CN106318644A - Preparation method of navel orange essential oil molecule distillation component - Google Patents
Preparation method of navel orange essential oil molecule distillation component Download PDFInfo
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- CN106318644A CN106318644A CN201610944365.9A CN201610944365A CN106318644A CN 106318644 A CN106318644 A CN 106318644A CN 201610944365 A CN201610944365 A CN 201610944365A CN 106318644 A CN106318644 A CN 106318644A
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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
- C11B9/027—Recovery of volatiles by distillation or stripping
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/08—Magnoliopsida [dicotyledons]
- A01N65/36—Rutaceae [Rue family], e.g. lime, orange, lemon, corktree or pricklyash
-
- 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
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- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
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- Agronomy & Crop Science (AREA)
- Zoology (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Plant Pathology (AREA)
- Dentistry (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Biotechnology (AREA)
- Environmental Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
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Abstract
The invention discloses a preparation method of a navel orange essential oil molecule distillation component. The preparation method comprises the following steps of: filling cold-pressed essential oil into a feeding bottle of a molecular distillation device, and starting a condenser; after cooling the system, setting the vacuum degree, and setting distillation temperature after the pressure is stabilized; and after both the vacuum degree and the temperature achieve the set values, regulating the rotating speed of a scraper membrane, switching on a feed valve, controlling the flow rate of materials, performing molecular distillation and collecting the distilled-off component. The cold-pressed orange essential oil is processed by applying a molecular distillation technology, the preparation method has the advantages that the vacuum degree is high, the heating temperature is low, thermosensitive substances are difficult to damage, any organic solvents cannot be brought in during distillation. The essential oil product prepared by adopting the method is free from pigments, wax, agricultural residues and the like, the smell is faintly scent, the components are natural, the antibacterial effect is obvious, and the essential oil product can be used as a new hidden source of antibacterial agents and food preservatives.
Description
Technical field
The present invention relates to the deep process technology field of agricultural product, particularly relate to a kind of navel orange essential oil molecule having bacteriostasis efficacy
The preparation method of distillation component.
Background technology
Citrus sinensis Osbeck with its meat tender and crispization slag, the dense sweet fragrance of local flavor and well-known.Citrus sinensis Osbeck peel accounts for the 20%-of fresh fruit weight
30%, containing multiple available compositions such as pectin, quintessence oil and flavone.The volatilization with aromatic odor of isolated in peel of Citrus sinensis Osbeck
Property oily mater is quintessence oil.Its main component is the composition such as terpenes, sesquiterpene and alcohols, aldehydes, ketone, esters
Oxygenatedchemicals, wherein limonene is main component.Containing several physiological active substances in orange quintessence oil, have antibacterial, antioxidation,
Antiinflammatory, subside a swelling, the multiple physiologically active such as analgesia, be widely used in multiple fields such as food, medicine, chemical industry and cosmetics,
There is important economic worth.
Cold-press method is the main method of extensive preparation orange quintessence oil, is during squeezing the juice, by the machinery pressure of crusher
Oil sac cell in Fructus Citri junoris outer peel is crushed by power effect, makes quintessence oil ooze out, and recycling disk centrifugal equipment carries out oil-water residue and divides
From.Cold pressed orange oil complicated component, is unfavorable for doing the composition of antimicrobial antistaling agent containing pigment, wax and agriculture are residual etc..
At present, along with people are to the concern of food safety and the requirement of exploitation crude antistaling agent, pressing down of natural plant essential oils
Bacterium effect has good prospect for field of food preservation.Orange quintessence oil be in the world yield and consumption most natural plants essence
Oil, processes navel orange essential oil with molecular distillation technique, and studies its antibacterial activity, develop novel antimicrobial antistaling agent, also
Not yet there are document and patent report.
Summary of the invention
The technical problem existed based on background technology, the present invention proposes a kind of navel orange essential oil molecule having bacteriostasis efficacy and steams
Evaporate the preparation method of component, specifically comprise the following steps that
1) quintessence oil of colding pressing is loaded in the feeding bottle of molecular distillation apparatus, open cold condenser；
2) after system cooling, set vacuum, after pressure stability, set vapo(u)rizing temperature；
3) after vacuum and temperature all reach setting value, regulate knifing rotating speed, open inlet valve, control mass flow, enter
Row molecular distillation, collects and distillates component.
Preferably, described step 2) in, vacuum is 8.0-12.0Torr, vapo(u)rizing temperature is 50.0-60.0 DEG C.
Preferably, described step 3) in, knifing rotating speed is 300-350r/min, mass flow is 2.5-3.5mL/min.
Compared with prior art, the device have the advantages that and be:
1. present invention application molecular distillation technique orange quintessence oil of colding pressing is processed, and has vacuum high, and heating-up temperature is low,
Heat-sensitive substance is not easily susceptible to destroy, the advantage that will not bring any organic solvent in still-process into.
2. the essential oil product that prepared by the inventive method eliminates the materials such as pigment, wax and agriculture be residual, abnormal smells from the patient delicate fragrance, composition sky
So, fungistatic effect is notable, can be as new antibacterial and the potential source of food preservative.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is explained orally further.
Embodiment 1
The present invention proposes the preparation method of a kind of navel orange essential oil molecular distillation component having bacteriostasis efficacy, and concrete steps are such as
Under:
1) preparation of navel orange essential oil
Employing mandate China national patent of invention (method that three grades of dish of a kind of employing reclaim, from system, navel orange essential oil of colding pressing,
2014, CN102719316 B) in method；While squeezing the juice, utilize pressure and the dissection of virgin cup, make peel extexine
Oil vacuole rupture release quintessence oil.Meanwhile, the ring-type water injector water spray on upper virgin cup top, the mixture of peel and quintessence oil is gone out
Enter conveying worm, through vibrosieve isolated yellow pureed liquid.Then disk centrifugal equipment is used to carry out oil-water residue separation,
Obtain navel orange essential oil of colding pressing, for orange transparent supernatant liquid.
2) preparation of navel orange essential oil molecular distillation component
(1) quintessence oil of being colded pressing by 500mL (422.5g) loads in the feeding bottle of molecular distillation apparatus, open cold condenser；
(2) after system cooling, set vacuum 8.0Torr, after pressure stability, set vapo(u)rizing temperature 50.0 DEG C；
(3), after vacuum and temperature all reach setting value, regulation knifing rotating speed is 300r/min, opens inlet valve, controls
Mass flow is 2.5mL/min, carries out molecular distillation, collects and distillates component, obtains 380.0g distillage, and productivity is
90.0%.
Embodiment 2
The present invention proposes the preparation method of a kind of navel orange essential oil molecular distillation component having bacteriostasis efficacy, and concrete steps are such as
Under:
1) preparation of navel orange essential oil
Employing mandate China national patent of invention (method that three grades of dish of a kind of employing reclaim, from system, navel orange essential oil of colding pressing,
2014, CN102719316 B) in method；While squeezing the juice, utilize pressure and the dissection of virgin cup, make peel extexine
Oil vacuole rupture release quintessence oil.Meanwhile, the ring-type water injector water spray on upper virgin cup top, the mixture of peel and quintessence oil is gone out
Enter conveying worm, through vibrosieve isolated yellow pureed liquid.Then disk centrifugal equipment is used to carry out oil-water residue separation,
Obtain navel orange essential oil of colding pressing, for orange transparent supernatant liquid.
2) preparation of navel orange essential oil molecular distillation component
(1) quintessence oil of being colded pressing by 500mL (422.5g) loads in the feeding bottle of molecular distillation apparatus, open cold condenser；
(2) after system cooling, set vacuum 12.0Torr, after pressure stability, set vapo(u)rizing temperature 60.0 DEG C；
(3), after vacuum and temperature all reach setting value, regulation knifing rotating speed is 350r/min, opens inlet valve, controls
Mass flow is 3.5mL/min, carries out molecular distillation, collects and distillates component, obtains 385.3g distillage, and productivity is
91.2%.
Embodiment 3
The present invention proposes the preparation method of a kind of navel orange essential oil molecular distillation component having bacteriostasis efficacy, and concrete steps are such as
Under:
1) preparation of navel orange essential oil
Employing mandate China national patent of invention (method that three grades of dish of a kind of employing reclaim, from system, navel orange essential oil of colding pressing,
2014, CN102719316 B) in method；While squeezing the juice, utilize pressure and the dissection of virgin cup, make peel extexine
Oil vacuole rupture release quintessence oil.Meanwhile, the ring-type water injector water spray on upper virgin cup top, the mixture of peel and quintessence oil is gone out
Enter conveying worm, through vibrosieve isolated yellow pureed liquid.Then disk centrifugal equipment is used to carry out oil-water residue separation,
Obtain navel orange essential oil of colding pressing, for orange transparent supernatant liquid.
2) preparation of navel orange essential oil molecular distillation component
(1) quintessence oil of being colded pressing by 500mL (422.5g) loads in the feeding bottle of molecular distillation apparatus, open cold condenser；
(2) after system cooling, set vacuum 10.0Torr, after pressure stability, set vapo(u)rizing temperature 55.0 DEG C；
(3), after vacuum and temperature all reach setting value, regulation knifing rotating speed is 325r/min, opens inlet valve, controls
Mass flow is 3.0mL/min, carries out molecular distillation, collects and distillates component, obtains 386.6g distillage, and productivity is
91.5%.
Embodiment 4
The present invention proposes the preparation method of a kind of navel orange essential oil molecular distillation component having bacteriostasis efficacy, and concrete steps are such as
Under:
1) preparation of navel orange essential oil
Employing mandate China national patent of invention (method that three grades of dish of a kind of employing reclaim, from system, navel orange essential oil of colding pressing,
2014, CN102719316 B) in method；While squeezing the juice, utilize pressure and the dissection of virgin cup, make peel extexine
Oil vacuole rupture release quintessence oil.Meanwhile, the ring-type water injector water spray on upper virgin cup top, the mixture of peel and quintessence oil is gone out
Enter conveying worm, through vibrosieve isolated yellow pureed liquid.Then disk centrifugal equipment is used to carry out oil-water residue separation,
Obtain navel orange essential oil of colding pressing, for orange transparent supernatant liquid.
2) preparation of navel orange essential oil molecular distillation component
(1) quintessence oil of being colded pressing by 500mL (422.5g) loads in the feeding bottle of molecular distillation apparatus, open cold condenser；
(2) after system cooling, set vacuum 10.0Torr, after pressure stability, set vapo(u)rizing temperature 60.0 DEG C；
(3), after vacuum and temperature all reach setting value, regulation knifing rotating speed is 350r/min, opens inlet valve, controls
Mass flow is 3.0mL/min, carries out molecular distillation, collects and distillates component, obtains 393.0g distillage, and productivity is
93.0%.
Embodiment 5
The present invention proposes the preparation method of a kind of navel orange essential oil molecular distillation component having bacteriostasis efficacy, and concrete steps are such as
Under:
1) preparation of navel orange essential oil
Employing mandate China national patent of invention (method that three grades of dish of a kind of employing reclaim, from system, navel orange essential oil of colding pressing,
2014, CN102719316 B) in method；While squeezing the juice, utilize pressure and the dissection of virgin cup, make peel extexine
Oil vacuole rupture release quintessence oil.Meanwhile, the ring-type water injector water spray on upper virgin cup top, the mixture of peel and quintessence oil is gone out
Enter conveying worm, through vibrosieve isolated yellow pureed liquid.Then disk centrifugal equipment is used to carry out oil-water residue separation,
Obtain navel orange essential oil of colding pressing, for orange transparent supernatant liquid.
2) preparation of navel orange essential oil molecular distillation component
(1) quintessence oil of being colded pressing by 500mL (422.5g) loads in the feeding bottle of molecular distillation apparatus, open cold condenser；
(2) after system cooling, set vacuum 9.0Torr, after pressure stability, set vapo(u)rizing temperature 58.0 DEG C；
(3), after vacuum and temperature all reach setting value, regulation knifing rotating speed is 320r/min, opens inlet valve, controls
Mass flow is 2.9mL/min, carries out molecular distillation, collects and distillates component, obtains 390.8g distillage, and productivity is
92.5%.
The navel orange essential oil obtained with embodiment 4 is as sample, and bacteriostasis efficacy research is as follows:
1) bacteriostatic experiment strain: escherichia coli, staphylococcus aureus, yeast, bacillus subtilis, all strains are equal
Purchased from Chinese microorganism strain preservation center.
2) evaluation criteria of bacteriostatic activity: antibacterial circle diameter is extreme sensitivity more than 20mm, is that height is quick during 15-20mm
Sense, is medium sensitivity during 10-15mm, is less sensitive during 7-9mm, be insensitive without inhibition zone person.
3) bacteriostatic experiment method:
(1) bacterium to be measured plate method of scoring being activated on solid medium, picking list bacterium colony accesses in fluid medium
Incubated overnight, then carries out 10 times of serial dilutions by bacterium solution, and antibacterial uses colony counting method, and yeast uses microscope directly to count
Method surveys thalline, and each bacterium colony liquid concentration being adjusted to is the bacteria suspension of 1 × 106CFU/mL, and various bacteria suspensions to be measured are respectively taken 0.15mL
Even spread on corresponding solid medium, makes containing bacterium flat board.The aseptic filter of circle of 4 5mm it is pasted in each plate
The scraps of paper, and be allowed to flatten.Dripping 5 μ L quintessence oils on 3 filter papers of each plane ware respectively, another filter paper is as right
According to, each strain parallel assay 3 times.Wherein staphylococcus aureus and escherichia coli are observed after cultivating 24h at 37 DEG C
Record, yeast, bacillus subtilis carry out observed and recorded, measure the diameter of inhibition zone, be averaged after cultivating 48h at 28 DEG C
Value, evaluates the antibacterial ability of quintessence oil with the diameter of inhibition zone.
(2) navel orange essential oil solvent dimethyl sulfoxide (DMSO) is diluted to final concentration 12.5,6.25,3.125,1.56,
0.78,0.39 μ L/mL, takes 5 μ L diluents and instills on filter paper, do blank with DMSO and sterilized water.Same golden yellow Portugal
Grape coccus and escherichia coli carry out observed and recorded after cultivating 24h at 37 DEG C, yeast, bacillus subtilis are cultivated at 28 DEG C
Carrying out observed and recorded after 48h, observe the growing state of thalline, each essential oil concentration gradient makees 3 groups of parallel tests, with matched group ratio
Relatively, observe inhibition zone size, be its minimum inhibitory concentration with the minimum essential oil concentration that minimum antibacterial circle diameter is corresponding.
4, bacteriostatic experiment result:
(1) navel orange essential oil antibacterial circle diameter:
(2) navel orange essential oil minimum inhibitory concentration to test strain
5, bacteriostatic experiment conclusion:
(1) after molecular distillation purifies, the light phase component of navel orange essential oil is to yeast and bacillus subtilis extreme sensitivity, to greatly
Enterobacteria and staphylococcus aureus are extremely sensitive.
(2) the Citrus sinensis Osbeck cold pressing quintessence oil crude oil purified without molecular distillation is to yeast, bacillus subtilis, escherichia coli
Little Mlc 1.56 μ L/mL, the MIC to staphylococcus aureus is 3.125 μ L/mL；And after molecular distillation purifies
Navel orange essential oil component bacteriostatic activity is greatly improved, and saccharomycetic MIC value is wherein respectively 0.39 μ L/mL, and cold pressed orange oil phase
Specific activity improves 3 times；Colibacillary bacteriostatic activity is improve 1 times.
As can be seen here, navel orange essential oil molecular distillation component to escherichia coli, bacillus subtilis, staphylococcus aureus and
Saccharomycetic have good inhibiting effect, and it is substantially better than antibacterial to the bacteriostatic activity of fungus, and molecular distillation technique can improve
The bacteriostatic activity of essential oil component.
The above, the only present invention preferably detailed description of the invention, but protection scope of the present invention is not limited thereto,
Any those familiar with the art in the technical scope that the invention discloses, according to technical scheme and
Inventive concept equivalent or change in addition, all should contain within protection scope of the present invention.
Claims (3)
1. the preparation method of the navel orange essential oil molecular distillation component having bacteriostasis efficacy, it is characterised in that specifically comprise the following steps that
1) quintessence oil of colding pressing is loaded in the feeding bottle of molecular distillation apparatus, open cold condenser；
2) after system cooling, set vacuum, after pressure stability, set vapo(u)rizing temperature；
3) after vacuum and temperature all reach setting value, regulate knifing rotating speed, open inlet valve, control mass flow, carry out point
Son distillation, collects and distillates component.
The preparation method of a kind of navel orange essential oil molecular distillation component having bacteriostasis efficacy the most according to claim 1, it is special
Levy and be, described step 2) in, vacuum is 8.0-12.0Torr, vapo(u)rizing temperature is 50.0-60.0 DEG C.
The preparation method of a kind of navel orange essential oil molecular distillation component having bacteriostasis efficacy the most according to claim 1, it is special
Levy and be, described step 3) in, knifing rotating speed is 300-350r/min, mass flow is 2.5-3.5mL/min.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106867676A (en) * | 2017-04-21 | 2017-06-20 | 贺州学院 | A kind of extracting method of navel orange pericarp essential oil |
| CN106978257A (en) * | 2017-05-12 | 2017-07-25 | 贺州学院 | The extracting method of navel orange pericarp essential oil |
| CN108467787A (en) * | 2018-05-07 | 2018-08-31 | 上海应用技术大学 | A kind of process for purifying distillation of cold press fingered citron essential oil molecule |
| CN109722342A (en) * | 2019-02-20 | 2019-05-07 | 上海应用技术大学 | A method of using two-stage molecular distillation Extracting And Purifying On Rose Oil |
| CN111265435A (en) * | 2020-03-24 | 2020-06-12 | 上海应用技术大学 | No-clean bacteriostatic hand sanitizer containing navel orange essential oil and preparation method thereof |
| CN111592935A (en) * | 2020-04-26 | 2020-08-28 | 浙江师范大学 | Method for enriching antibacterial components of cinnamomum camphora essential oil |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106867676A (en) * | 2017-04-21 | 2017-06-20 | 贺州学院 | A kind of extracting method of navel orange pericarp essential oil |
| CN106978257A (en) * | 2017-05-12 | 2017-07-25 | 贺州学院 | The extracting method of navel orange pericarp essential oil |
| CN108467787A (en) * | 2018-05-07 | 2018-08-31 | 上海应用技术大学 | A kind of process for purifying distillation of cold press fingered citron essential oil molecule |
| CN109722342A (en) * | 2019-02-20 | 2019-05-07 | 上海应用技术大学 | A method of using two-stage molecular distillation Extracting And Purifying On Rose Oil |
| CN111265435A (en) * | 2020-03-24 | 2020-06-12 | 上海应用技术大学 | No-clean bacteriostatic hand sanitizer containing navel orange essential oil and preparation method thereof |
| CN111592935A (en) * | 2020-04-26 | 2020-08-28 | 浙江师范大学 | Method for enriching antibacterial components of cinnamomum camphora essential oil |
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Application publication date: 20170111 |