CN107189860A - The preparation method of Luo Xianzi essential oils and its application for removing free radical - Google Patents
The preparation method of Luo Xianzi essential oils and its application for removing free radical Download PDFInfo
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- CN107189860A CN107189860A CN201710450326.8A CN201710450326A CN107189860A CN 107189860 A CN107189860 A CN 107189860A CN 201710450326 A CN201710450326 A CN 201710450326A CN 107189860 A CN107189860 A CN 107189860A
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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
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K35/00—Medicinal preparations containing materials or reaction products thereof with undetermined constitution
- A61K35/56—Materials from animals other than mammals
- A61K35/63—Arthropods
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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
- C11B9/022—Refining
Abstract
The invention discloses the application of a kind of preparation method of Luo Xianzi essential oils and its removing free radical.The present invention prepares the significant Luo Xianzi essential oils of effect by specific solvent, operating process and ginseng data qualification.Luo Xianzi essential oils prepared by the inventive method have good purity, appearance character is significantly improved, for the golden yellow of clear, and penetrating odor is significantly reduced, wherein the fatty acid species contained are more, yield is high, wherein saturated fatty acid and unrighted acid ratio are 41.4%/58.5%, stability is good, and specific antioxidation well and the effect for removing free radical, application value are extensive.
Description
Technical field
The invention belongs to animal extraction of essential oil technical field, and in particular to the preparation method of a kind of Luo Xianzi essential oils and its clear
Except the application of free radical.
Background technology
Chinese medicine fairy maiden sieve, is Calliphoridae (Calliphoridae) chrysomyia megacephala (Chrysomyia megacephala).It is main
Originate in Hubei Hanchuan, Hanyang, Zhejiang Lanxi；Also produce on the ground such as Anhui, Guangdong.According to《Compendium of Materia Medica》、《Book on Chinese herbal medicine asks former》Record, this product
It is cold in nature, nontoxic, there is clearing heat and detoxicating, disperse accumulationsization stagnant.It is for oral administration to be used for treatment abdominal distension, infantile malnutrition, noma, aphtha etc.；
After drying and grinding, for putting deposited external application on the skin, the infectious surgical disease such as ulcer on the shank, lip pustule and ulcer can be treated.
Chemical analysis shows that Luo Xianzi contains crude protein 59~65%, it is necessary to which total amino acid content is 43.83%, and fat content is about
12%, unrighted acid accounts for 68.2% in grease, it is necessary to which aliphatic acid accounts for 36%.Clinic study finds Luo Xianzi in recent years
Medicinal material dry powder is for promoting infective wound surface healing, anti-curing arthritis and cardiovascular and cerebrovascular disease etc. to have good therapeutic effect.Pharmacological evaluation is demonstrate,proved
A variety of pharmacological activity such as real Luo Xianzi water extracts have antibacterial anti-inflammatory, antitumor and antiatherosclerosis.For Luo Xianzi essences
The research of oil is very few, and rarely seen so far its causes scorching, burn and scald to have significant curative effect mouse hyperlipemia, chemistry；Fatty acid F A1 and
FA2 significantly inhibits effect to human leukemia cell, human lung carcinoma cell, HIV-1 integrases.
The content of the invention
It is an object of the invention to provide a kind of preparation method of Luo Xianzi essential oils.
Another object of the present invention is to provide a kind of Luo Xianzi essential oils.
It is still another object of the present invention to provide the above method prepare Luo Xianzi essential oils prepare anti-oxidation preparation or/and
Remove the application in free based formulation.
The technical solution used in the present invention is：
The preparation method of Luo Xianzi essential oils, comprises the following steps：
1) preparation of Luo Xianzi crude oils：Luo Xianzi powder and solvent hexane are mixed, solid-liquid ratio is 1：15~1：25, surpass
Sound is extracted 2~4 times, 30~50min every time, and ultrasonic power is 400~500W；Filtering, is recovered under reduced pressure solvent, obtains Luo Xianzi thick
Oil；
2) crude oil degumming：Water is added when Luo Xianzi crude oils are heated into 48~52 DEG C, is crude oil volume with water volume
15%~20%, 10~22min is stirred under the conditions of 48~52 DEG C, centrifugation takes supernatant, obtains degummed oil；
3) depickling：Degummed oil is heated to 50~60 DEG C, being added according to degummed oil acid number can just antacid alkali soluble
Liquid, adds the aqueous slkali that volume is degumming oil volume 0.15%~0.2%, continues at 50~60 DEG C of heating stirrings, treat in addition
The floccule of generation stops stirring after condensing, centrifuging and taking supernatant obtains depickling oil；
4) wash：Depickling oil obtained by upper step is heated to 80~85 DEG C, 80~85 DEG C of water are added, water volume is depickling oil
28%~32%, continue to be heated to 80~85 DEG C of 28~32min of stirring, stratification, it is Luo Xianzi essential oils to take oil reservoir.
Further, step 2) described in centrifugation time be 4~6min, centrifugal rotational speed be 3500~4500r/min.
Further, step 2) described in aqueous slkali be 8%~12%w/v NaOH solution.
Further, step 3) described in heating stirring time be 28~32min.
Further, described water is distilled water.
Further, the above method comprises the following steps：
1) preparation of Luo Xianzi crude oils：Luo Xianzi powder and solvent hexane are mixed, solid-liquid ratio is 1：25, ultrasonic extraction
3 times, each 30min, ultrasonic power is 450W；Filtering, is recovered under reduced pressure solvent, obtains Luo Xianzi crude oils；
2) crude oil degumming：Distilled water is added when Luo Xianzi crude oils are heated into 50 DEG C, distilled water volume is crude oil volume
20%, 20min is stirred under the conditions of 50 DEG C, is centrifuged, is taken supernatant, obtain degummed oil；
3) depickling：Degummed oil is heated to 50 DEG C, according to degummed oil acid number add can just antacid NaOH solution,
The NaOH solution that volume is degumming oil volume 0.2% is added in addition, 50 DEG C of heating stirrings are continued at, and floccule to be generated coagulates
Stop stirring after knot, centrifuging and taking supernatant obtains depickling oil；
The NaOH solution concentration is 10%w/v；
4) wash：Depickling oil obtained by upper step is heated to 80 DEG C, 80~85 DEG C of distilled water are added, distilled water volume is depickling
The 30% of oil, continues to be heated to 80 DEG C of stirring 30min, stratification, and it is Luo Xianzi essential oils to take oil reservoir.
Further, above-mentioned steps 2) described in centrifugation time be 5min, centrifugal rotational speed is 4000r/min.
Further, above-mentioned steps 3) described in heating stirring time be 30min.
Luo Xianzi essential oils prepared by any of the above-described methods described.
Luo Xianzi essential oils prepared by any of the above-described methods described are in preparing anti-oxidation preparation or removing free based formulation
Using.
The beneficial effects of the invention are as follows：
Luo Xianzi essential oils prepared by the inventive method have good purity, and appearance character is significantly improved, and is clear
Golden yellow, and penetrating odor significantly reduces, wherein the fatty acid species contained are more, yield is high, wherein saturated fatty acid with
Unrighted acid ratio is 41.4%/58.5%, and stability is good, specific antioxidation well or the work for removing free radical
With application value is extensive.
Brief description of the drawings
Fig. 1 is Luo Xianzi essential oils and the appearance character comparison diagram of crude oil, and wherein A is crude oil, and B is essential oil；
Fig. 2 is the GC-MS chromatograms of Luo Xianzi essential oils.
Embodiment
With reference to specific embodiment, the present invention is further illustrated.
The preparation method of sieve fairy maiden's essential oil of embodiment 1
1) preparation of Luo Xianzi crude oils：After Luo Xianzi larva microwave dryings, Luo Xianzi powder is pulverized to obtain, by Luo Xianzi powder
Mixed with solvent hexane, solid-liquid ratio is 1：25, ultrasonic extraction 3 times, each 30min, ultrasonic power is 450W；Filtering, decompression
Recycling design, obtains Luo Xianzi crude oils；
2) crude oil degumming：Distilled water is added when Luo Xianzi crude oils are heated into 50 DEG C, distilled water volume is crude oil volume
20%, 20min is stirred under the conditions of 50 DEG C, is centrifuged, is taken supernatant, obtain degummed oil；
3) depickling：Degummed oil is heated to 50 DEG C, according to degummed oil acid number add can just antacid NaOH solution,
The NaOH solution (hereinafter referred to as excess alkali quantity) that volume is degumming oil volume 0.2% is added in addition, continues at 50 DEG C of heating stirrings
After 30min, the floccule of generation condenses, and stops stirring, and 4000r/min centrifugation 5min take supernatant to obtain depickling oil；The NaOH is molten
Liquid concentration is 10%w/v；
4) wash：Depickling oil obtained by upper step is heated to 80 DEG C, 80~85 DEG C of distilled water are added, distilled water volume is depickling
The 30% of oil, continues to be heated to 80 DEG C of stirring 30min, stratification, and it is Luo Xianzi essential oils to take oil reservoir.
The preparation method of sieve fairy maiden's essential oil of embodiment 2
1) preparation of Luo Xianzi crude oils：After Luo Xianzi larva microwave dryings, Luo Xianzi powder is pulverized to obtain, by Luo Xianzi powder
Mixed with solvent hexane, solid-liquid ratio is 1：15, ultrasonic extraction 2 times, each 50min, ultrasonic power is 400W；Filtering, decompression
Recycling design, obtains Luo Xianzi crude oils；
2) crude oil degumming：Distilled water is added when Luo Xianzi crude oils are heated into 48 DEG C, distilled water volume is crude oil volume
15%, 22min is stirred under the conditions of 48 DEG C, is centrifuged, is taken supernatant, obtain degummed oil；
3) depickling：Degummed oil is heated to 60 DEG C, according to degummed oil acid number add can just antacid NaOH solution,
The NaOH solution that volume is degumming oil volume 0.15% is added in addition, is continued at after 60 DEG C of heating stirring 32min, the wadding of generation
Shape thing condenses, and stops stirring, and 4500r/min centrifugation 4min take supernatant to obtain depickling oil；
The NaOH solution concentration is 12%w/v；
4) wash：Depickling oil obtained by upper step is heated to 85 DEG C, 85 DEG C of distilled water are added, distilled water volume is depickling oil
32%, continue to be heated to 85 DEG C of stirring 28min, stratification, it is Luo Xianzi essential oils to take oil reservoir.
The preparation method of sieve fairy maiden's essential oil of embodiment 3
1) preparation of Luo Xianzi crude oils：After Luo Xianzi larva microwave dryings, Luo Xianzi powder is pulverized to obtain, by Luo Xianzi powder
Mixed with solvent hexane, solid-liquid ratio is 1：20, ultrasonic extraction 4 times, each 30min, ultrasonic power is 500W；Filtering, decompression
Recycling design, obtains Luo Xianzi crude oils；
2) crude oil degumming：Distilled water is added when Luo Xianzi crude oils are heated into 52 DEG C, distilled water volume is crude oil volume
18%, 10min is stirred under the conditions of 52 DEG C, is centrifuged, is taken supernatant, obtain degummed oil；
3) depickling：Degummed oil is heated to 55 DEG C, according to degummed oil acid number add can just antacid NaOH solution,
The NaOH solution that volume is degumming oil volume 0.18% is added in addition, is continued at after 55 DEG C of heating stirring 28min, the wadding of generation
Shape thing condenses, and stops stirring, and 3500r/min centrifugation 6min take supernatant to obtain depickling oil；The NaOH solution concentration is 8%w/v；
4) wash：Depickling oil obtained by upper step is heated to 80 DEG C, 80 DEG C of distilled water are added, distilled water volume is depickling oil
28%, continue to be heated to 80 DEG C of stirring 32min, stratification, it is Luo Xianzi essential oils to take oil reservoir.
Further effect detection is made to Luo Xianzi essential oils prepared by the above embodiment of the present invention below.
First, the physics and chemistry value of Luo Xianzi essential oils and crude oil compares
Method：Take Luo Xianzi essential oils and Luo Xianzi crude oils progress acid number, iodine number, peroxide value and saponification prepared by the present invention
The measure of value, statistics and analysis, and appearance character is contrasted.
Acid number and determination of POV refer to standard GB/T/T 5009.37-2003.Determination of iodine value refers to national standard
GB/T5532-2008.Soap value test refers to standard GB/T/T5534-2008.
As a result：
Luo Xianzi essential oils and the appearance character of crude oil are as shown in figure 1, there it can be seen that Luo Xianzi essential oils appearance character is aobvious
Writing improves, and the golden yellow of clear is switched to by muddy sticky yellowish-brown, color is light, clarity is good, mobility is preferable, grease
Purity is high, and penetrating odor is significantly reduced.
Luo Xianzi essential oils and Luo Xianzi crude oils acid number, iodine number, the measurement result of peroxide value and saponification number are as shown in table 1.
Acid number represents the content of free fatty in grease, to evaluate the important indicator of oil quality, country of People's Republic of China (PRC) mark
Essential oil acid number is dictated in quasi- GBT26516-2011 massage essential oils and GBT 29990-2013 soothing oils, required respectively
Less than≤7mg/g and≤5mg/g, Luo Xianzi essential oils prepared by the present invention meet above standard regulation.In addition prepared by the present invention
Luo Xianzi essential oils iodine number be 18g/100g, peroxide value is 0.0164g/100g, saponification number 130.2122mg/g.
The fairy maiden sieve essential oil of table 1 and Luo Xianzi crude oil physics and chemistry value contrast (N=3)
2nd, Luo Xianzi Essential Oil Chemistries composition and ratio analysis
Method：
(1) preparation of fatty acid methyl ester
Precision weighs the Luo Xianzi essential oil 0.15g of the preparation of embodiment 1, adds 0.5mol/L potassium hydroxide-methanol solution
2mL, 65 DEG C of water-bath to oil droplets are wholly absent, and 14% boron trifluoride-methanol solution 2mL is added after cooling, and 10min is boiled in water-bath,
Cooled down in room temperature, add isooctane 10mL, saturated nacl aqueous solution 20mL, take supernatant in test tube, plus anhydrous sodium sulfate, from
The heart is layered, and takes supernatant to save backup.
(2) GC-MS analysis conditions
Chromatographic condition：Chromatographic column HP-5MS (30m × 0.25mm × 0.25 μm)；Using temperature programming, 160 DEG C of initial temperature, with 5
DEG C/min is warming up to 170 DEG C, and 176 DEG C are warming up to 3 DEG C/min, keeps 2min, and 190 DEG C, holding are warming up to 5 DEG C/min
10min；280 DEG C of injector temperature；250 DEG C of detector temperature；Carrier gas is high-purity helium, flow velocity 1.0mL/min；The μ of sample size 1.0
L, split ratio 40: 1.
Mass Spectrometry Conditions：Ionization mode is electron bombardment (EI), electron energy 70eV, 250 DEG C of interface temperature；Mass scanning model
Enclose (m/z) 35~500u.Mass spectrum retrieves software NIST02, and quantitative analysis is carried out using peak area normalization method.
As a result：
The GC-MS chromatograms of Luo Xianzi essential oils as shown in Fig. 2 using gas chromatograph-mass spectrometer to the chemistry in Luo Xianzi essential oils into
Be grouped into and relative amount detection and analysis result as shown in table 2, containing 13 kinds of fatty acid composition, wherein saturated fatty acid with
Unrighted acid ratio is 41.4%/58.5%.
The composition and relative amount of aliphatic acid in Luo Xianzi essential oils prepared by the present invention of table 2
3rd, Luo Xianzi essential oils autoxidation stability study
The influence for the Luo Xianzi essential oil stability that environment temperature and illumination are prepared to the inventive method is investigated, with acid number and mistake
Oxidation number is used as evaluation index.
(1) influence of the temperature to Luo Xianzi essential oil stability
Precision weighs 3 parts of Luo Xianzi essential oils prepared by the present invention, and every part of 100g is placed in 250mL conical flask, respectively at 4
DEG C, 25 DEG C, lucifuge condition is placed under 55 DEG C of different temperatures.Its peroxide value, acid number are determined every 3d in 20d, is surveyed 5 times altogether.By
Table 2,3 understands that variation of ambient temperature is to the acid number and peroxide value of Luo Xianzi essential oils without significant change.
The temperature of table 3 to the present invention prepare Luo Xianzi essential oil acid numbers influence (N=3, mg/g)
The temperature of table 4 to the present invention prepare Luo Xianzi essential oil peroxide values influence (N=3, g/100g)
(2) influence of the illumination to Luo Xianzi essential oil stability
Precision weighs 2 parts of Luo Xianzi essential oils prepared by the present invention, and every part of 100g is placed in 250mL conical flask, 25 DEG C of bars
Under part, portion is kept in dark place, and portion is exposed under natural light, the acid number and peroxide value for determining essential oil every 3d, is surveyed 5 times altogether.
From table 5, table 6, under the conditions of illumination or lucifuge, the acid number and peroxide value of Luo Xianzi essential oils are without significant change.
The illumination of table 5 to the present invention prepare Luo Xianzi essential oil acid numbers influence (N=3, mg/g)
The illumination of table 6 to the present invention prepare Luo Xianzi essential oil peroxide values influence (N=3, g/100g)
To sum up, temperature has not significant impact with illumination to the stability of Luo Xianzi essential oils, shows sieve prepared to the present invention
Fairy maiden's essential oil self stability is preferable, it is easy to preserve.
4th, the external effect of scavenging radical research of Luo Xianzi essential oils
Material：2,2- connection nitrogen-two (3- ethyls-benzothiazole -6- sulfonic acid) di-ammonium salts (ABTS) (lot number 201603101),
1,1- diphenyl -2- hardship diazanyls (DPPH) (lot number 201608101) are purchased from Chengdu Chinese mugwort Kodak chemical reagent Co., Ltd；Vitamin C
Sour (Vc, purity 98%) is purchased from Tianjin great Mao chemical reagent factories.
The preparation of reference substance solution：Take Vc with 95% ethanol constant volume in volumetric flask, be configured to original concentration for 0.5mg/
ML Vc solution；The Vc solution for drawing different volumes distinguishes constant volume in 10mL volumetric flasks with 95% ethanol, obtains Vc concentration models
Enclose 0.002~0.008mg/mL solution.
The preparation of need testing solution：Take Luo Xianzi essential oil ethyl acetate constant volumes prepared by the present invention in volumetric flask, match somebody with somebody
The sample solution that original concentration is 0.5g/mL is made；The sample solution for drawing different volumes is held with ethyl acetate constant volume in 10mL
In measuring bottle, 0.02~0.07g/mL of concentration range sample solution is obtained.
The preparation of working solution：DPPH working solutions are prepared：0.0041g DPPH powder ethyl acetate constant volumes are taken in 100mL
In volumetric flask, 105 μm of ol/L DPPH solution, lucifuge sealing preserve are configured to.
ABTS working solutions are prepared：The ABTS powder for weighing 0.3841g is dissolved in 100mL distilled water and is configured to 7mmol/L's
ABTS solution, weighs 0.0993gK2S2O8It is dissolved in the K that 7.35mmol/L is configured in 50mL distilled water2S2O8Solution, ABTS is molten
Liquid and K2S2O8Solution by volume 2:12~16h of reacting at normal temperature without light after 1 mixing, obtains ABTS+Storing solution, uses preceding use nothing
Water-ethanol dilution is between its absorbance is at 734nm for 0.70 ± 0.02.
(1)DPPH+Scavenging activity is determined
Sample solution is to DPPH+Scavenging activity is determined：The sample solution and 2mL of 2mL different quality concentration are drawn respectively
DPPH+ working solutions are mixed, and dark place stands 10min after eddy oscillating 30s, and its absorbance is determined at 517nm, and each concentration is parallel
Survey three times, clearance rate and IC are calculated by formula (1)50Value (mass concentration of sample when clearance rate is 50%).Vc is to DPPH+Remove
The same sample of ability assay method.
K=[1- (Ai-Aj)/Ac] × 100%
The absorbance of Ai-2mL DPPH solution+2mL samples；The absorbance of Aj-2mL sample+2mL ethyl acetate；Ac-2mL
The absorbance of DPPH solution+2mL ethyl acetate.
As a result：Luo Xianzi essential oils prepared by the inventive method act on DPPH radicals scavengings measurement result as shown in table 7,
As can be seen that Luo Xianzi essential oils have certain Scavenging activity to DPPH free radicals in asking, in selected concentration range, sample
Concentration and there is good linear relationship to free radical scavenging activity, according to calibration curve equation calculate IC50Value.
Luo Xianzi essential oils prepared by the inventive method of table 7 act on measurement result to DPPH radicals scavengings
(2)ABTS+Scavenging activity is determined
Sample is to ABTS+Scavenging activity is determined：The sample solution and 2mL ABTS of 1mL different quality concentration are drawn respectively+Work
Make room temperature dark place after liquid mixing, eddy oscillating 30s and react 8min, absorbance is determined at 734nm wavelength, each concentration is parallel to be surveyed
Three times, clearance rate and IC are calculated by formula (1)50Value (mass concentration of sample when clearance rate is 50%).Vc is to ABTS+Remove energy
The same sample of power assay method.
The absorbance of Ai-2mL ABTS solution+1mL samples；The absorbance of Aj-1mL sample+2mL ethanol；Ac-2mLABTS
The absorbance of solution+1mL ethyl acetate.
Luo Xianzi essential oils prepared by the inventive method of table 8 are to ABTS radical scavenging activity measurement results
As a result：Luo Xianzi essential oils prepared by the inventive method are as described in Table 8 to ABTS radical scavenging activities measurement result,
Luo Xianzi essential oils to ABTS free radicals also have certain Scavenging activity, in selected concentration range, the concentration of sample with to from
There is good linear relationship by base clearance rate, IC is calculated according to calibration curve equation50Value.
In research process of the present invention, inventor have also been devised substantial amounts of contrast experiment, and its extraction effect is not as good as this hair
Bright method.
First, comparative analysis of the different extracting modes to Luo Xianzi crude oil yield
(1) cold-maceration extraction method
Precision weighs Luo Xianzi powder 20g, in the conical flask for being placed in tool plug, adds n-hexane 500mL, and room temperature is extracted 3 times,
Each 8h, filtering merges extract solution, and solvent is recovered under reduced pressure to constant weight, oil yield is determined.
(2) soxhlet extraction
Precision weighs Luo Xianzi powder 20g, is placed in apparatus,Soxhlet's, using 500mL n-hexanes as solvent extraction 3 times, often
Secondary 8h, merges extract solution, and solvent is recovered under reduced pressure to constant weight, oil yield is determined.
(3) supercritical fluid extraction
Precision weighs Luo Xianzi powder 100g and loads CO2In supercritical extraction reactor, extracting pressure is set as 30MPa, is extracted
58 DEG C of temperature, CO2Flow 25L/h, extraction time 90min, increasing temperature and pressure to setting value are extracted, isolated fairy maiden sieve of separating still
Crude oil, determines oil yield.
(4) ultrasonic extraction of the present invention
Precision weighs Luo Xianzi powder 20g, is placed in conical flask, adds 500mL n-hexanes, 3 (power of ultrasonic extraction
400W), each 30min, filtering, is recovered under reduced pressure solvent, obtains Luo Xianzi crude oils.
As a result：
The oil yield of different crude oil extracting methods is as shown in table 9, there it can be seen that the oil yield row of Different Extraction Method
Sequence is：Ultrasonic extraction>Surname extraction>Cold soaking>Means of supercritical extraction, the effect of other crude oil extracting methods is super not as good as the present invention
Sound method extraction effect.
Under the conditions of the Different Extraction Method of table 9 Luo Xianzi crude oils yield (N=3)
2nd, the Contrast on effect analysis that different solvents are extracted
Precision weighs 4 parts of Luo Xianzi dry powder, every part of 20g, respectively with 500mL petroleum ether-acetone, n-hexane-acetone, stone
Oily ether and the n-hexane of the present invention are used as Extraction solvent, ultrasonic extraction 3 times (power 400W), each 30min.
As shown in Table 10, n-hexane-acetone, two kinds of solvents of petroleum ether-acetone oil yield it is slightly higher, but gained crude oil color depth
Muddiness, no explanation impurity content is excessive.The grease obtained color of n-hexane extraction is light, and clarity is good, mobility is preferable, grease is pure
Degree is high, is contrasted through comprehensive analysis, and the effect of other 3 kinds of solvent extractions is not as good as the effect of n-hexane extraction.
The different solvents of table 10 oil yield (N=3)
3rd, different feed liquid compares than carrying out the effect of Luo Xianzi crude oil extractions
Precision weighs 5 parts of Luo Xianzi dry powder, every part of 20g, respectively according to solid-liquid ratio 1:5、1:10、1:15、1:20、1:25 Hes
1：30 add hexane solution, ultrasonic extraction 3 times (power 400W), each 30min.
As shown in Table 11, extraction efficiency and solvent-oil ratio are considered, solid-liquid ratio is 1:15~1:25, most preferably 1：
25。
The different feed liquid of table 11 than oil yield (N=3)
4th, influence of the different ultrasonic number of times to Luo Xianzi crude oil extraction effects
Precision weighs 5 parts of Luo Xianzi dry powder, every part of 20g, by solid-liquid ratio 1:25 add n-hexanes, respectively ultrasonic extraction 1,2,
3rd, 4,5 (power 400W), each 30min.Consider extraction efficiency and time cost,
As shown in Table 12,2~4 effects of ultrasonic extraction are preferable, most preferably 4 times.
The different ultrasonic number of times of table 12 oil yield (N=3)
5th, influence of the different ultrasonic extraction times to Luo Xianzi crude oil extraction effects
Precision weighs 5 parts of Luo Xianzi dry powder, every part of 20g, by solid-liquid ratio 1:25 add n-hexane, 3 (power of ultrasonic extraction
400W), every time 30,40,50,60,70min.
As shown in Table 13, extraction efficiency and time cost are considered, effect is preferable when extraction time is 30~50min.
The different ultrasonic times of table 13 oil yield (N=3)
6th, influence of the different supersonic frequencies to Luo Xianzi crude oil extraction effects
Precision weighs 5 parts of Luo Xianzi dry powder, every part of 20g, by solid-liquid ratio 1:25 add n-hexane, 3 (power of ultrasonic extraction
400W), each 30min, supersonic frequency is 300 respectively, 350,400,450,500W.
As shown in Table 14, effect is preferable when supersonic frequency is 400~500W.
The different supersonic frequencies of table 14 oil yield (N=3)
7th, crude oil extraction factor is analyzed
Solid-liquid ratio, ultrasonic number of times, the factor of ultrasonic time three are carried out to the inspection of effect between main body, the assay such as institute of table 15
Show.
The inspection of effect between the main body of table 15
a.R2=0.986 (adjustment R2=0.945)
As shown in Table 15, influence of each factor to oil yield：Ultrasonic number of times (B) ＞ solid-liquid ratio (A) ＞ ultrasonic times (C).
Wherein factor A and B influence is more notable；Optimum condition is A3B3C1.Therefore optimal Luo Xianzi crude oil extraction conditions are：Feed liquid
Than 1:25th, ultrasound number of times 3 times, extraction time 30min.
8th, influence of the different amount of water to degumming efficiency, essential oil yield
5 test tubes are taken, precision weighs appropriate Luo Xianzi crude oils respectively, be heated to 50 DEG C, investigate the addition point of distilled water
Not Wei crude oil volume 5%, 10%, 15%, 20%, 30% when influence to degumming efficiency, essential oil yield.Except scouring processes
Middle each group water consumption is different, and other operations are all identical, and the operation recorded according to embodiment 1 is carried out.
When amount of water is 15%~20%, thoroughly, gained oil color switchs to clarification golden yellow by muddy yellowish-brown for degumming,
And essential oil yield is preferably (up to more than 88.75%), wherein the best results when amount of water is 20%；And when amount of water is other feelings
During condition, or degumming is not thorough, or essential oil yield is too low, or easily cooperating microorganisms cause corruption, it is unfavorable for the guarantor of essential oil
Deposit.
9th, influence of the acid adding amount to degumming efficiency, essential oil yield
5 test tubes are taken, precision weighs appropriate Luo Xianzi crude oils respectively, are heated to 50 DEG C, amount of water is under conditions of 20%,
Investigate the influence to degumming efficiency, essential oil yield when phosphoric acid addition is respectively 0.3%, 0.4%, 0.5%, 0.6%, 0.7%.
Except each group acid adding amount is different in scouring processes, other operations are all identical, and the operation recorded according to embodiment 1 is carried out.
As a result show, sour addition is not obvious to Luo Xianzi crude oils degumming effect, unobvious is improved to essential oil character, and draw
The corruption of essential oil, influence essential oil yield (table 16) are played.Therefore be not suitable for acid adding in the preparation process of Luo Xianzi essential oils of the present invention
Carry out degumming.
The acid adding amount of table 16 to essential oil yield after degumming influence (N=3)
Tenth, influence of the heating-up temperature to degumming efficiency, essential oil yield
5 test tubes are taken, precision weighs appropriate Luo Xianzi crude oils respectively, amount of water is under conditions of 20%, to investigate heating temperature
Degree is respectively 30,40,50,60,70 DEG C when influence to degumming efficiency, essential oil yield.Except each group heating temperature in scouring processes
Degree is different, and other operations are all identical, and the operation recorded according to embodiment 1 is carried out.
As shown in Table 17, when heating-up temperature is 30 DEG C, 40 DEG C, 60 DEG C, 70 DEG C essential oil yield is 50 not as good as temperature
DEG C when essential oil yield.
The heating-up temperature of table 17 to essential oil yield after degumming influence (N=3)
11, influence of the heat time to degumming efficiency, essential oil yield
5 test tubes are taken, precision weighs appropriate Luo Xianzi crude oils respectively, are heated to 50 DEG C, amount of water is under conditions of 20%,
Investigate the heat time be respectively 10,20,30,40,50min when influence to degumming efficiency, essential oil yield.Except in scouring processes
The each group heat time is different, and other operations are all identical, and the operation recorded according to embodiment 1 is carried out.
As shown in Table 18, the heat time is significantly higher than the essential oil of other plus heat time for 10~20min essential oil yield
Yield.
The heat time of table 18 to essential oil yield after degumming influence (N=3)
12, deacidification alkali concn and alkali number influence on deacidification efficiency, essential oil yield
Precision weighs the degummed oil in appropriate above-described embodiment, according to standard GB/T/T 5009.37-2003 regulation sides
Method determines acid value, and total caustic dosage is calculated according to acid number.Degummed oil is heated to 50 DEG C, appropriate NaOH solution, magnetic force is rapidly joined
Stirring is thoroughly mixed alkali lye and oil, occurs tiny neat soap gradually, stops stirring after floccule fully condenses, and centrifuges.
Supernatant is placed 80 DEG C are heated in beaker, add 80-85 DEG C of distilled water, water is the 30% of oil mass volume, continues to stir
After 30min, it is statically placed in separatory funnel and separates, a few drop instructions phenolphthalein solutions is added dropwise in the waste water separated, be washed in waste water and phenol is added dropwise
Nondiscolouring can stop washing after phthalein.
M1=7.13 × VA × G0/10000C；M2=G0×w；
In formula：M1- theory caustic dosages (g)；M2- excess alkali quantities (g)；The acid number (mg/g) of sieve's VA- fairy maiden's degummed oil；G0- sieve
The quality (g) of fairy maiden's degummed oil；The mass fraction (%) of C-NaOH solution；W- excess alkali quantities account for the percentage of Luo Xianzi degumming oil masses
(%).
(1) influence of the alkali concn to deacidification efficiency
Except each group NaOH alkaline concentrations w/v is different (2%, 6%, 10%, 14%, 18%) in deacidification, other
Operation is all identical, and the operation recorded according to embodiment 1 is carried out.
Acid number and oil yield using Luo Xianzi essential oils is index, and overall merit deacidification efficiency works as alkali concn as shown in Table 19
Essential oil yield and the overall merit highest of essential oil acid number during for 10%w/v, when alkali concn is 2%, 6%, 14% or 18%
Essential oil yield is too low, otherwise essential oil acid number is higher.
The alkali concn of table 19 on deacidification efficiency influence (N=3)
(2) influence of the excess alkali quantity to deacidification efficiency
Except excess alkali quantity is different in deacidification, i.e., 10%w/v NaOH solutions consumption is being capable of antacid base in each group
The amount that volume is degumming oil volume 0.05%, 0.1%, 0.15%, 0.2%, 0.25% is separately added on plinth again, other operations are all
Identical, the operation recorded according to embodiment 1 is carried out.
Acid number and oil yield using essential oil is index, overall merit deacidification efficiency, as shown in Table 20 when excess alkali quantity is degumming
During oil volume 0.15%~0.2%, the overall merit highest of essential oil yield and essential oil acid number, when excess alkali quantity is other situations,
Essential oil yield is too low, otherwise essential oil acid number is higher.
The excess alkali quantity of table 20 on deacidification efficiency influence (N=3)
13, deacidification heating-up temperature influences on deacidification efficiency, essential oil yield
Except each group heating-up temperature is different (be respectively set to 40,50,60,70,80 DEG C) in deacidification, other operations are all
Identical, the operation recorded according to embodiment 1 is carried out.
Acid number and oil yield using essential oil is index, overall merit deacidification efficiency, as shown in Table 21 when heating-up temperature is 50
At~60 DEG C, the overall merit highest of essential oil yield and essential oil acid number, or essential oil yield is too low under its temperature conditions
Essential oil acid number is higher.
The heating-up temperature of table 21 to deacidification efficiency influence (N=3)
13, the deacidification heat time influences on deacidification efficiency, essential oil yield
Except in deacidification each group heat time it is different (be respectively set to 15,20,25,30,35min), other operations
All identical, the operation recorded according to embodiment 1 is carried out.
Acid value and oil yield using essential oil is index, overall merit deacidification efficiency, and the heat time is 30min as shown in Table 22
When, the overall merit highest of essential oil yield and essential oil acid number, the heat time be 15,20,25,35min when, or essential oil yield is too
It is low, otherwise essential oil acid number is higher.
The heat time of table 22 to deacidification efficiency influence (N=3)
Above-described embodiment is preferably embodiment, but embodiments of the present invention are not by above-described embodiment of the invention
Limitation, other any Spirit Essences without departing from the present invention and the change made under principle, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. the preparation method of sieve fairy maiden's essential oil, it is characterised in that comprise the following steps：
1) preparation of Luo Xianzi crude oils：Luo Xianzi powder and solvent hexane are mixed, solid-liquid ratio is 1：(15~25), ultrasound is carried
Take 2~4 times, every time 30~50min, ultrasonic power is 400~500W；Filtering, is recovered under reduced pressure solvent, obtains Luo Xianzi crude oils；
2) crude oil degumming：Add water when Luo Xianzi crude oils are heated into 48~52 DEG C, with 15% that water volume is crude oil volume~
20%, 10~22min is stirred under the conditions of 48~52 DEG C, centrifugation takes supernatant, obtains degummed oil；
3) depickling：Degummed oil is heated to 50~60 DEG C, according to degummed oil acid number add can just antacid aqueous slkali, separately
It is outer to add the aqueous slkali that volume is degumming oil volume 0.15%~0.2%, 50~60 DEG C of heating stirrings are continued at, it is to be generated
Floccule stops stirring after condensing, centrifuging and taking supernatant obtains depickling oil；
4) wash：Depickling oil obtained by upper step is heated to 80~85 DEG C, 80~85 DEG C of water are added, water volume is the 28% of depickling oil
~32%, continue to be heated to 80~85 DEG C of 28~32min of stirring, stratification, it is Luo Xianzi essential oils to take oil reservoir.
2. centrifugation time described according to the method described in claim 1, it is characterised in that step 2) is 4~6min, centrifugation turns
Speed is 3500~4500r/min.
3. aqueous slkali described according to the method described in claim 1, it is characterised in that step 2) is 8%~12%w/v's
NaOH solution.
4. the time of heating stirring described according to the method described in claim 1, it is characterised in that step 3) be 28~
32min。
5. according to the method described in claim 1, it is characterised in that described water is distilled water.
6. according to the method described in claim 1, it is characterised in that comprise the following steps：
1) preparation of Luo Xianzi crude oils：Luo Xianzi powder and solvent hexane are mixed, solid-liquid ratio is 1：25, ultrasonic extraction 3 times,
Each 30min, ultrasonic power is 450W；Filtering, is recovered under reduced pressure solvent, obtains Luo Xianzi crude oils；
2) crude oil degumming：Distilled water is added when Luo Xianzi crude oils are heated into 50 DEG C, distilled water volume is the 20% of crude oil volume,
20min is stirred under the conditions of 50 DEG C, is centrifuged, is taken supernatant, obtain degummed oil；
3) depickling：Degummed oil is heated to 50 DEG C, according to degummed oil acid number add can just antacid NaOH solution, in addition
The NaOH solution that volume is degumming oil volume 0.2% is added, 50 DEG C of heating stirrings are continued at, after floccule to be generated condenses
Stop stirring, centrifuging and taking supernatant obtains depickling oil；
The NaOH solution concentration is 10%w/v；
4) wash：Depickling oil obtained by upper step is heated to 80 DEG C, 80~85 DEG C of distilled water are added, distilled water volume is depickling oil
30%, continue to be heated to 80 DEG C of stirring 30min, stratification, it is Luo Xianzi essential oils to take oil reservoir.
7. method according to claim 6, it is characterised in that step 2) described in centrifugation time be 5min, centrifugal rotational speed
For 4000r/min.
8. method according to claim 6, it is characterised in that step 3) described in time of heating stirring be 30min.
9. the Luo Xianzi essential oils prepared by any one of claim 1~8 methods described.
10. Luo Xianzi essential oils prepared by any one of claim 1~8 methods described are preparing anti-oxidation preparation or/and removed certainly
By the application in based formulation.
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