease from coffee grounds using ultrasonic subcritical fluid extraction technology |
| CN111280356A (en) * | 2020-03-27 | 2020-06-16 | 中国科学院兰州化学物理研究所 | Medlar beverage and preparation method thereof |
| CN112251284A (en) * | 2020-10-11 | 2021-01-22 | 甘肃省科学院生物研究所 | Method for extracting and refining sea-buckthorn whole fruit oil |
| CN114158621A (en) * | 2021-12-10 | 2022-03-11 | 宁夏九宝生态农业科技发展有限公司 | Composition of wolfberry fruit oil and walnut oil and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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| CN111280356A (en) * | 2020-03-27 | 2020-06-16 | 中国科学院兰州化学物理研究所 | Medlar beverage and preparation method thereof |
| CN112251284A (en) * | 2020-10-11 | 2021-01-22 | 甘肃省科学院生物研究所 | Method for extracting and refining sea-buckthorn whole fruit oil |
| CN114158621A (en) * | 2021-12-10 | 2022-03-11 | 宁夏九宝生态农业科技发展有限公司 | Composition of wolfberry fruit oil and walnut oil and application thereof |
| CN114158621B (en) * | 2021-12-10 | 2024-03-26 | 宁夏九宝生态农业科技发展有限公司 | A composition containing oleum Lycii and oleum Juglandis and its application |
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