CN108424817A - A kind of method of processing of Panax ginseng waste extraction ginseng essential oil - Google Patents

A kind of method of processing of Panax ginseng waste extraction ginseng essential oil Download PDF

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Publication number
CN108424817A
CN108424817A CN201810587846.8A CN201810587846A CN108424817A CN 108424817 A CN108424817 A CN 108424817A CN 201810587846 A CN201810587846 A CN 201810587846A CN 108424817 A CN108424817 A CN 108424817A
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ginseng
essential oil
panax
extraction
processing
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CN201810587846.8A
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赵凤云
姜永久
赵卉
唐贵才
贾清文
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Baishan Science & Technology Inst
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Baishan Science & Technology Inst
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Priority to CN201810587846.8A priority Critical patent/CN108424817A/en
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/025Recovery by solvent extraction
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/027Recovery 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)
  • Fats And Perfumes (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

The invention discloses a kind of methods that processing of Panax ginseng waste extracts ginseng essential oil, and volatile oil steams the technical issues of discharging, causing the significant wastage of resource with vapor during solving processing red ginseng, belongs to the technical field of ginseng essential oil extraction.Method includes collection, extraction, separation concentration, distillation and the refined step of distilled panax water, obtains refined ginseng essential oil.The present invention is collected using the by-product water steam during processing of Panax ginseng as object using condensing plant, and the means such as solvent extraction, separation, distillation are passed through, carry out the extraction of ginseng essential oil, turned waste into wealth with reaching, reduce the purpose of cost so that the precious resources are utilized to better.

Description

A kind of method of processing of Panax ginseng waste extraction ginseng essential oil
Technical field
The present invention relates to the technical fields of ginseng essential oil extraction more particularly to a kind of processing of Panax ginseng waste to extract panax ginseng extractum The method of oil.
Background technology
Ginseng is rare Chinese medicine, and medical value is higher, and the market price is also high, and it is (i.e. smart that complete stool contains volatile oil Oil), it is documented that ginseng essential oil has anti-inflammatory, calmness, decompression, antibechic, antifatigue, stimulating central nervous system, inhibits tumour Effect, the generation of the poly- enzyme of gucosamine in skin can be accelerated, have activation to skin regeneration.Ginseng essential oil has shield Skin health-care effect is used for cosmetics and skin care item, and the percutaneous osmosis of ginseng essential oil is absorbed by the body, hence into blood Liquid recycles and metabolism, promotes the development and nutrition of skin cell, increases skin gloss, has wrinkle resistant, cold-resistant and UV resistance The pharmacological action of beta radiation.
Current ginseng essential oil research carries out the extraction of volatile oil primarily directed to the root of ginseng, stem, leaf, flower and fruit Research, and is concentrated mainly on laboratory stage, as the extraction of Soxhlet extraction ether, the extraction of steam distillation ether, continuous backflow, The methods of supercritical ultrasonics technology, can not Instructing manufacture, and solvent ether used is product of keeping under strict control, and cannot carry out actual production and answer With.
Since volatile oil content is relatively low in ginseng, it is unrealistic and uneconomic to make raw material extraction volatile oil with ginseng. But ginseng, during making red ginseng, volatile oil is as vapor is carried over during steaming ginseng, and nearly 70% volatile oil is all It lost, all lost using this part by-product as waste material, very unfortunately.For example, Baishan has 2.5 ten thousand tons of fresh ginsengs every year It is processed into red ginseng, there are about 5000 tons for annual red ginseng yield, and volatile oil content is and most in 0.1%-0.5% or so in ginseng It concentrates in ginseng skin, volatile oil is steamed with vapor during processing red ginseng, is discharged, is caused the significant wastage of resource. Therefore, by this part, distilled water collects, and therefrom extracts volatile oil, improves value-added content of product, and it is ten to increase economic benefit Divide necessary.
Invention content
The present invention in view of the above technical problems, provides a kind of method of processing of Panax ginseng waste extraction ginseng essential oil, with people By-product water steam during participation work is object, is collected using condensing plant, passes through solvent extraction, separation, distillation Etc. means, carry out the extraction of ginseng essential oil, turned waste into wealth with reaching, reduce the purpose of cost.
To achieve the goals above, the present invention provides the following technical solutions:
A kind of method of processing of Panax ginseng waste extraction ginseng essential oil, includes the following steps:
(1) collection of distilled panax water:Vapor during steaming ginseng is collected using condensing unit, obtains distilled panax water;
(2) it extracts:By distilled panax water plus petroleum ether according to 1:1 volume ratio is extracted, and addition 10g/L inorganic salts carry out salt Analysis, extraction process need to stir;
(3) separation concentration:By the solution stand after extraction, detached after solution layering, upper layer is solvent layer, as Concentrate;Lower layer is water layer, and water layer carries out single extraction, separation concentration again;Merge concentrate twice;
(4) it distills:Concentrate is distilled, when efflux reaches 20 drops/timesharing, is considered as titration end-point, obtains coarse-fine Oil;
(5) it refines:Coarse-fine oil is evaporated under reduced pressure, when efflux reaches 5~10 drops/timesharing, is considered as distillation end point, obtains To refined ginseng essential oil.
Further, the specific method of the collection of step (1) described distilled panax water is:Condenser air inlet pipe is gone out with steaming ginseng cabinet Tracheae connects, and connects cooling water, when steaming ginseng cabinet pressure reaches steaming ginseng pressure, slowly opens outlet valve, carries out distilled panax water It collects, acquisition time is first 1.5~2.0 hours.
Further, the inorganic salts described in step (2) are sodium chloride.
Further, the solution stand time in step (3) after extraction is 4~8 hours.
Further, for step (4) when concentrate is distilled, magnet ring, which is added, prevents bumping.
Further, the temperature distilled in step (4) is controlled at 60 DEG C~85 DEG C.
Further, the pressure being evaporated under reduced pressure in step (5) is controlled in 0.03~0.05MPa.
Compared with prior art, beneficial effects of the present invention are:
The present invention is to pass through advanced rational extraction using the by-product distilled water generated during processing of Panax ginseng as object Technique recycles ginseng essential oil, achievees the purpose that waste recycles, reduces the processing cost of enterprise so that the precious resources To preferably utilize.Products obtained therefrom of the present invention is mainly used for clinical and cosmetic industry.Although ginseng essential oil is deep by cosmetics The favor of colleague, but be unattainable product, due to its expensive raw material price, the essential oil price of extraction is quite high, many Enterprise dare not set foot in, only by micro constitutent in the cosmetics of super quality.Implementation through the invention reduces being extracted into for product This, to also reduce the market price, will make its application range more wide.
Description of the drawings
In order to illustrate the technical solutions in the embodiments of the present application or in the prior art more clearly, below will be to institute in embodiment Attached drawing to be used is needed to be briefly described, it should be apparent that, the accompanying drawings in the following description is only one described in the present invention A little embodiments, for those of ordinary skill in the art, other drawings may also be obtained based on these drawings.
Fig. 1 is process flow chart provided in an embodiment of the present invention.
Specific implementation mode
In order to make those skilled in the art more fully understand technical scheme of the present invention, below in conjunction with attached drawing to this hair It is bright to be further detailed.
Embodiment 1
Shown in Figure 1, the method for processing of Panax ginseng waste extraction ginseng essential oil of the invention includes the following steps:
(1) collection of distilled panax water:Condenser air inlet pipe is connect with steaming ginseng cabinet escape pipe, cooling water is connected, works as steaming ginseng cabinet When pressure reaches steaming ginseng pressure, outlet valve is slowly opened, carries out the collection of distilled panax water, acquisition time is first 1.5 hours;
(2) it extracts:According to distilled panax water and petroleum ether volume ratio 1:1 ratio is extracted, add the sodium chloride of 10g/L into Row is saltoutd, and extraction process needs to stir;
(3) it concentrates:It by the solution stand 4 hours after extraction, is detached after layering, upper layer is solvent layer, is directly carried out Distillation;Lower layer is water layer, then carries out single extraction, separation, concentration, merges concentrate twice;
(4) it distills:Concentrate is distilled, magnet ring, which is added, prevents bumping, temperature from controlling at 60 DEG C, when efflux reaches 20 drops/timesharing, are considered as titration end-point, obtain coarse-fine oil;
(5) it refines:Coarse-fine oil is evaporated under reduced pressure, pressure control is in 0.03MPa, when efflux reaches 5 drops/timesharing, It is considered as distillation end point, obtains refined ginseng essential oil.Ginseng essential oil yield is 0.1%.
Embodiment 2
Shown in Figure 1, the method for processing of Panax ginseng waste extraction ginseng essential oil of the invention includes the following steps:
(1) collection of distilled panax water:Condenser air inlet pipe is connect with steaming ginseng cabinet escape pipe, cooling water is connected, works as steaming ginseng cabinet When pressure reaches steaming ginseng pressure, outlet valve is slowly opened, carries out the collection of distilled panax water, acquisition time is first 1.5 hours;
(2) it extracts:According to distilled panax water and petroleum ether volume ratio 1:1 ratio is extracted, add the sodium chloride of 10g/L into Row is saltoutd, and extraction process needs to stir;
(3) it concentrates:It by the solution stand 6 hours after extraction, is detached after layering, upper layer is solvent layer, is directly carried out Distillation;Lower layer is water layer, then carries out single extraction, separation, concentration, merges concentrate twice;
(4) it distills:Concentrate is distilled, magnet ring, which is added, prevents bumping, temperature from controlling at 75 DEG C, when efflux reaches 20 drops/timesharing, are considered as titration end-point, obtain coarse-fine oil;
(5) it refines:Coarse-fine oil is evaporated under reduced pressure, pressure control is in 0.04MPa, when efflux reaches 7 drops/timesharing, It is considered as distillation end point, obtains refined ginseng essential oil.Ginseng essential oil yield is 0.2%.
Embodiment 3
Shown in Figure 1, the method for processing of Panax ginseng waste extraction ginseng essential oil of the invention includes the following steps:
(1) collection of distilled panax water:Condenser air inlet pipe is connect with steaming ginseng cabinet escape pipe, cooling water is connected, works as steaming ginseng cabinet When pressure reaches steaming ginseng pressure, outlet valve is slowly opened, carries out the collection of distilled panax water, acquisition time is first 2.0 hours;
(2) it extracts:According to distilled panax water and petroleum ether volume ratio 1:1 ratio is extracted, add the sodium chloride of 10g/L into Row is saltoutd, and extraction process needs to stir;
(3) it concentrates:It by the solution stand 8 hours after extraction, is detached after layering, upper layer is solvent layer, is directly carried out Distillation;Lower layer is water layer, then carries out single extraction, separation, concentration, merges concentrate twice;
(4) it distills:Concentrate is distilled, magnet ring, which is added, prevents bumping, temperature from controlling at 85 DEG C, when efflux reaches 20 drops/timesharing, are considered as titration end-point, obtain coarse-fine oil;
(5) it refines:Coarse-fine oil is evaporated under reduced pressure, pressure control is in 0.05MPa, when efflux reaches 10 drops/timesharing, It is considered as distillation end point, obtains refined ginseng essential oil.Ginseng essential oil yield is 0.25%.
4 physical and chemical index of embodiment
Ginseng essential oil prepared by Example 1~3, is respectively detected its state, smell, index of refraction and proportion, examines Survey method is as follows:
(1) state:Sense organ measures
(2) smell:Sense organ measures
(3) index of refraction:It is detected using Abbe refractometer.
Specific method:1, prism cleans;2, water bath with thermostatic control is connected;3, correction refractometer reading;4, drop sample is on prism; 5, eyepiece is observed;6 read refraction index.
(4) proportion:The specific gravity bottle for taking clean, dry precision weighing, after filling sample, sets in 20 DEG C of water-baths and soaks 0.5 hour, So that the temperature of content is reached 20 DEG C, cover bottle cap, fine filtering paper slip is used in combination to suck the sample on branch pipe graticule, is taken after covering small cap Go out, will be dried, set in balance room 0.5 hour outside specific gravity bottle with filter paper, weighed.Sample is poured out again, specific gravity bottle is cleaned, fills Water is operated as above-mentioned from " set in 20 DEG C of water-baths and soak 0.5 hour " in accordance with the law below.There cannot be bubble in specific gravity bottle, in balance room Otherwise temperature cannot use this method no more than 20 DEG C.
Calculation formula:X=(m2-m0)/(m1-m0)
Wherein, X:The proportion of sample;
mo:The quality of specific gravity bottle, g;
m1:The quality of specific gravity bottle and water, g;
m2:The quality of specific gravity bottle and sample, g.
Testing result is shown in Table 1.
1 physical and chemical index testing result of table
5 chemical composition of embodiment detects
Separation determination is carried out to the volatile ingredient in ginseng essential oil using GC-MS methods.
Detection method is specially:It is diluted with petroleum ether dissolution ginseng essential oil and step by step, appropriate anhydrous sodium sulfate is added After water removal, upper machine is to be measured after crossing 0.22 μm of filter membrane.
GC test conditions:Chromatographic column is DB-5MS (0.25 μm of the μ ms of 30m × 250);Column temperature:Initial 50 DEG C, keep 2min Afterwards, 170 DEG C are warming up to the rate of 10 DEG C/min, keep 2min, then 280 DEG C are warming up to the rate of 8 DEG C/min, keeps 10min;250 DEG C of injector temperature;Carrier gas is high-purity helium, flow 1.0ml/min;1.0 μ L of sampling volume, input mode are point Flow into sample, split ratio 100:1.
MS test conditions:The source electron bombardment ion (EI);280 DEG C of ion source temperature;Electron energy 70eV;Transmission line temperature 280℃;Scanning quality ranging from 50~550amu of m/z.
It is analyzed the mass spectrum of component using NIST08.L library searchings, and artificial nucleus couple are carried out to whole results and are confirmed, Obtain final testing result.The ginseng essential oil that wherein prepared by Examples 1 to 3 plants volatile ingredient containing more than 30, and content is big In 3% ingredient as shown in table 2~4:
The measurement result of volatile ingredient in the ginseng essential oil of 2 embodiment 1 of table
The measurement result of volatile ingredient in the ginseng essential oil of 3 embodiment 2 of table
The measurement result of volatile ingredient in the ginseng essential oil of 4 embodiment 3 of table
Above certain exemplary embodiments that the present invention is only described by way of explanation, undoubtedly, for ability The those of ordinary skill in domain without departing from the spirit and scope of the present invention can be with a variety of different modes to institute The embodiment of description is modified.Therefore, above-mentioned attached drawing and description are regarded as illustrative in nature, and should not be construed as to the present invention The limitation of claims.

Claims (7)

1. a kind of method of processing of Panax ginseng waste extraction ginseng essential oil, which is characterized in that include the following steps:
(1) collection of distilled panax water:Vapor during steaming ginseng is collected using condensing unit, obtains distilled panax water;
(2) it extracts:By distilled panax water plus petroleum ether according to 1:1 volume ratio is extracted, and addition 10g/L inorganic salts are saltoutd, Extraction process needs to stir;
(3) separation concentration:By the solution stand after extraction, detached after solution layering, upper layer is solvent layer, is as concentrated Liquid;Lower layer is water layer, and water layer carries out single extraction, separation concentration again;Merge concentrate twice;
(4) it distills:Concentrate is distilled, when efflux reaches 20 drops/timesharing, is considered as titration end-point, obtains coarse-fine oil;
(5) it refines:Coarse-fine oil is evaporated under reduced pressure, when efflux reaches 5~10 drops/timesharing, is considered as distillation end point, obtains essence The ginseng essential oil of system.
2. the method for processing of Panax ginseng waste extraction ginseng essential oil as described in claim 1, which is characterized in that step (1) institute The specific method for stating the collection of distilled panax water is:Condenser air inlet pipe is connect with steaming ginseng cabinet escape pipe, connects cooling water, is joined when steaming When cabinet pressure reaches steaming ginseng pressure, outlet valve is slowly opened, carries out the collection of distilled panax water, acquisition time is preceding 1.5~2.0 small When.
3. the method for processing of Panax ginseng waste extraction ginseng essential oil as described in claim 1, which is characterized in that in step (2) The inorganic salts are sodium chloride.
4. the method for processing of Panax ginseng waste extraction ginseng essential oil as described in claim 1, which is characterized in that in step (3) The solution stand time after extraction is 4~8 hours.
5. the method for processing of Panax ginseng waste extraction ginseng essential oil as described in claim 1, which is characterized in that step (4) exists When concentrate is distilled, magnet ring, which is added, prevents bumping.
6. the method for processing of Panax ginseng waste extraction ginseng essential oil as described in claim 1, which is characterized in that in step (4) The temperature of distillation is controlled at 60 DEG C~85 DEG C.
7. the method for processing of Panax ginseng waste extraction ginseng essential oil as described in claim 1, which is characterized in that in step (5) The pressure of vacuum distillation is controlled in 0.03~0.05MPa.
CN201810587846.8A 2018-06-08 2018-06-08 A kind of method of processing of Panax ginseng waste extraction ginseng essential oil Pending CN108424817A (en)

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Cited By (5)

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CN110051782A (en) * 2019-05-22 2019-07-26 长春中医药大学 Ginseng extract and its preparation process
CN110684594A (en) * 2019-10-11 2020-01-14 吉林人参研究院(吉林省长白山天然药物研究院) A method for preparing Ginseng radix volatile oil from steamed ginseng distillate
CN111616225A (en) * 2020-06-22 2020-09-04 吉林大学 Steamed ginseng milk cap beverage and preparation method thereof
CN111676097A (en) * 2020-06-01 2020-09-18 蓝彤生物科技(吉林)有限公司 Extraction method of ginseng essential oil
CN112574821A (en) * 2020-12-02 2021-03-30 太极集团重庆涪陵制药厂有限公司 Traditional Chinese medicine volatile oil extraction equipment and extraction method

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110051782A (en) * 2019-05-22 2019-07-26 长春中医药大学 Ginseng extract and its preparation process
CN110684594A (en) * 2019-10-11 2020-01-14 吉林人参研究院(吉林省长白山天然药物研究院) A method for preparing Ginseng radix volatile oil from steamed ginseng distillate
CN111676097A (en) * 2020-06-01 2020-09-18 蓝彤生物科技(吉林)有限公司 Extraction method of ginseng essential oil
CN111616225A (en) * 2020-06-22 2020-09-04 吉林大学 Steamed ginseng milk cap beverage and preparation method thereof
CN112574821A (en) * 2020-12-02 2021-03-30 太极集团重庆涪陵制药厂有限公司 Traditional Chinese medicine volatile oil extraction equipment and extraction method
CN112574821B (en) * 2020-12-02 2023-05-09 太极集团重庆涪陵制药厂有限公司 Traditional Chinese medicine volatile oil extraction equipment and extraction method

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