CN108949351A - Fennel seeds extraction process of active component - Google Patents
Fennel seeds extraction process of active component Download PDFInfo
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- CN108949351A CN108949351A CN201710379748.0A CN201710379748A CN108949351A CN 108949351 A CN108949351 A CN 108949351A CN 201710379748 A CN201710379748 A CN 201710379748A CN 108949351 A CN108949351 A CN 108949351A
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- fennel seeds
- extracting method
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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
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
-
- 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
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
- Fats And Perfumes (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The present invention relates to active constituent extractive technique field more particularly to fennel seeds extraction process of active component.The present invention provides the extracting method of fennel seeds active material, this method first is extracted to obtain medicinal extract with subcritical extraction method, then volatile oil and fat oil are separated from medicinal extract.Wherein, the yield of medicinal extract is 10%~15%.The yield of volatile oil is 1.6%~2.1%, wherein the relative amount of trans--isoesdragol is 70%~80%；The yield of fat oil is 8%~13.2%, and wherein the relative amount of petroselinic acid is 65%.
Description
Technical field
The present invention relates to active constituent extractive technique field more particularly to fennel seeds extraction process of active component.
Background technique
Fennel seeds (Foeniculu Vulgare Mill) are annual herb plant, also known as bosom is fragrant, the fragrant son in bosom, fennel
Son.Fennel seeds are a kind of multiduty plants, and during dish, medicine, fragrance are built, fresh and tender cauline leaf is edible vegetable, and fruit is culinary art
Fragrance, root, leaf, fruit and herb are all traditional Chinese medicine.Fennel seeds are loaded in Tang Materia Medica as common Chinese medicine earliest,
Its dry mature fruit has the function of regulating qi-flowing for harmonizing stomach, eliminating cold to stop pain, thus be usually used in treat cold hernia stomachache, dysmenorrhea, deficiency of food vomit and diarrhoea,
The illnesss such as abdomen crymodynia, abdominal distention, the testis swelling and hanging down of either of the testes and hydrocele testis.At abroad, the fruit or essential oil of fennel are also extensive
(such as applied to medicine and pharmacology (such as nourishing agent, peptic, excitant, carminative, galactopoietic, antemetic, expectorant), cosmetics
Toothpaste, perfumed soap, pastil, leaves shampoo etc.) and food additives (bread, cake, sweet wine and pickles etc.).
Currently, the processing and utilization of fennel seeds is mainly used for extracting volatile oil.Work of the Fructus Foeniculi volatile oil as fennel seeds
Property one of ingredient, main component is trans--isoesdragol, and verified, Fructus Foeniculi volatile oil has antibacterial, anti-oxidant, desinsection
The effects of, and can be used for improving infantile diarrhea, improve primary dysmenorrhea, protection hepatic injury etc..Common volatile oil extracting side
Method is steam distillation.This method is after directly moistening the immersion of fennel seeds fragment, and heating distills or is passed through direct steam, makes
Volatile component is taken out of with steam distillation, is condensed aggregation and (essence) oil that volatilized after water-oil separating.Vapor steams
Although evaporating method simple process, volatilization oil yield is lower, and remaining solid residue carries out secondary mention after extraction volatile oil
Need to remove water dry solvent extraction again when (extract medicinal extract) being taken to utilize, when consumption energy consumption.
In addition, another kind of main active constituent is fat oil in fennel seeds, the main component of fennel seeds fat oil is ocean
Ceriander seed acid (Petroselinic acid, tarelaidic acid), since fennel seeds fat oil belongs to unsaturated fat
Acid, so the metabolism of animal will be played an important role.Also, due to the special construction of petroselinic acid, may be used also
For use as production nylon66 fiber or lauric raw material.
However, the volatile oil of fennel seeds is had focused largely on to the research of fennel seeds main active extraction process at present
On, and research to fatty oil extract and few.Also, fat oil is separated with prior art, during the separation process, volatile oil
It is heated to be scattered and disappeared.And the part also unrenewable extraction in fat oil remaining after fennel seeds extraction volatile oil.Therefore, it develops
One kind can efficiently and high-quality extracts fatty oil component in fennel seeds, and can facilitate the process of separation and Extraction volatile oil,
And be easily achieved and applied in production, it is always institute of manufacturer urgent problem to be solved in the industry.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is that providing fennel seeds extraction process of active component；The present invention
The method of offer can make full use of raw material, utilize same a raw material, not only fractionation of fatty oil, but also separation volatile oil.
The extracting method of fennel seeds active constituent provided by the invention, comprising:
After fennel seeds seed is crushed, subcritical abstraction is carried out by extractant of butane, fennel fruit is made through precipitation in extract liquor
Fragrant medicinal extract；
The fennel seeds medicinal extract is extracted with steam distillation, and vapor portion separates light phase after condensing as fennel seeds volatilization
Oil；Fennel seeds medicinal extract after extraction is through dry obtained fennel seeds fat oil.
In the embodiment of the present invention, it is 0.2~0.5mm that fennel seeds seed, which is crushed to partial size,.
Subcritical abstraction (Sub-critical fluid extraction technology) is to utilize subcritical fluids
As extractant, closed, anaerobic, low pressure pressure vessel in, according to the similar principle to mix of organic matter, pass through extraction material
With molecule diffusion process of the extractant in soaking process, reach the extraction that the liposoluble constituent in solid material is transferred to liquid
In agent, then by be evaporated under reduced pressure process extractant is separated with purpose product, finally obtain purpose product a kind of extraction and
Isolation technics.The present invention selects butane as extractant.The high osmosis that subcritical butane has is extracted using subcritical butane
The extraction efficiency of fennel seeds medicinal extract is high, can closed extraction at relatively low temperatures and pressures, and to be not required to heating i.e. gasifiable
It is separated with extract, no solvent residue, heat-sensitive ingredients are not damaged.
In the embodiment of the present invention, quality-volume ratio of fennel seeds seed and butane is 5~8g/mL after the crushing.It is i.e. every
5~8g fennel seeds seed is extracted with the butane of 1mL.
In the embodiment of the present invention, the temperature of the subcritical abstraction is 30~50 DEG C, and extracting pressure is 0.2~0.45MPa,
Extraction time is 20~50min.
In some embodiments, quality-volume ratio of fennel seeds seed and butane is 5g/mL after crushing；Subcritical abstraction
Temperature is 30 DEG C, extracting pressure 0.2MPa, extraction time 20min.
In some embodiments, quality-volume ratio of fennel seeds seed and butane is 8g/mL after crushing；Subcritical abstraction
Temperature is 50 DEG C, extracting pressure 0.45MPa, extraction time 50min.
In some embodiments, quality-volume ratio of fennel seeds seed and butane is 6g/mL after crushing；Subcritical abstraction
Temperature is 40 DEG C, extracting pressure 0.35MPa, extraction time 30min.
The precipitation refers to removing solvent.In the embodiment of the present invention, the mode of the precipitation is that constant temperature depressurizes precipitation, will be divided
It is reduced from pressure tank.The temperature of the precipitation is 50~60 DEG C.
Steam distillation extraction is meant the medicinal material containing volatile component and water condistillation, steams volatile component with water
Gas distillates together, and the leach extraction method of volatile component is taken through condensation point.In the embodiment of the present invention, the steam distillation is extracted
In, the mass ratio of water and the fennel seeds medicinal extract is (1~2): 1.
In the embodiment of the present invention, the vapo(u)rizing temperature that the steam distillation is extracted is 80~90 DEG C, distillation time is 90~
150min。
In some embodiments, the mass ratio of water and the fennel seeds medicinal extract is 1:1.Vapo(u)rizing temperature is 80 DEG C, distillation time
For 90min.
In some embodiments, the mass ratio of water and the fennel seeds medicinal extract is 2:1.Vapo(u)rizing temperature is 90 DEG C, distillation time
For 150min.
In some embodiments, the mass ratio of water and the fennel seeds medicinal extract is 1.5:1.Vapo(u)rizing temperature is 85 DEG C, when distillation
Between be 120min.
Specifically, extracting method of the invention are as follows:
It is 0.2~0.5mm that fennel seeds seed, which is crushed to partial size, and with butane, (every 5~8g fennel seeds seed adds 1mL fourth
Alkane) it is that extractant carries out subcritical abstraction, through 30~50 DEG C, 0.2~0.45MPa, extract 20~50min；Extract liquor is through constant temperature
Fennel seeds medicinal extract is made in (50~60 DEG C) decompression precipitations；
The fennel seeds medicinal extract is mixed with the water of 1~2 times of quality, and 80~90 DEG C of steam distillations extract 90~150min,
It is Fructus Foeniculi volatile oil that vapor portion separates light phase after condensing；Fennel seeds medicinal extract after extraction is through dry obtained fennel seeds fat
Oil.
Fennel seeds medicinal extract is carried out steam distillation and extracts volatile oil by the present invention, rather than directlys adopt fennel powder, can
To substantially reduce the dosage of water, only 1/5 or so of conventional method, and extraction time is only the 1/2 of conventional method, extracts temperature
Degree also reduces by 20~30 DEG C compared with conventional method, therefore substantially reduces energy consumption, also improves extraction efficiency.
The present invention provides Fructus Foeniculi volatile oil made from extracting method.
The present invention provides fennel seeds fat oil made from extracting method.
The present invention provides the extracting method of fennel seeds active material, this method first is extracted to obtain with subcritical extraction method
Medicinal extract, then volatile oil and fat oil are separated from medicinal extract.Wherein, the yield of medicinal extract is 10%~15%.The yield of volatile oil is
1.6%~2.1%, wherein the relative amount of trans--isoesdragol is 70%~80%；The yield of fat oil be 8%~
13.2%, wherein the relative amount of petroselinic acid is 65%.
Specific embodiment
The present invention provides fennel seeds extraction process of active component, those skilled in the art can use for reference present disclosure, fit
When improvement realization of process parameters.In particular, it should be pointed out that all similar substitutions and modifications are for a person skilled in the art
It is it will be apparent that they are considered as being included in the present invention.Method of the invention and application passed through preferred embodiment into
Description is gone, related personnel can obviously not depart from the content of present invention, carried out in spirit and scope to methods herein and application
Change or appropriate changes and combinations, carry out implementation and application the technology of the present invention.
Below with reference to embodiment, the present invention is further explained:
Embodiment 1
A) pretreatment of raw material
Fennel fruit perfume material is crushed, sieving, makes the control of fennel particle size between 0.2~0.5mm.
B) the extraction of medicinal extract
Fennel powder, which is fitted into both ends, to be had in the stainless steel barrel of fine and close mesh, and then barrel is put into extraction kettle；
5 times of fennel powder quality (mL/g) of butane is imported into extraction kettle carries out subcritical abstraction；Extraction temperature is 30 DEG C, extraction pressure
Power is 0.2MPa, extraction time 20min.After the completion of extraction, extract liquor is imported in separating still, carries out (50 DEG C) of constant temperature decompressions
Precipitation, it is reusable after solvent recovery；Fennel seeds medicinal extract, yield of extract 10% are obtained after extract liquor precipitation.
C) volatile oil separates
Obtained fennel seeds medicinal extract is imported in distillation still, 1 times of water that medicinal extract quality is added is distilled, and vapo(u)rizing temperature is
80 DEG C, distillation time 90min, cooling recovered steam；After the completion of distillation, the liquid water-oil separating that recycling is obtained is separated
It is Fructus Foeniculi volatile oil to light phase, volatile oil yield is 1.6%.Wherein, the mass fraction of trans--isoesdragol is 70%.
After the completion of distillation, the medicinal extract remained in distillation still separation water removal is obtained into the fennel seeds fat oil without volatile oil, fat oil
Yield is 8%.Wherein, the mass fraction of petroselinic acid is 65%.
Embodiment 2
A) pretreatment of raw material
Fennel fruit perfume material is crushed, sieving, makes the control of fennel particle size between 0.2~0.5mm.
B) the extraction of medicinal extract
Fennel powder, which is fitted into both ends, to be had in the stainless steel barrel of fine and close mesh, and then barrel is put into extraction kettle；
8 times of fennel powder quality (mL/g) of butane is imported into extraction kettle carries out subcritical abstraction；Extraction temperature is 50 DEG C, extraction pressure
Power is 0.45MPa, extraction time 50min.After the completion of extraction, extract liquor is imported in separating still, constant temperature (60 DEG C) is carried out and subtracts
Pressure-off is molten, reusable after solvent recovery；Fennel seeds medicinal extract, yield of extract 15% are obtained after extract liquor precipitation.
C) volatile oil separates
Obtained fennel seeds medicinal extract is imported in distillation still, 2 times of water that medicinal extract quality is added are distilled, and vapo(u)rizing temperature is
90 DEG C, distillation time 150min, cooling recovered steam；After the completion of distillation, the liquid water-oil separating that recycling is obtained is separated
It is Fructus Foeniculi volatile oil to light phase, volatile oil yield is 2.1%.Wherein, the mass fraction of trans--isoesdragol is 80%.
After the completion of distillation, the medicinal extract remained in distillation still separation water removal is obtained into the fennel seeds fat oil without volatile oil, fat oil
Yield is 13.2%.Wherein, the mass fraction of petroselinic acid is 65%.
Embodiment 3
A) pretreatment of raw material
Fennel fruit perfume material is crushed, sieving, makes the control of fennel particle size between 0.2~0.5mm.
B) the extraction of medicinal extract
Fennel powder, which is fitted into both ends, to be had in the stainless steel barrel of fine and close mesh, and then barrel is put into extraction kettle；
6 times of fennel powder quality (mL/g) of butane is imported into extraction kettle carries out subcritical abstraction；Extraction temperature is 40 DEG C, extraction pressure
Power is 0.35MPa, extraction time 30min.After the completion of extraction, extract liquor is imported in separating still, constant temperature (55 DEG C) is carried out and subtracts
Pressure-off is molten, reusable after solvent recovery；Fennel seeds medicinal extract, yield of extract 13% are obtained after extract liquor precipitation.
C) volatile oil separates
Obtained fennel seeds medicinal extract is imported in distillation still, 1.5 times of water that medicinal extract quality is added are distilled, vapo(u)rizing temperature
It is 85 DEG C, distillation time 120min, cooling recovered steam；After the completion of distillation, the liquid water-oil separating that recycling is obtained, separation
Obtaining light phase is Fructus Foeniculi volatile oil, and volatile oil yield is 1.9%.Wherein, the mass fraction of trans--isoesdragol is
76%.After the completion of distillation, the medicinal extract remained in distillation still separation water removal is obtained into the fennel seeds fat oil without volatile oil, rouge
Fat oil yield is 12%.Wherein, the mass fraction of petroselinic acid is 65%.
Comparative example 1
A) pretreatment of raw material
Fennel fruit perfume material is crushed, sieving, makes the control of fennel particle size between 0.2~0.5mm.
B) the extraction of medicinal extract
Fennel powder, which is fitted into both ends, to be had in the stainless steel barrel of fine and close mesh, and then barrel is put into extraction kettle；
The n-hexane that fennel powder quality 10 times (mL/g) is imported into extraction kettle carries out heating extraction；Extraction temperature is 70 DEG C, extraction
Pressure is 0.1MPa, extraction time 120min.After the completion of extraction, extract liquor is imported in separating still, is carried out constant temperature (90 DEG C)
Precipitation is depressurized, it is reusable after solvent recovery；Fennel seeds medicinal extract, yield of extract 7% are obtained after extract liquor precipitation.
C) volatile oil separates
Obtained fennel seeds medicinal extract is imported in distillation still, 2 times of water that medicinal extract quality is added are distilled, and vapo(u)rizing temperature is
90 DEG C, distillation time 150min, cooling recovered steam；After the completion of distillation, the liquid water-oil separating that recycling is obtained is separated
It is Fructus Foeniculi volatile oil to light phase, volatile oil yield is 0.5%.Wherein, the mass fraction of trans--isoesdragol is 10%.
After the completion of distillation, the medicinal extract remained in distillation still separation water removal is obtained into the fennel seeds fat oil without volatile oil, fat oil
Yield is 7.0%.Wherein, the mass fraction of petroselinic acid is 60%.
As it can be seen that extracting fat oil with the prior art, the yield of medicinal extract will be substantially less than Examples 1 to 3, p < 0.05.And
And cannot be isolated from the medicinal extract volatile oil (in volatile oil effective component and Examples 1 to 3 there are significant difference, p <
0.05), and after separation volatile oil, the fat oil in medicinal extract is also by serious destruction.
Comparative example 2
A) pretreatment of raw material
Fennel fruit perfume material is crushed, sieving, makes the control of fennel particle size between 0.2~0.5mm.
B) volatile oil separates
Fennel powder is fitted into and is imported in distillation still, 8 times of water that medicinal extract quality is added are distilled, vapo(u)rizing temperature 110
DEG C, distillation time 240min, cooling recovered steam；After the completion of distillation, the liquid water-oil separating that recycling is obtained is isolated
Light phase is Fructus Foeniculi volatile oil, and volatile oil yield is 0.8%.Wherein, the relative amount of trans--isoesdragol is 50%.
C) the extraction of fat oil
By after the fennel seeds seed drying for extracting volatile oil, then barrel is put into extraction kettle；It is led into extraction kettle
Enter 8 times of fennel powder quality (mL/g) of butane and carries out subcritical abstraction；Extraction temperature is 50 DEG C, extracting pressure 0.45MPa,
Extraction time is 50min.After the completion of extraction, extract liquor is imported in separating still, carries out (60 DEG C) decompression precipitations of constant temperature, solvent returns
It is reusable after receipts；Fennel seeds medicinal extract, yield of extract 9% are obtained after extract liquor precipitation.Wherein, the quality of petroselinic acid
Score is 61%.
As it can be seen that extracting volatile oil with the prior art, the yield of volatile oil will be substantially less than Examples 1 to 3, p < 0.05.
Also, cannot isolating fat oil from the substance after the extraction volatile oil, (effective component in aliphatic oil is deposited with Examples 1 to 3
In significant difference, p < 0.05), and after separation volatile oil, the fat oil in medicinal extract is also by serious destruction.
The above is only the preferred embodiment of the present invention, it is noted that those skilled in the art are come
It says, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications also should be regarded as
Protection scope of the present invention.
Claims (9)
1. the extracting method of fennel seeds active constituent characterized by comprising
After fennel seeds seed is crushed, subcritical abstraction is carried out by extractant of butane, extract liquor is made fennel seeds through precipitation and soaks
Cream；
The fennel seeds medicinal extract is extracted with steam distillation, and it is Fructus Foeniculi volatile oil that vapor portion separates light phase after condensing；It mentions
Fennel seeds medicinal extract after taking is through dry obtained fennel seeds fat oil.
2. extracting method according to claim 1, which is characterized in that the fennel seeds seed be crushed to partial size be 0.2~
0.5mm。
3. extracting method according to claim 1, which is characterized in that the matter of fennel seeds seed and butane after the crushing
Amount-volume ratio is 5~8g/mL.
4. extracting method according to claim 1, which is characterized in that the temperature of the subcritical abstraction is 30~50 DEG C,
Extracting pressure is 0.2~0.45MPa, and extraction time is 20~50min.
5. extracting method according to claim 1, which is characterized in that the mode of the precipitation is that constant temperature depressurizes precipitation；Institute
The temperature for stating precipitation is 50~60 DEG C.
6. extracting method according to claim 1, which is characterized in that during the steam distillation is extracted, water with it is described small
The mass ratio of fennel medicinal extract is (1~2): 1.
7. extracting method according to claim 1, which is characterized in that the vapo(u)rizing temperature that the steam distillation is extracted is 80
~90 DEG C, distillation time is 90~150min.
8. Fructus Foeniculi volatile oil made from any one of claim 1~7 extracting method.
9. fennel seeds fat oil made from any one of claim 1~7 extracting method.
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Application publication date: 20181207 |
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| RJ01 | Rejection of invention patent application after publication |