CN110129124A - A kind of extracting method of geranium oil - Google Patents

A kind of extracting method of geranium oil Download PDF

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Publication number
CN110129124A
CN110129124A CN201910375126.XA CN201910375126A CN110129124A CN 110129124 A CN110129124 A CN 110129124A CN 201910375126 A CN201910375126 A CN 201910375126A CN 110129124 A CN110129124 A CN 110129124A
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geranium oil
stem
pelargonium roseum
leaf
added
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金岩
冯柏成
玄光善
董静静
路建强
王铁林
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Qingdao University of Science and Technology
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Qingdao University of Science and Technology
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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
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/02Pretreatment
    • C11B1/025Pretreatment by enzymes or microorganisms, living or dead
    • 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
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/02Pretreatment
    • C11B1/04Pretreatment of vegetable raw material
    • 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
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/10Production of fats or fatty oils from raw materials by extracting
    • C11B1/106Production of fats or fatty oils from raw materials by extracting using ultra-sounds

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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)
  • Biochemistry (AREA)
  • Microbiology (AREA)
  • Fats And Perfumes (AREA)

Abstract

The invention belongs to plant perfume extractive technique fields, and in particular to a kind of extracting method of geranium oil.A kind of extracting method of geranium oil provided by the present invention includes the following steps: the stem and leaf of (1) selection raw material Pelargonium roseum;(2) stem and leaf are broken into paste;(3) it digests;(4) yeast powder processing is added;(5) high-temperature process;(6) emulsifying homogeneous;(7) ultrasonication;(8) it is concentrated;(9) it distills.Geranium oil is extracted using method of the invention, it is a significant increase spiceleaf recovery rate, and method of the invention uses the mild mode of action of reaction condition, overcome environmental problem brought by traditional organic solvent extraction and avoid it is subsequent organic solvent is recycled or is handled brought by many and diverse process.

Description

A kind of extracting method of geranium oil
Technical field
The invention belongs to plant perfume extractive technique fields, and in particular to a kind of extracting method of geranium oil.
Background technique
Geranium oil is one of most important essential oil in global perfume industry, and fragrance is sweet and lasting stability, is often prepared The fragrance of flavoring rose essence is also commonly used for the essence such as rose, hyacinth, carnation, lilac, tuberose, the lily of the valley and violet and matches Fang Zhong.In recent years discovery geranium oil has stable medium curative effect to animal tumor, has apparent lethal effect to cancer cell in vitro. Its oral capsule and pill, suppository are clinically used for treatment cervical carcinoma and have a better effect.
The acquisition of geranium oil generally uses steam distillation, and this method mainly includes four processes, that is, the leaf that dries in the air, enter rice steamer, The duration and degree of heating, time.Bhaskaruni R etc. reports different cutting techniques to the rose pelargonium essential oil content for originating in India and changes The influence studied point.
Stone is with regard to equal ingredient using microwave irradiation induction extraction extraction Pelargonium roseum, by extraction conditions Research obtains preferred process, and the fresh Pelargonium roseum blade of 50 g uses ethyl alcohol and n-hexane extraction 40s at 648W respectively, Using residue filter, reduced pressure, geranium oil purification process after, it is normal that the recovery rate of Herba Pelargonii Graveolentis extract, which is 0 .7 %, 5 times of the lower n-hexane extraction recovery rate of temperature, and its fragrance is natural, compared with other extracting methods, microwave irradiation induction Extraction has the advantages that the time is short, recovery rate is high, operating cost is low etc..But chemical solvent is used in above method, hold It easily leads to organic solvent residual and there are certain safety problems.
Aqueous enzymatic extraction is to be destroyed cell wall structure in oil using enzymolysis, to grease be released, the party Method is mild, extraction process is simple, no solvent residue.
CN95112535.4 discloses a kind of geranium oil and its manufacturing method, it is characterized in that: by clean natural elm spiceleaf 2.5-6kg, peel garlic bulblet 1-4kg, octagonal 1-2kg, cloves 0.5-1.5kg, and after removing impurity, clear water is added in grinds 10kg is mixed thoroughly, is added vegetable oil 100kg and is mixed thoroughly, is then slowly introducing steaming bubble and is heated while stirring and reach 120-180 to temperature DEG C, it is filtered after natural cooling, filtrate is manufactured geranium oil finished product.
CN105505583A discloses a kind of method that subcritical normal butane fluid extracts geranium oil from spiceleaf, feature It is, includes the following steps: 1) to be crushed to 40~60 mesh, so first by the spiceleaf cleaned up drying to Han Shui Liang≤7wt% It is fitted into 200~300 mesh material bags that volume is 2~3L afterwards;2) start heat recirculated water system, preheat 55~60 DEG C of extractor, By described in step 1) be equipped with spiceleaf material bag put into extractor, it is closed, be evacuated to vacuum degree be 0.05~0.1MPa, discharge extraction Take air in tank;3) n-butane solvent is imported in extractor described in step 2) with plunger pump;4) start heat recirculated water system, It is extracted;5) separation then is evaporated under reduced pressure with diaphragm type compressor and vacuum pump linkage in knockout drum;6) merge step 5) Obtained geranium oil obtains final spiceleaf oil product through molecular distillation.
In above method, extraction efficiency is high, equipment manufacturing cost is low, feed throughput is big, process flow is simple, is produced into This is low, and whole process carries out under low temperature, anaerobic state, extracts, separate while carrying out, and extraction rate is fastly, it can be achieved that solvent Recycling.But which employs n-butane solvents
Jinsong ZHANG of Yunnan Prov Agriculture University et al. is " with external source enzymatic treatment Pelargonium roseum cauline leaf to extraction of essential oil rate and fragrance Influence " it discloses in a text, various carbohydrases are contained using Novi letter ViscozymeL(, including pectase, araban Combizym including enzyme, cellulase, dextranase, hemicellulase and zytase) it is 3.3-5 in pH and temperature is It under conditions of 40-50 DEG C, digests, in A sample, pure water is added, water-bath heats steam oil with electric jacket after drying;In B sample, it is added Enzyme dilution water-bath 2 hours, heats steam oil with electric jacket after drying;In C sample, enzyme dilution is added, is placed at room temperature for 24 hours, Steam oil is heated with electric jacket after drying;It was found that processed extraction of essential oil rate has been respectively increased 45% than untreated in B and C sample With 75%, the chemical component ratio of essential oil is also changed.Fragrance becomes more sweet tea, more rose rhythms, few soap gas, and lasting is more longlasting.
The recovery rate for how further improving geranium oil needs further progress research and explores.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of works that can significantly improve geranium oil recovery rate Skill.
The feature of a kind of extracting method of geranium oil, this method maximum is to digest the stem of raw material Pelargonium roseum and leaf, Add yeast powder processing.
Specifically, above-mentioned method includes the following steps: the stem and leaf of (1) selection raw material Pelargonium roseum;(2) by stem Paste is broken into leaf;(3) it digests;(4) yeast powder processing is added;(5) high-temperature process;(6) emulsifying homogeneous;(7) ultrasonication; (8) it is concentrated;(9) it distills.
This method includes the following steps:
(1) in 4 annual~October, the stem and leaf of Pelargonium roseum is taken, cleans and dries, then by the stem of Pelargonium roseum It is cut into section, the leaf of Pelargonium roseum is cut into area no more than 4cm2Small pieces;
(2) the Pelargonium roseum leaf of the Pelargonium roseum stem of the section shape in (1) and strip is added to the water, Pelargonium roseum stem Solid and liquid weight ratio with Pelargonium roseum Ye Yushui is 1:2~4, is broken into paste;
(3) temperature of pasty material is adjusted to 45~55 DEG C, cellulase is added in material, and additional amount is that pasty material is total The 0.2~0.5% of weight digests 20~40 minutes, 8~10min of destroy the enzyme treatment at 95 DEG C;
(4) saccharomycete powder is added in the enzymolysis liquid in (3), additional amount is the 0.2~0.4% of enzymolysis liquid weight;In 35~40 15~20min is kept at DEG C;
(5) raw material in (4) is placed in 10~20min of holding at 100 DEG C;
(6) material in (5) is placed in 5 ~ 15min of processing in emulsifying homogeneous machine;
(7) material in (5) is cooled to 45~55 DEG C, 15~20min of ultrasonication;
(8) material in (7) is concentrated into the 1/3 of its original volume, obtains concentrate;
(9) concentrate is heated under conditions of 240~260 DEG C to distillation under vacuum state, obtains geranium oil.
(6) condition of emulsifying homogeneous is in: 2000~2400 r of revolving speed/min;Temperature is 35~45 DEG C.
The condition of ultrasonication is that frequency is 60~80kHz.
Saccharomycete powder is purchased from Angel Yeast Co., Ltd.
(9) vacuum condition are as follows: 0.24~0.5 kPa.
Preferably, the extracting method of above-mentioned a kind of geranium oil, includes the following steps:
(1) in 4 annual~October, the stem and leaf of Pelargonium roseum is taken, cleans and dries, then by the stem of Pelargonium roseum It is cut into section, it is 1~4cm that the leaf of Pelargonium roseum, which is cut into area,2Small pieces;
(2) the Pelargonium roseum leaf of the Pelargonium roseum stem of the section shape in (1) and strip is added to the water, Pelargonium roseum stem Solid and liquid weight ratio with Pelargonium roseum Ye Yushui is 1:3, is broken into paste;
(3) temperature of pasty material is adjusted to 50 DEG C, cellulase is added in material, and additional amount is pasty material total weight 0.3%, digest 30 minutes, the destroy the enzyme treatment 9min at 95 DEG C;
(4) saccharomycete powder is added in the enzymolysis liquid in (3), additional amount is the 0.3% of enzymolysis liquid weight;It is kept at 40 DEG C 20min;
(5) raw material in (4) is placed at 100 DEG C and keeps 15min;
(6) material in (5) is placed in emulsifying homogeneous machine and handles 10min;2200 r of revolving speed/min;Temperature is 40 DEG C;
(7) material in (5) is cooled to 50 DEG C, ultrasonication 15min, frequency 70kHz
(8) material in (7) is concentrated into the 1/3 of its original volume, obtains concentrate;
(9) concentrate is heated under conditions of 250 DEG C to distillation under vacuum state, obtains geranium oil;Vacuum condition are as follows: 0.3 kPa。
As an improvement of the present invention, further include (10), active carbon or carclazyte are added in the geranium oil in (9), adds Heat is stirred to 50~60 DEG C with the revolving speed of 20~40r/min, and filtering obtains geranium oil.
Specifically, active carbon or carclazyte are added in the geranium oil in (9), 55 DEG C are heated to, with 30r/min in (10) Revolving speed stirring, filtering, obtain geranium oil.
In the present invention, raw material is first broken into paste, then use the technique of water phase enzyme pretreatment, using water as dispersed phase, enzyme It is hydrolyzed in this water phase, makes grease be easy to escape from oil plant solids, using the good hydrophily of solids, make Solids are scattered in water phase and separate with grease.After broken material is added in enzyme, material natural enzymolysis can be promoted.
In background technique " with influence of the external source enzymatic treatment Pelargonium roseum cauline leaf to extraction of essential oil rate and fragrance " in a text Various carbohydrases are contained using Novi letter ViscozymeL(, including pectase, arabanase, cellulase, glucan Combizym including enzyme, hemicellulase and zytase) enzymatic hydrolysis, heats steam oil with electric jacket, can obtain spiceleaf essential oil.
But the inventors discovered that, using single cellulase, it is aided with yeast treatment technology, can similarly reaches and obtain Obtain the purpose of geranium oil.Also, the present inventor has carried out a large amount of experiment, in various comparisons to verify the effect of complex enzyme It was found that, the solution of the present invention be better than compound enzyme effect, and in general complex enzyme be better than using its effect it is single Enzyme, present invention conclusion obtained is exactly the opposite, the function and effect of complex enzyme can be reached using single enzyme, the present inventor pushes away It surveys, it may be possible to because of its in effect of other enzymes in hydrolysis in complex enzyme and the raw material in the little or present invention The content of its substance is considerably less, and the enzyme of other types is caused to add either to be not added and all influence on whole hydrolysis effect and little.
The effect of saccharomycete was to take off bitter and deodorant to enzymolysis liquid, but in the present invention, ferment is added inventors have found that working as originally After female bacterium, saccharomycete acts on the fractions in enzymolysis liquid, so that later period oil yield significantly increases.Inventor analyzes former Cause, it may be possible to saccharomycete (although phenomenon of the present inventor without the method interpretation mystery, pass through the experiment in specific embodiment, The present inventor shows this phenomenon), it is above during the experiment to be the discovery that unexpected effect, art technology Personnel are anyway also unimaginable to use saccharomycete to improve the oil yield of geranium oil.
The beneficial effects of the present invention are extract geranium oil using method of the invention, increase perfume (or spice) significantly Leaf recovery rate, and method of the invention uses the mild mode of action of reaction condition, overcomes traditional organic solvent and mentions Environmental problem brought by following the example of and avoid it is subsequent organic solvent is recycled or is handled brought by many and diverse process.
Detailed description of the invention
Fig. 1 is the liquid chromatogram of the geranium oil in the embodiment of the present invention 1.
Specific embodiment
In order to make those skilled in the art better understand the present invention, the present invention is carried out now in conjunction with specific embodiment It is further to illustrate.
Embodiment 1
(1) in June, the stem and leaf of Pelargonium roseum is taken, cleans and dries, the stem of Pelargonium roseum is then cut into section, it will It is 1~4cm that the leaf of Pelargonium roseum, which is cut into area,2Small pieces;
(2) the Pelargonium roseum leaf of the Pelargonium roseum stem of the section shape in (1) and strip is added to the water, Pelargonium roseum stem Solid and liquid weight ratio with Pelargonium roseum Ye Yushui is 1:3, is broken into paste;
(3) temperature of pasty material is adjusted to 50 DEG C, cellulase is added in material, and additional amount is pasty material total weight 0.3%, digest 30 minutes, the destroy the enzyme treatment 9min at 95 DEG C;
(4) saccharomycete powder is added in the enzymolysis liquid in (3), additional amount is the 0.3% of enzymolysis liquid weight;It is kept at 40 DEG C 20min;
(5) raw material in (4) is placed at 100 DEG C and keeps 15min;
(6) material in (5) is placed in emulsifying homogeneous machine and handles 10min;Revolving speed 2200r/min;Temperature is 40 DEG C;
(7) material in (5) is cooled to 50 DEG C, ultrasonication 15min, frequency 70kHz
(8) material in (7) is concentrated into the 1/3 of its original volume, obtains concentrate;
(9) concentrate is heated to distillation, vacuum condition under vacuum state under conditions of 250 DEG C are as follows: 0.3 kPa is obtained fragrant Leaf oil.
Attached drawing 1 is the gas chromatogram of the fatty acid composition measuring in the geranium oil in embodiment 1, in the map, chromatography Column: HP-5 fused-silica capillary column (30m × 0.25mm × 0.25 μm);Carrier gas: nitrogen;Flow velocity 1.5mL/min;Constant current mould Formula: 230 DEG C of injector temperature;Split ratio 10:1;Column temperature: it 75 DEG C of initial temperature, is kept for 4 minutes, is heated up with the speed of 5 DEG C/min To 200 DEG C, detector temperature is 250 DEG C.
From figure 1 it appears that citronellol, formic acid citronellol, geraniol and geranyl formate, rose oxide in geranium oil It is main component therein with linalool, linalool oxide;
The recovery rate (%) of geranium oil=geranium oil actual extracting quality/spiceleaf stem and leaf raw material oil content × 100%;
Through detecting, the oil content in leaf used in Example 1 and stem (stem) is 0.198%;
Total weight × 100% of spiceleaf stem and oil content × leaf and stem (stem) in leaf raw material oil content=leaf and stem (stem).
Embodiment 2
On the basis of embodiment 1, continue step (10), active carbon is added in the geranium oil in (9), is heated to 55 DEG C, with The revolving speed of 30r/min stirs, and filtering obtains geranium oil.
Embodiment 3
(1) in May, the stem and leaf of Pelargonium roseum is taken, cleans and dries, the stem of Pelargonium roseum is then cut into section, it will It is 1~4cm that the leaf of Pelargonium roseum, which is cut into area,2Small pieces;
(2) the Pelargonium roseum leaf of the Pelargonium roseum stem of the section shape in (1) and strip is added to the water, Pelargonium roseum stem Solid and liquid weight ratio with Pelargonium roseum Ye Yushui is 1:2, is broken into paste;
(3) temperature of pasty material is adjusted to 55 DEG C, cellulase is added in material, and additional amount is pasty material total weight 0.2%, digest 40 minutes, the destroy the enzyme treatment 9min at 95 DEG C;
(4) saccharomycete powder is added in the enzymolysis liquid in (3), additional amount is the 0.2% of enzymolysis liquid weight, is kept at 40 DEG C 20min;
(5) raw material in (4) is placed at 100 DEG C and keeps 15min;
(6) material in (5) is placed in emulsifying homogeneous machine and handles 8min;2400 r of revolving speed/min;Temperature is 40 DEG C;
(7) material in (5) is cooled to 50 DEG C, ultrasonication 15min, frequency 70kHz
(8) material in (7) is concentrated into the 1/3 of its original volume, obtains concentrate;
(9) concentrate is heated under conditions of 240 DEG C or so to distillation, vacuum condition are as follows: 0.3 kPa is obtained under vacuum state Obtain geranium oil.
Embodiment 4
(1) in annual July, the stem and leaf of Pelargonium roseum is taken, cleans and dries, is then cut into the stem of Pelargonium roseum Section, it is 1~4cm that the leaf of Pelargonium roseum, which is cut into area,2Small pieces;
(2) the Pelargonium roseum leaf of the Pelargonium roseum stem of the section shape in (1) and strip is added to the water, Pelargonium roseum stem Solid and liquid weight ratio with Pelargonium roseum Ye Yushui is 1:4, is broken into paste;
(3) temperature of pasty material is adjusted to 45 DEG C, cellulase is added in material, and additional amount is pasty material total weight 0.4%, digest 40 minutes, the destroy the enzyme treatment 9min at 95 DEG C;
(4) saccharomycete powder is added in the enzymolysis liquid in (3), additional amount is the 0.4% of enzymolysis liquid weight;It is kept at 40 DEG C 40min;
(5) raw material in (4) is placed at 100 DEG C and keeps 15min;
(6) material in (5) is placed in emulsifying homogeneous machine and handles 5min;2400 r of revolving speed/min;Temperature is 40 DEG C;
(7) material in (5) is cooled to 50 DEG C, ultrasonication 15min, frequency 70kHz
(8) material in (7) is concentrated into the 1/3 of its original volume, obtains concentrate;
(9) concentrate is heated to distillation, vacuum condition under vacuum state under conditions of 250 DEG C are as follows: 0.3 kPa is obtained fragrant Leaf oil.
Embodiment 5
(1) in annual August part, the stem and leaf of Pelargonium roseum is taken, cleans and dries, is then cut into the stem of Pelargonium roseum Section, it is 1~4cm that the leaf of Pelargonium roseum, which is cut into area,2Small pieces;
(2) the Pelargonium roseum leaf of the Pelargonium roseum stem of the section shape in (1) and strip is added to the water, Pelargonium roseum stem Solid and liquid weight ratio with Pelargonium roseum Ye Yushui is 1:3, is broken into paste;
(3) temperature of pasty material is adjusted to 48 DEG C, cellulase is added in material, and additional amount is pasty material total weight 0.25%, digest 25 minutes, the destroy the enzyme treatment 6min at 95 DEG C;
(4) saccharomycete powder is added in the enzymolysis liquid in (3), additional amount is the 0.3% of enzymolysis liquid weight;It is kept at 35 DEG C 15min;
(5) raw material in (4) is placed at 100 DEG C and keeps 15min;
(6) material in (5) is placed in emulsifying homogeneous machine and handles 10min;2200 r of revolving speed/min;Temperature is 40 DEG C;
(7) material in (5) is cooled to 50 DEG C, ultrasonication 15min, frequency 70kHz
(8) material in (7) is concentrated into the 1/3 of its original volume, obtains concentrate;
(9) concentrate is heated to distillation, vacuum condition under vacuum state under conditions of 250 DEG C are as follows: 0.3 kPa is obtained fragrant Leaf oil;
Comparative example 1
It is with the difference of embodiment 1, is not handled using yeast in comparative example 1;Remaining step is same as Example 1, specific to walk It is rapid as follows:
(1) in June, the stem and leaf of Pelargonium roseum is taken, cleans and dries, the stem of Pelargonium roseum is then cut into section, it will It is 1~4cm that the leaf of Pelargonium roseum, which is cut into area,2Small pieces;
(2) the Pelargonium roseum leaf of the Pelargonium roseum stem of the section shape in (1) and strip is added to the water, Pelargonium roseum stem Solid and liquid weight ratio with Pelargonium roseum Ye Yushui is 1:3, is broken into paste;
(3) temperature of pasty material is adjusted to 50 DEG C, cellulase is added in material, and additional amount is pasty material total weight 0.3%, digest 30 minutes, the destroy the enzyme treatment 9min at 95 DEG C, obtain enzymolysis liquid;
(4) enzymolysis liquid in (3) is placed at 100 DEG C and keeps 15min;
(5) material in (4) is placed in emulsifying homogeneous machine and handles 10min;2200 r of revolving speed/min;Temperature is 40 DEG C;
(6) material in (5) is cooled to 50 DEG C, ultrasonication 15min, frequency 70kHz
(7) material in (6) is concentrated into the 1/3 of its original volume, obtains concentrate;
(8) concentrate is heated to distillation, vacuum condition under vacuum state under conditions of 250 DEG C are as follows: 0.3 kPa is obtained fragrant Leaf oil.
Comparative example 2
Compared with Example 1, plain enzymatic treatment without added fiber in comparative example 2, is handled only with yeast;, the specific steps are as follows:
(1) in June, the stem and leaf of Pelargonium roseum is taken, cleans and dries, the stem of Pelargonium roseum is then cut into section, it will It is 1~4cm that the leaf of Pelargonium roseum, which is cut into area,2Small pieces;
(2) the Pelargonium roseum leaf of the Pelargonium roseum stem of the section shape in (1) and strip is added to the water, Pelargonium roseum stem Solid and liquid weight ratio with Pelargonium roseum Ye Yushui is 1:3, is broken into paste;
(3) temperature of pasty material is adjusted to 40 DEG C, saccharomycete powder is added, and additional amount is the 0.3% of pasty material weight;In 20min is kept at 40 DEG C;
(4) raw material in (3) is placed at 100 DEG C and keeps 15min;
(5) material in (4) is placed in emulsifying homogeneous machine and handles 10min;2200 r of revolving speed/min;Temperature is 40 DEG C;
(6) material in (5) is cooled to 50 DEG C, ultrasonication 15min, frequency 70kHz
(7) material in (6) is concentrated into the 1/3 of its original volume, obtains concentrate;
(8) concentrate is heated to distillation, vacuum condition under vacuum state under conditions of 250 DEG C are as follows: 0.3 kPa is obtained fragrant Leaf oil.
Comparative example 3
In comparative example 3, joined cellulase and both compound enzymatic treatments of pectase, remaining the step of it is complete with embodiment 1 It is identical, the specific steps are as follows:
(1) in June, the stem and leaf of Pelargonium roseum is taken, cleans and dries, the stem of Pelargonium roseum is then cut into section, it will It is 1~4cm that the leaf of Pelargonium roseum, which is cut into area,2Small pieces;
(2) the Pelargonium roseum leaf of the Pelargonium roseum stem of the section shape in (1) and strip is added to the water, Pelargonium roseum stem Solid and liquid weight ratio with Pelargonium roseum Ye Yushui is 1:3, is broken into paste;
(3) temperature of pasty material is adjusted to 50 DEG C, and cellulase and pectase, cellulase and pectase are added in material Additional amount be the 0.3% of pasty material total weight, the weight ratios of two kinds of enzyme powders is 1:1, is digested 30 minutes, the enzyme deactivation at 95 DEG C Handle 9min;
(4) saccharomycete powder is added in the enzymolysis liquid in (3), additional amount is the 0.3% of enzymolysis liquid weight;It is kept at 40 DEG C 20min;
(5) raw material in (4) is placed at 100 DEG C and keeps 15min;
(6) material in (5) is placed in emulsifying homogeneous machine and handles 10min;2200 r of revolving speed/min;Temperature is 40 DEG C;
(7) material in (6) is cooled to 50 DEG C, ultrasonication 15min, frequency 70kHz
(8) material in (7) is concentrated into the 1/3 of its original volume, obtains concentrate;
(9) concentrate is heated to distillation, vacuum condition under vacuum state under conditions of 250 DEG C are as follows: 0.3 kPa is obtained fragrant Leaf oil.
Comparative example 4
It is with the difference of comparative example 3, yeast processing is not added in comparative example 4, remaining step is identical as comparative example 1, specific to walk It is rapid as follows:
(1) in June, the stem and leaf of Pelargonium roseum is taken, cleans and dries, the stem of Pelargonium roseum is then cut into section, it will It is 1~4cm that the leaf of Pelargonium roseum, which is cut into area,2Small pieces;
(2) the Pelargonium roseum leaf of the Pelargonium roseum stem of the section shape in (1) and strip is added to the water, Pelargonium roseum stem Solid and liquid weight ratio with Pelargonium roseum Ye Yushui is 1:3, is broken into paste;
(3) temperature of pasty material is adjusted to 50 DEG C, and cellulase and pectase, cellulase and pectase are added in material Additional amount be the 0.3% of pasty material total weight, the weight ratios of two kinds of enzyme powders is 1:1, is digested 30 minutes, the enzyme deactivation at 95 DEG C Handle 9min;
(4) raw material in (3) is placed at 100 DEG C and keeps 15min;
(5) material in (4) is placed in emulsifying homogeneous machine and handles 10min;Revolving speed 2200r/min;Temperature is 40 DEG C;
(6) material in (5) is cooled to 50 DEG C, ultrasonication 15min, frequency 70kHz
(7) material in (6) is concentrated into the 1/3 of its original volume, obtains concentrate;
(8) concentrate is heated to distillation, vacuum condition under vacuum state under conditions of 250 DEG C are as follows: 0.3 kPa is obtained fragrant Leaf oil.
Comparative example 5
It is with the difference of embodiment 1, without emulsifying homogeneous machine processing after (5), is directly entered ultrasonic treatment, remaining step and reality It is identical to apply example 1.
Comparative example 6
It is with the difference of embodiment 1, it is not sonicated after (6), it is directly entered (8) concentration step;Remaining step and implementation Example 1 is identical.
Comparative example 7
It is with the difference of comparative example 3, the enzyme used is cellulase and hemicellulase, the dosage and ratio of the two and comparison Example 3 is identical.
Comparative example 8
It is with the difference of comparative example 3, for the enzyme used for cellulase and dextranase, the dosage and comparative example 3 of the two are complete It is identical.
Comparative example 9
It is with the difference of embodiment 1, the enzyme used is hemicellulase, the use of the cellulase in dosage and embodiment 1 Equivalent is measured, remaining is identical with embodiment 1.
Comparative example 10
It is with the difference of comparative example 3, for the enzyme used for cellulase and hemicellulase, the dosage and ratio of the two are comparisons 2 times of two kinds of compound enzyme dosages in example 3, remaining is identical with comparative example 3.
Comparative example 11
In the present invention, using the method for solvent extraction, specific method is as follows:
By be cut into section respectively with the spiceleaf stem of batch and spiceleaf in embodiment 1 and be cut into area be 1~4cm2Small pieces;Then It is mixed by the two plus with the water of 1:1, is broken into paste, add the extraction of organic solvent methanol, Extracting temperature is 35 DEG C, then uses stone Oily ether continues to extract;Solid-liquid ratio is 10:1;Distillation obtains geranium oil.The method uses two kinds of organic solvents to extract, and mentions Take rate or Africa high, if a kind of solvent extraction.The present inventor did a kind of experiment that organic solvent extracts, Recovery rate is low compared with comparative example 11, so the present inventor compares comparison object using a kind of conduct that recovery rate is high, more there is persuasion Power and comparative.
About the recovery rate of the geranium oil in embodiment 1-5 and comparative example 1-8, it is computed, as a result as follows:
The recovery rate (%) of the geranium oil obtained in 1 embodiment of table and comparative example
It can be seen that in comparative example 1 from the data in above table, yeast processing be not added, the recovery rate of geranium oil is only 75.73%, relative to embodiment 1-5, have dropped nearly 10 percentage point, for the extraction of geranium oil, 10 percentage points Improve it is hard-earned, and be not added yeast processing, for the extraction of geranium oil, influence be it is bigger, this illustrates yeast Important effect is played during extracting geranium oil, specific to act on, inventor's analysis may be that saccharomycete has Specifically there is decomposition or suction-operated to the Cucumber in spiceleaf enzymolysis liquid, be conducive to the extraction of subsequent geranium oil;
Plain enzymatic treatment without added fiber in comparative example 2, the effect extracted is very poor, from this, enzyme especially cellulose Enzymatic treatment has made biggish contribution in the extraction of geranium oil;
Cellulase and two kinds of compound enzymatic treatments of pectase are added in comparative example 3, use cellulase and half fiber in comparative example 7 Cellulase and dextranase are used in the plain enzyme of dimension, comparative example 8, the effect of geranium oil is extracted after the hydrolysis of these types of complex enzyme Instead not as good as being only added the effect extracted after a kind of this enzymatic treatment of cellulase in embodiment 1, this explanation, the addition of complex enzyme, Its effect is not fully better than single enzyme hydrolysis.Analyze reason, it may be possible to which the pH of enzymatic hydrolysis either temperature is not most suitable for Two kinds of enzymes enzyme simultaneously, or be possible to two kinds of enzymes play the role of in effect it is a kind of mutually inhibit, make so as to cause two kinds of enzymes With its effect and not as good as a kind of effect of single enzyme hydrolysis;
Comparative example 4 joined two kinds of enzymatic treatments compared with comparative example 3, but yeast processing is not added, and recovery rate is still relatively real It applies example 1 and wants much lower, even if this, which has further been confirmed, is added two kinds of enzymatic treatments, yeast processing is not added, recovery rate can be by To large effect, it is seen that yeast act on extraction during played the role of being bigger.
Homogenization is not used in comparative example 5, the recovery rate of geranium oil also will receive certain influence, and analysis may be cream Change " cavitation " processing of homogenization combination ultrasonic wave, so that geranium oil is easier dissolution subsequent to be extracted.
Ultrasonication is not used in comparative example 6, is influenced also than more significant, its recovery rate significantly drops compared with embodiment 1 It is low.
In comparative example 9, the type of enzyme is changed, the cellulase in embodiment 1 is replaced with into hemicellulase, it is acquired Geranium oil recovery rate be 75.97%, it is seen then that its extraction effect of cellulase employed in the present invention is better than hemicellulose Enzyme.
In comparative example 10, the dosage of the complex enzyme used is 2 times in comparative example 3, this has just reached and other implementations The effect that example is close, but its cost greatly increases;
It in comparative example 11, is extracted using the method for solvent, action condition is than stronger, the recovery rate and embodiment of geranium oil Substantially quite.But during solvent extraction, a large amount of solvent is used.
It can be seen that method of the invention from above data and extract geranium oil, effect is best.If changing it One of enzyme either by cellulase of the invention replace with complex enzyme composed by two kinds of enzymes (be detailed in comparative example 3,7, 8), the recovery rate of geranium oil is low instead.
Also, yeast plays unexpected technical effect in extraction of the invention, this is to enable the present inventor very frightened It is odd and unexpected;In addition present invention employs ultrasonications and emulsifying homogeneous to handle, and being for extracting has biggish promotion to make With.
Method action condition of the invention is mild, and compared with the solvent extraction in comparative example 10, the recovery rate of the two is differed And less, but method of the invention is because of action condition mildly and need not handle subsequent chemical solvent, environmentally friendly, Thus have more certain progressive.

Claims (10)

1. a kind of extracting method of geranium oil, it is characterised in that: digest the stem of raw material Pelargonium roseum and leaf, add yeast Powder processing.
2. a kind of extracting method of geranium oil as described in claim 1, it is characterised in that: this method includes the following steps: (1) stem and leaf of raw material Pelargonium roseum are selected;(2) stem and leaf are broken into paste;(3) it digests;(4) yeast powder processing is added; (5) high-temperature process;(6) emulsifying homogeneous;(7) ultrasonication;(8) it is concentrated;(9) it distills.
3. a kind of extracting method of geranium oil as described in claim 1, it is characterised in that: this method includes the following steps:
(1) in 4 annual~October, the stem and leaf of Pelargonium roseum is taken, cleans and dries, then by the stem of Pelargonium roseum It is cut into section, the leaf of Pelargonium roseum is cut into area no more than 4cm2Small pieces;
(2) the Pelargonium roseum leaf of the Pelargonium roseum stem of the section shape in (1) and strip is added to the water, Pelargonium roseum stem Solid and liquid weight ratio with Pelargonium roseum Ye Yushui is 1:2~4, is broken into paste;
(3) temperature of pasty material is adjusted to 45~55 DEG C, cellulase is added in material, and additional amount is that pasty material is total The 0.2~0.5% of weight digests 20~40 minutes, 8~10min of destroy the enzyme treatment at 95 DEG C;
(4) saccharomycete powder is added in the enzymolysis liquid in (3), additional amount is the 0.2~0.4% of enzymolysis liquid weight;In 35~40 15~20min is kept at DEG C;
(5) raw material in (4) is placed in 10~20min of holding at 100 DEG C;
(6) material in (5) is placed in 5 ~ 15min of processing in emulsifying homogeneous machine;
(7) material in (5) is cooled to 45~55 DEG C, 15~20min of ultrasonication;
(8) material in (7) is concentrated into the 1/3 of its original volume, obtains concentrate;
(9) concentrate is heated under conditions of 240~260 DEG C to distillation under vacuum state, obtains geranium oil.
4. a kind of extracting method of geranium oil as described in claim 1, it is characterised in that: (6) condition of emulsifying homogeneous is in: 2000~2400 r of revolving speed/min;Temperature is 35~45 DEG C.
5. a kind of extracting method of geranium oil as described in claim 1, it is characterised in that: the condition of ultrasonication is frequency Rate is 60~80kHz.
6. a kind of extracting method of geranium oil as described in claim 1, it is characterised in that: saccharomycete powder is purchased from Angel Yeast Limited liability company.
7. a kind of extracting method of geranium oil as described in claim 1, it is characterised in that: (9) vacuum condition are as follows: 0.24~ 0.5 kPa。
8. a kind of extracting method of geranium oil as described in claim 1, includes the following steps:
(1) in 4 annual~October, the stem and leaf of Pelargonium roseum is taken, cleans and dries, then by the stem of Pelargonium roseum It is cut into section, it is 1~4cm that the leaf of Pelargonium roseum, which is cut into area,2Small pieces;
(2) the Pelargonium roseum leaf of the Pelargonium roseum stem of the section shape in (1) and strip is added to the water, Pelargonium roseum stem Solid and liquid weight ratio with Pelargonium roseum Ye Yushui is 1:3, is broken into paste;
(3) temperature of pasty material is adjusted to 50 DEG C, cellulase is added in material, and additional amount is pasty material total weight 0.3%, digest 30 minutes, the destroy the enzyme treatment 9min at 95 DEG C;
(4) saccharomycete powder is added in the enzymolysis liquid in (3), additional amount is the 0.3% of enzymolysis liquid weight;It is kept at 40 DEG C 20min;
(5) raw material in (4) is placed at 100 DEG C and keeps 15min;
(6) material in (5) is placed in emulsifying homogeneous machine and handles 10min;2200 r of revolving speed/min;Temperature is 40 DEG C;
(7) material in (5) is cooled to 50 DEG C, ultrasonication 15min, frequency 70kHz
(8) material in (7) is concentrated into the 1/3 of its original volume, obtains concentrate;
(9) concentrate is heated under conditions of 250 DEG C to distillation under vacuum state, obtains geranium oil;Vacuum condition are as follows: 0.3 kPa。
9. a kind of extracting method of geranium oil as described in claim 3 or 8, it is characterised in that: further include (10), in (9) Geranium oil in active carbon or carclazyte is added, be heated to 50~60 DEG C, stirred with the revolving speed of 20~40r/min, filtering obtains fragrant Leaf oil.
10. a kind of extracting method of geranium oil as described in claim 3 or 8, it is characterised in that: further include (10), in (9) Geranium oil in active carbon or carclazyte is added, be heated to 55 DEG C, stirred with the revolving speed of 30r/min, filtering obtains geranium oil.
CN201910375126.XA 2019-05-07 2019-05-07 A kind of extracting method of geranium oil Pending CN110129124A (en)

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