CN111621365A - Zanthoxylum essential oil and extraction process thereof - Google Patents

Zanthoxylum essential oil and extraction process thereof Download PDF

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Publication number
CN111621365A
CN111621365A CN202010499675.0A CN202010499675A CN111621365A CN 111621365 A CN111621365 A CN 111621365A CN 202010499675 A CN202010499675 A CN 202010499675A CN 111621365 A CN111621365 A CN 111621365A
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pepper
extraction
essential oil
oil
extraction process
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王佐军
任超
李�浩
凡彩凤
张峻川
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Chengdu Taylor Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/025Recovery by solvent extraction
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/022Refining
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/027Recovery of volatiles by distillation or stripping

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Fats And Perfumes (AREA)
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Abstract

The invention discloses a pepper essential oil and an extraction process thereof. Removing impurities from fresh pepper, repeatedly freezing and thawing for 2-3 times, naturally standing to recover room temperature, and crushing the pepper into powder to obtain pepper powder; distilling and roughly extracting the pepper powder, separating distilled water to obtain an oily crude extract, and then finely extracting the oily extract, wherein subcritical fluid extraction is assisted for finely extracted oil to obtain semi-finished essential oil; and finally, separating the semi-finished essential oil, adsorbing by using an adsorbent, and filtering to obtain the pepper essential oil. The pepper essential oil prepared by the method effectively reserves flavor substances in pepper, can prevent the passivation or inactivation of active substances in pepper, and also can reserve the natural fragrance of grease to a great extent by performing freeze thawing treatment and then crushing on pepper, so that the pepper essential oil has more flavor.

Description

Zanthoxylum essential oil and extraction process thereof
Technical Field
The invention belongs to the technical field of deep processing of food ingredients, and particularly relates to pepper essential oil and an extraction process thereof, and pepper essential oil prepared by the process, and particularly relates to pepper essential oil prepared by a subcritical extraction process.
Background
Chinese prickly ash (zanthoxylum bungeanum Maxim.)Zanthoxylum bungeanum Maxim.) Is a fruit of deciduous small trees of Zanthoxylum of Rutaceae, and is also called as pericarpium zanthoxyli because of wide planting in Shaanchuan area of China. As one of the eight major seasonings, the pepper is pungent and numb in taste and unique in fragrance, so that the pepper is widely applied to food cooking, and the pepper is commonly used in the Sichuan dish to enhance the fragrance and improve the taste, so that the taste of the dish is improved. The zanthoxylum essential oil can be obtained by extracting and processing zanthoxylum, the ingredients of the zanthoxylum essential oil mainly comprise limonene, zanthoxylum alkene, zanthoxylum amide, phytosterol, unsaturated organic acid and the like, the substances are the main sources of the fragrance of the zanthoxylum, can be used in the food industry as high-grade seasonings and spices, and meanwhile, researches show that the zanthoxylum essential oil has stronger pharmacological activity, such as the efficacies of killing insects, sterilizing, relieving pain and stopping itching.
For a long time, the main product form of the pepper is pepper granules or pepper powder, the application range is limited, and the transportation and preservation cost is higher. The essential oil of the pepper is a secondary metabolite of the pepper and also a main source of the fragrance of the pepper. As a deep-processing product of the zanthoxylum, the zanthoxylum essential oil is not only an important food additive and seasoning, but also has stronger pharmacological activity, such as disinsection, bacteriostasis, anti-inflammation, analgesia, anti-tumor, antioxidation, platelet aggregation inhibition and the like, has larger application prospect in the fields of medicine, cosmetics, agriculture and the like, and has wide development and utilization values. The essential oil and the numb element in the pricklyash peel essential oil are main components generating the special flavor of the pricklyash peel, the essential oil is composed of various compounds such as olefin, alcohol, ketone, aldehyde and the like, and has better lipid solubility, while the main component of the numb element in the pricklyash peel is an amide compound, is soluble in hot ethanol and benzene, is slightly soluble in water, is insoluble in petroleum ether, mainly exists in the peel of the pricklyash peel, and also has a small part existing in the flower and the leaf of the pricklyash peel.
The huge development prospect of the zanthoxylum essential oil makes the extraction of the product become a research hotspot in the food and medicine industry at the present stage. The related extraction method of the pepper essential oil relates to a squeezing method, a steam distillation method, a leaching method, a microwave method and the like, wherein the squeezing method, the steam distillation method and the leaching method have the defects of low oil yield or high energy consumption, so that the extraction method is limited in the industrial amplification process; in addition, although the main components of the pepper essential oil obtained by the methods are approximately same, the extraction efficiency, chemical components and content of the final essential oil have certain differences due to the difference of the extraction methods and the difference of research materials, and partial methods have low extraction efficiency, incomplete effective components and great difference of product flavor and natural pepper. The steam distillation method is also reported for extracting the components of the pepper, but the method has higher operation temperature and large energy consumption, can cause loss or damage of characteristic fragrance and numb taste components in the pepper to different degrees, and has lower extraction efficiency on fat-soluble components in the raw materials and lower resource utilization rate. The organic solvent method has problems of organic solvent residue and loss of beneficial components, and thus is discouraged. The supercritical and subcritical extraction technology is a novel oil extraction technology, and has the advantages of no solvent residue, high extraction rate, beneficial component protection and the like, such as supercritical carbon dioxide extraction technology and subcritical propane extraction technology. The supercritical carbon dioxide extraction technology refers to the advantages of simple extraction process operation, short time consumption, high product quality and the like by using carbon dioxide as an extraction solvent to extract grease under a supercritical condition. But the operation process adopts high pressure which is usually more than or equal to 27MPa, the requirement on equipment is high, and the investment cost is high; in addition, the solubility of the oil in carbon dioxide is low, and the extraction efficiency of the oil is limited and is about 81%; and heat energy is required to evaporate the solvent from the oil, which is costly to operate.
The subcritical fluid extraction technology is a technical means of efficiently, quickly and simply separating a material into a target product by taking subcritical fluid as an extraction solvent under the condition of being lower than the critical temperature and the critical pressure of the subcritical fluid, and the technology has the advantages of energy conservation, low operation cost and the like. At present, the subcritical extraction technology is generally applied to the extraction, separation and purification processes of natural products such as natural pigments, vegetable essential oils, grease and the like. However, the crude prickly ash seed oil contains a large amount of unsaturated fatty acid, the acid value and the wax value are both high, the acid value is generally 40-60 mg KOH/g, the mouthfeel is poor, the cost of the subsequent processing technology is high, and the oil yield of the finished oil is low.
Chinese patent application No. 201010134174.9 discloses a method for extracting pepper seed oil from pepper seeds, which utilizes subcritical technology to extract crude pepper seed oil, but the crude pepper seed oil extracted by the method is subjected to simple centrifugation treatment, and the obtained oil product does not meet the standard of edible oil. The Chinese patent with the application number of 201910761277.9 discloses a processing technology of low-acid-value zanthoxylum seed oil, the method improves the oil yield by utilizing a secondary deacidification mode after subcritical extraction of crude oil, reduces the process cost, but the problem that flavor substances are volatilized and depleted at high temperature in the subsequent refining process is still not solved, although the prepared zanthoxylum seed oil can reach the national edible oil standard, the sense organ enjoyment of consumers is influenced by the loss of the flavor substances, particularly various aromatic essential oils such as beta-phellandrene, butanone, aristolocene, beta-myrcene and the like with rich fragrance.
How to improve the prior art of extracting the zanthoxylum essential oil by subcritical fluid to obtain the preparation method of the zanthoxylum essential oil with low cost, high oil yield, special flavor of the zanthoxylum essential oil and strong operability is a technical problem to be solved at present.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention mainly aims to provide an extraction process of pepper essential oil. The method can simultaneously extract the effective characteristic components such as volatile oil, numb taste essence and the like in the pepper, furthest reserve the special fragrance and numb taste of the pepper, and effectively avoid resource waste. The invention also aims to provide the zanthoxylum essential oil obtained by the method.
The purpose of the invention is realized by the following scheme:
the extraction process of the pepper essential oil is characterized by comprising the following steps of:
(1) pretreatment: removing impurities from fresh pepper, repeatedly freezing and thawing for 2-3 times, naturally standing to recover room temperature, and crushing the pepper into powder to obtain pepper powder for later use;
(2) coarse extraction: distilling and roughly extracting the pepper powder, and separating distilled water to obtain an oily crude extract for later use;
(3) fine extraction: carrying out fine extraction on the oily crude extract to obtain fine extracted grease for later use;
(4) subcritical extraction: performing subcritical fluid extraction on the refined extracted oil to obtain semi-finished essential oil;
(5) refining: and separating the semi-finished essential oil, finally adsorbing by using an adsorbent, and filtering to obtain the zanthoxylum essential oil.
Further, the freeze-thaw conditions in step (1) are as follows: freezing for 6-8 min at-12 to-6 ℃, and unfreezing at normal temperature.
Further, the distillation conditions in the step (2) are as follows: extracting under reflux for 3-4 h by using water vapor, collecting distillate, cooling to room temperature, separating in an oil-water separator, drying and separating an oil layer to obtain an oily crude extract.
Further, the fine extraction conditions in the step (3) are as follows: distilling at 60-80 ℃ and under the vacuum degree of 40-80 mbar, the flow rate of 0.5-1.5 ml/ml and the film scraping rotation speed of 60-300 r/min, cooling the distilled product after the distillation is finished, and separating light components to obtain the refined extracted oil.
Further, the cooling temperature is minus 8 ℃ to minus 2 ℃.
Further, the subcritical extraction conditions in step (4) are as follows: extracting for 3-5 times at 35-55 ℃ and 0.75-0.95 Mpa for 40-60 min each time.
Further, the separation conditions in the step (5) are as follows: the temperature is 48-55 ℃, and the pressure is 8-10 Mpa.
Further, the adsorption conditions in the step (5) are as follows: adsorbing for 2-4 times at 48-56 deg.C for 30min each time.
Further, the adsorbent is a mixture of diatomite and bentonite.
The invention also discloses the zanthoxylum essential oil prepared by any one of the extraction processes.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the invention has simple operation, good stability, low design and manufacturing cost and operation cost of equipment and easy realization of large-scale production.
2. The pepper essential oil prepared by the invention effectively retains flavor substances in pepper, the whole process effectively prevents the passivation or inactivation of active substances in pepper, and the process can effectively prolong the preservation time of pepper essential oil and reduce the influence of heating treatment on food quality.
3. According to the invention, the pepper is firstly subjected to freeze thawing treatment and then crushed, so that the release of flavor substances in pepper cells into an extraction medium is accelerated, and the flavor substances are quickly volatilized when the pepper is subjected to later-stage distillation; after the coarse extraction → the fine extraction → the subcritical extraction → the refining treatment, the alkaloid yield, the essential oil yield, the volatile oil extraction rate and the numb element extraction rate of the pepper essential oil can be effectively improved, the natural fragrance of the grease is kept to the maximum extent, and the pepper essential oil has more flavor.
4. According to the invention, various additives and organic solvents are not used, compared with the prior art in which organic solvents are used for extraction, the original fragrance of the volatile oil is greatly retained, the obtained pepper volatile oil has more abundant fragrance, and because no organic solvent is used, the subsequent solvent removal treatment step is omitted, the treatment is more convenient, the obtained volatile oil is not subjected to residual organic solvents, and the method is safer and pollution-free.
It should be noted that the technical effect of the present invention is the result of the mutual cooperation and interaction of the process steps and parameters, and is not the superposition of simple processes, and the effect produced by the organic combination of the processes far exceeds the superposition of the functions and effects of each single process, so the present invention has better advancement and practicability.
Drawings
Fig. 1 shows the results of alkaloid yield and essential oil yield of the zanthoxylum oil prepared in example 1 and comparative examples 1-3, and the legends in fig. 1 are, from left to right, example 1, comparative example 2 and comparative example 3.
FIG. 2 shows the results of the volatile oil extraction rate and the sesamin extraction rate of the essential oils of Zanthoxylum bungeanum obtained in example 1 and comparative examples 1-3, and the legends in FIG. 2 are, from left to right, example 1, comparative example 2 and comparative example 3.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
Extraction process of pepper essential oil
(1) Pretreatment: removing impurities from fresh pepper, and repeatedly freezing and thawing for 2 times, wherein the freezing and thawing conditions are as follows: freezing at-9 deg.C for 7min, and thawing at normal temperature; then naturally standing to restore the room temperature, and crushing the pepper into powder to obtain pepper powder for later use;
(2) coarse extraction: distilling and roughly extracting the pepper powder, wherein the distillation conditions are as follows: extracting under reflux with water vapor for 3.5 hr, collecting distillate, cooling to room temperature, separating in oil-water separator, drying oil layer, and separating distilled water to obtain oily crude extract;
(3) fine extraction: finely extracting the oily crude extract, distilling at 70 deg.C, vacuum degree of 60 mbar, flow rate of 1ml/ml, and knifing rotation speed of 180r/min, cooling at-5 deg.C after distillation, and separating light components to obtain finely extracted oil;
(4) subcritical extraction: performing subcritical fluid extraction on the refined oil, and extracting at 45 deg.C and 0.85Mpa for 50min for 4 times to obtain semi-finished product of essential oil;
(5) refining: separating the semi-finished essential oil at 51 deg.C under 9Mpa, adsorbing at 52 deg.C for 3 times (30 min each time) with adsorbent of mixture of diatomaceous earth and bentonite, and filtering to obtain fructus Zanthoxyli essential oil.
Example 2
Extraction process of pepper essential oil
(1) Pretreatment: removing impurities from fresh pepper, and repeatedly freezing and thawing for 2 times, wherein the freezing and thawing conditions are as follows: freezing at-12 deg.C for 6min, and thawing at normal temperature; then naturally standing to restore the room temperature, and crushing the pepper into powder to obtain pepper powder for later use;
(2) coarse extraction: distilling and roughly extracting the pepper powder, wherein the distillation conditions are as follows: extracting under reflux with water vapor for 3 hr, collecting distillate, cooling to room temperature, separating in oil-water separator, drying oil layer, and separating distilled water to obtain oily crude extract;
(3) fine extraction: finely extracting the oily crude extract, distilling at 60 deg.C, vacuum degree of 40mbar, flow rate of 0.5ml/ml and knifing rotation speed of 60r/min, cooling at-8 deg.C after distillation, and separating light components to obtain finely extracted oil;
(4) subcritical extraction: performing subcritical fluid extraction on the refined oil, and extracting at 35 deg.C and 0.75Mpa for 3 times, each for 40min to obtain semi-finished product of essential oil;
(5) refining: separating the semi-finished essential oil at 48 deg.C under 8Mpa, adsorbing at 48 deg.C for 2 times (30 min each time) with adsorbent of mixture of diatomaceous earth and bentonite, and filtering to obtain fructus Zanthoxyli essential oil.
Example 3
Extraction process of pepper essential oil
(1) Pretreatment: removing impurities from fresh pepper, and repeatedly freezing and thawing for 3 times, wherein the freezing and thawing conditions are as follows: freezing at-6 deg.C for 8min, and thawing at normal temperature; then naturally standing to restore the room temperature, and crushing the pepper into powder to obtain pepper powder for later use;
(2) coarse extraction: distilling and roughly extracting the pepper powder, wherein the distillation conditions are as follows: extracting under reflux with water vapor for 4 hr, collecting distillate, cooling to room temperature, separating in oil-water separator, drying oil layer, and separating distilled water to obtain oily crude extract;
(3) fine extraction: finely extracting the oily crude extract, distilling at 80 deg.C, vacuum degree of 80 mbar, flow rate of 1.5ml/ml, and knifing rotation speed of 300 r/min, cooling at-2 deg.C after distillation, and separating light components to obtain finely extracted oil;
(4) subcritical extraction: performing subcritical fluid extraction on the refined oil, and extracting at 55 deg.C and 0.95Mpa for 60min for 5 times to obtain semi-finished product of essential oil;
(5) refining: separating the semi-finished essential oil at 55 deg.C under 10Mpa, adsorbing at 56 deg.C for 4 times (30 min each time) with adsorbent of mixture of diatomaceous earth and bentonite, and filtering to obtain fructus Zanthoxyli essential oil.
Comparative example 1
Compared with example 1, the repeated freeze thawing operation is eliminated, and the rest steps are the same as example 1
(1) Pretreatment: crushing fresh pepper into powder to obtain pepper powder for later use;
(2) coarse extraction: distilling and roughly extracting the pepper powder, wherein the distillation conditions are as follows: extracting under reflux with water vapor for 3.5 hr, collecting distillate, cooling to room temperature, separating in oil-water separator, drying oil layer, and separating distilled water to obtain oily crude extract;
(3) fine extraction: finely extracting the oily crude extract, distilling at 70 deg.C, vacuum degree of 60 mbar, flow rate of 1ml/ml, and knifing rotation speed of 180r/min, cooling at-5 deg.C after distillation, and separating light components to obtain finely extracted oil;
(4) subcritical extraction: performing subcritical fluid extraction on the refined oil, and extracting at 45 deg.C and 0.85Mpa for 50min for 4 times to obtain semi-finished product of essential oil;
(5) refining: separating the semi-finished essential oil at 51 deg.C under 9Mpa, adsorbing at 52 deg.C for 3 times (30 min each time) with adsorbent of mixture of diatomaceous earth and bentonite, and filtering to obtain fructus Zanthoxyli essential oil.
Comparative example 2
Compared with the operation of eliminating the rough extraction and the fine extraction in the embodiment 1, the rest steps are the same as the embodiment 1
(1) Pretreatment: removing impurities from fresh pepper, and repeatedly freezing and thawing for 2 times, wherein the freezing and thawing conditions are as follows: freezing at-9 deg.C for 7min, and thawing at normal temperature; then naturally standing to restore the room temperature, and crushing the pepper into powder to obtain pepper powder for later use;
(2) subcritical extraction: performing subcritical fluid extraction on fructus Zanthoxyli powder, and extracting at 45 deg.C and 0.85Mpa for 50min each time to obtain semi-finished essential oil;
(3) refining: separating the semi-finished essential oil at 51 deg.C under 9Mpa, adsorbing at 52 deg.C for 3 times (30 min each time) with adsorbent of mixture of diatomaceous earth and bentonite, and filtering to obtain fructus Zanthoxyli essential oil.
Comparative example 3
The purification operation is omitted compared with the operation of example 1, and the rest steps are the same as the operation of example 1
(1) Pretreatment: removing impurities from fresh pepper, and repeatedly freezing and thawing for 2 times, wherein the freezing and thawing conditions are as follows: freezing at-9 deg.C for 7min, and thawing at normal temperature; then naturally standing to restore the room temperature, and crushing the pepper into powder to obtain pepper powder for later use;
(2) coarse extraction: distilling and roughly extracting the pepper powder, wherein the distillation conditions are as follows: extracting under reflux with water vapor for 3.5 hr, collecting distillate, cooling to room temperature, separating in oil-water separator, drying oil layer, and separating distilled water to obtain oily crude extract;
(3) fine extraction: finely extracting the oily crude extract, distilling at 70 deg.C, vacuum degree of 60 mbar, flow rate of 1ml/ml, and knifing rotation speed of 180r/min, cooling at-5 deg.C after distillation, and separating light components to obtain finely extracted oil;
(4) subcritical extraction: performing subcritical fluid extraction on the refined oil, and extracting at 45 deg.C and 0.85Mpa for 50min for 4 times to obtain pericarpium Zanthoxyli essential oil.
Test example 1
The zanthoxylum essential oil prepared in example 1 and comparative examples 1-3 is selected to be subjected to alkaloid yield and essential oil yield determination, and the details are shown in figure 1 (each legend in figure 1 is example 1, comparative example 2 and comparative example 3 from left to right in sequence). The essential oil of the zanthoxylum bungeanum prepared in example 1 and comparative examples 1-3 is selected to be subjected to volatile oil extraction rate and sesamin extraction rate measurement, and the specific situation is shown in figure 2 (each figure in figure 2 is that example 1, comparative example 2 and comparative example 3 are sequentially arranged from left to right).
According to the results shown in fig. 1, the yield of the alkaloid and the yield of the essential oil of the zanthoxylum bungeanum bunge prepared by the process are both obviously higher than those of the essential oil in the comparative examples 1-3 (P is less than 0.05), and the difference has statistical significance. According to the results shown in fig. 2, the extraction rate of the essential oil of the zanthoxylum bungeanum prepared by the process is obviously higher than that of the comparative examples 1-3 (P is less than 0.05), and the difference has statistical significance.
Therefore, after the coarse extraction → the fine extraction → the subcritical extraction → the refining treatment, the flavor substances in the pepper are effectively retained, and the passivation or inactivation of the active substances in the pepper is prevented. Firstly, the pepper is subjected to freeze thawing treatment and then crushed, so that the release of flavor substances in pepper cells into an extraction medium is accelerated, and the flavor substances are quickly volatilized when the pepper is subjected to later-stage distillation; can effectively improve the alkaloid yield, the essential oil yield, the volatile oil extraction rate and the numb element extraction rate of the zanthoxylum essential oil, and furthest reserve the natural fragrance of oil, so that the zanthoxylum essential oil has more flavor.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.

Claims (10)

1. The extraction process of the pepper essential oil is characterized by comprising the following steps of:
(1) pretreatment: removing impurities from fresh pepper, repeatedly freezing and thawing for 2-3 times, naturally standing to recover room temperature, and crushing the pepper into powder to obtain pepper powder for later use;
(2) coarse extraction: distilling and roughly extracting the pepper powder, and separating distilled water to obtain an oily crude extract for later use;
(3) fine extraction: carrying out fine extraction on the oily crude extract to obtain fine extracted grease for later use;
(4) subcritical extraction: performing subcritical fluid extraction on the refined extracted oil to obtain semi-finished essential oil;
(5) refining: and separating the semi-finished essential oil, finally adsorbing by using an adsorbent, and filtering to obtain the zanthoxylum essential oil.
2. The extraction process according to claim 1, wherein the freeze-thaw conditions of step (1) are: freezing for 6-8 min at-12 to-6 ℃, and unfreezing at normal temperature.
3. The extraction process according to claim 1, wherein the distillation conditions of step (2) are: extracting under reflux for 3-4 h by using water vapor, collecting distillate, cooling to room temperature, separating in an oil-water separator, drying and separating an oil layer to obtain an oily crude extract.
4. The extraction process according to claim 1, wherein the fine extraction conditions of step (3) are: distilling at 60-80 ℃ and under the vacuum degree of 40-80 mbar, the flow rate of 0.5-1.5 ml/ml and the film scraping rotation speed of 60-300 r/min, cooling the distilled product after the distillation is finished, and separating light components to obtain the refined extracted oil.
5. The extraction process according to claim 4, wherein the cooling temperature is from-8 ℃ to-2 ℃.
6. The extraction process according to claim 1, wherein the subcritical extraction conditions of step (4) are: extracting for 3-5 times at 35-55 ℃ and 0.75-0.95 Mpa for 40-60 min each time.
7. The extraction process according to claim 1, wherein the separation conditions of step (5) are: the temperature is 48-55 ℃, and the pressure is 8-10 Mpa.
8. The extraction process according to claim 1, wherein the adsorption conditions of step (5) are: adsorbing for 2-4 times at 48-56 deg.C for 30min each time.
9. The extraction process according to claim 8, wherein the adsorbent is a mixture of diatomaceous earth and bentonite.
10. A zanthoxylum essential oil prepared by any one of the extraction processes according to claims 1 to 9.
CN202010499675.0A 2020-06-04 2020-06-04 Zanthoxylum essential oil and extraction process thereof Pending CN111621365A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113355164A (en) * 2020-12-17 2021-09-07 贵州玄德生物科技股份有限公司 Separation and purification device and method for pepper aromatic substances and spicy substances
CN113528244A (en) * 2021-06-17 2021-10-22 罗静 Method for removing impurities from plant essential oil for cosmetics
CN114958487A (en) * 2022-06-15 2022-08-30 银谷芳香科技有限公司 Industrial extraction process method of Roman chamomile oil

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