Method for extracting pepper essential oil by ultrasonic-assisted simultaneous distillation and extraction

Abstract

The invention belongs to the technical field of extraction, and discloses a method for extracting pepper essential oil through ultrasonic-assisted simultaneous distillation extraction, the pepper essential oil is extracted through the ultrasonic-assisted simultaneous distillation extraction method, the raw materials are cheap and easy to obtain, the cost is low, the process is simple, the reaction conditions are mild, and the method is suitable for industrial production. The energy consumption is low. According to the Chinese prickly ash essential oil extraction method provided by the invention, the ultrasonic cavitation effect and the simultaneous distillation and extraction are synergistic, so that the extraction rate of the Chinese prickly ash essential oil is improved, and the product is high in yield and good in quality. According to the pepper essential oil extraction method provided by the invention, the equipment universality is high, the used ultrasonic cleaner, electric jacket, rotary evaporator and the like are conventional laboratory or industrial equipment, special devices do not need to be customized, and the industrial popularization cost is reduced.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of extraction and extraction, and relates to a method for extracting Zanthoxylum bungeanum essential oil by ultrasonic-assisted simultaneous distillation extraction. BACKGROUND

[0002] The mainstream extraction process of Zanthoxylum bungeanum essential oil has the following methods and limitations: the traditional steam distillation method has simple equipment and operation, low cost, and can avoid steam damage, but has low yield, long time consumption, and may cause loss of heat-sensitive components. Solvent extraction is widely used due to low price, wide source and mildness to heat-sensitive substances, but has problems such as solvent residue, large amount of reagent and poor environmental protection. The superhigh pressure extraction method has the advantages of short time, low energy consumption, less impurities and green environmental protection, but has high requirements for equipment and relatively complicated operation. The supercritical CO2 extraction method has high efficiency, short extraction time, no need for organic solvent, moderate temperature and high purity of essential oil, but has high equipment investment, high energy consumption and difficulty in recycling CO2, which limits its industrial scale application. The simultaneous distillation extraction method can simplify the steps, save the solvent and reduce the sample loss, but the high-temperature operation may cause distortion of aroma components. The microwave-assisted extraction method has low solvent consumption, less waste, short extraction time, and can be combined with other technologies to make up for the limitations, but has problems of uneven heating, microwave leakage and equipment maintenance cost. The ultrasonic-assisted extraction method has short time consumption, low energy consumption and high mass transfer efficiency, and is especially suitable for heat-sensitive and unstable compounds, but the safety of ultrasonic device and the attenuation factor are still the constraints. The enzyme-assisted extraction process is simple, has low energy consumption, little damage to effective components and good economic benefit, but its effect is greatly affected by external conditions such as temperature and pH.

[0003] The UAE-SDE technology is proposed to integrate the synergistic advantages of the two methods. Ultrasonic pretreatment can instantaneously break the cell wall of Zanthoxylum bungeanum through cavitation, release intracellular oil, and significantly increase the dissolution efficiency of essential oil precursors. SDE can capture the released volatile components in a closed system, and the volatile components can be quickly distilled with water vapor and condensed in situ with low-temperature extraction solvent to minimize the loss and oxidation risk of heat-sensitive components.

[0004] Through the above analysis, the problems and defects of the prior art are:

[0005] (1) The traditional extraction method has low yield of essential oil, and heat-sensitive components are easily lost;

[0006] (2) The problem of solvent residue is prominent, and the food safety cannot be guaranteed;

[0007] (3) The supercritical extraction equipment has high cost and is difficult to be applied on a large scale;

[0008] (4) Single ultrasonic extraction has low efficiency in capturing volatile components. SUMMARY

[0009] In view of the problems of the prior art, the present application provides a method for extracting pepper essential oil by ultrasonic-assisted simultaneous distillation and extraction, which is simple in process, high in efficiency, high in quality, low in cost, low in operation energy consumption and capable of being used on a large scale.

[0010] To achieve the above object, the present application is implemented by the following technical scheme: a method for extracting pepper essential oil by ultrasonic-assisted simultaneous distillation and extraction, comprising the following steps:

[0011] S1, crushing and screening the selected high-quality pepper and collecting the undersize as the extraction raw material;

[0012] S2, loading the extraction raw material into a round-bottom flask, mixing with distilled water according to a solid-liquid ratio of 1:15 g / ml, and then placing in an ultrasonic cleaner for ultrasonic treatment, so that the cell wall microscale is broken under the ultrasonic cavitation effect;

[0013] S3, connecting the raw material bottle and the solvent bottle after ultrasonic treatment into a simultaneous distillation and extraction device, and performing simultaneous distillation and extraction under the condition of maintaining the raw material bottle in a micro-boiling state and the solvent bottle in a stable evaporation state, for 2-3 hours, so as to realize the mass transfer of volatile aromatic components in the raw material;

[0014] S4, transferring the mixture obtained after extraction to a separatory funnel to separate from water, to obtain a petroleum ether-essential oil mixture;

[0015] S5, connecting the petroleum ether-essential oil mixture into a rotary evaporator for rotary evaporation, to obtain a light yellow transparent pepper essential oil.

[0016] Further, in the step S1, the high-quality pepper selected by hand and meeting the predetermined sensory and physical standards is first crushed by a shear-type crusher in an intermittent and low-speed operation mode. The core purpose of this operation is to destroy the macroscopic structure of the pepper by controllable mechanical force, while maximizing the integrity of the oil gland cells rich in essential oil inside, to avoid pre-loss of volatile components due to excessive crushing or instantaneous high temperature.

[0017] In the step S1, the crushed product is classified and screened through a 50-mesh standard screen, and the undersize with the best particle size uniformity passing through the screen is accurately collected as the raw material for this extraction. This pretreatment process accurately controls the particle size and specific surface area of the raw material, laying a crucial physical foundation for the uniform and efficient action of ultrasonic energy and solvent medium in the subsequent steps.

[0018] The ultrasonic treatment in step S2 opens the oil glands of the aromatic oil through cavitation effect, forms internal microchannel structure conducive to subsequent steam carrying volatile components, thereby reducing the internal diffusion resistance in the simultaneous distillation extraction process;

[0019] The ultrasonic treatment in step S2 precisely acts on the cell wall structure of the Zanthoxylum bungeanum raw material, selectively causes "micro-scale rupture" and "porous", thereby efficiently releasing the intracellularly wrapped oil gland contents and dispersing them in the water phase without causing significant thermal degradation, and prepares a high concentration of "precursor" for the subsequent simultaneous distillation extraction step.

[0020] In step S3, the device uses an asymmetric heating system: the raw material bottle is heated by an electric heating jacket to maintain its contents at a micro-boiling state, and the solvent bottle is controlled by a constant temperature water bath to ensure that petroleum ether is in a stable and continuous evaporation state.

[0021] In step S3, in this synergistic system, the pre-processed material in the raw material bottle can be efficiently penetrated by water vapor due to the internal microchannel network formed, and the released volatile essential oil components are carried out. At the same time, the petroleum ether vapor evaporated from the solvent bottle meets the water vapor and essential oil components in the middle of the device, and efficient mass transfer is completed at the gas-liquid interface, and the essential oil components are selectively extracted into the petroleum ether phase.

[0022] In step S3, this process lasts for 2 to 3 hours to ensure sufficient and complete mass transfer. The entire system is maintained at a low temperature of 10-20°C by circulating cooling water in the condensation section, aiming to achieve immediate condensation of the steam backflow, maximize the residence time of heat-sensitive components in the high-temperature zone, and thus ensure the authenticity of the essential oil aroma and the integrity of the components.

[0023] In step S3, under the synergistic conditions of micro-boiling in the raw material bottle and stable evaporation in the solvent bottle, water vapor is more easily introduced into the ultrasonic-broken tissue structure, realizing the enhancement of nonlinear migration of volatile components, to improve the actual extraction rate of essential oil and improve the phase separation behavior in the subsequent separation and rotary evaporation process.

[0024] In step S4, the separation process benefits from the optimization of the cell structure of the raw material by the previous ultrasonic pretreatment, and the content of resin macromolecules and hydrophilic impurities in the obtained extraction phase is significantly reduced, so that the oil-water interface is more clear and distinct, effectively avoiding the occurrence of emulsification. In the separation operation, the lower water phase is accurately discarded, and the upper clear petroleum ether-essential oil mixed solution is precisely collected and transferred to a dedicated rotary evaporation bottle for subsequent processing.

[0025] The optimization of parameter combination in step S5 aims to achieve efficient and rapid evaporation of petroleum ether while maximizing the avoidance of the escape or chemical structure destruction of heat-sensitive aromatic components in essential oil. The constant rotation of the rotary bottle forms a uniform film on the bottle wall, greatly increasing the evaporation surface area, thereby achieving efficient stripping of the solvent under low temperature and low pressure conditions.

[0026] Further, the selection conditions of high-quality Zanthoxylum bungeanum in S1 are as follows: uniform color and luster, emitting rich and pure pepper aroma, and the particles are full, oil cell is dense, opening rate is high, dryness is moderate, hand feeling is crisp, impurities are few, and there are no signs of mildew, insect damage, and rancid smell.

[0027] Further, the crushing in S1 is performed by using a crusher, and then 50 mesh standard sieve is selected for screening, to ensure uniformity of the raw material particles.

[0028] Further, the storage method in S1 is to store the obtained sample in a 4°C refrigerator.

[0029] Further, the ultrasonic treatment by the ultrasonic cleaner in S2 has a power of 200W, an ultrasonic temperature of 10-20°C, and an ultrasonic time of 1 hour, and the water level is preferably 2-3cm higher than the liquid level of the round-bottom flask.

[0030] Further, the solvent in the solvent bottle in S3 is petroleum ether (analytical pure, 60-90°C), and the solvent dosage is just enough to cover the raw material.

[0031] Further, the raw material bottle and the solvent bottle in S3 are respectively located on the left and right sides of the simultaneous distillation and extraction device. In the device, the position of the raw material bottle is lower than that of the solvent bottle.

[0032] Further, the heating devices of the raw material bottle and the solvent bottle in S3 are different. The raw material bottle is heated by an electric heating jacket, and the voltage of the electric heating jacket is set to 100-150V. The solvent bottle is heated by a water bath, and the water bath temperature is set to 80-90°C.

[0033] Further, the condenser tube of the simultaneous distillation and extraction device in S3 is connected to circulating cooling water to ensure that the condensation temperature is maintained at 10-20°C, ensuring efficient condensation of the steam.

[0034] Further, the method of separating the mixture from water in S4 is as follows: after the mixture in the collection bottle is cooled to room temperature, it is transferred to a separatory funnel, and is allowed to stand for 30-45 minutes. The oil and water are separated by their density difference, the lower water phase is discarded, and the upper petroleum ether-essential oil mixture is collected in a rotary evaporation bottle.

[0035] Further, the parameters of the rotary evaporator in S5 are set as follows: the rotation speed is 30-40 r / min, the water bath temperature is 40-50 DEG C, and the vacuum degree is 0.08-0.09 Mpa.

[0036] Further, the rotary evaporation time in S5 is 5-6 min, and the distillation process is observed in real time; when no obvious solvent drops out of the rotary evaporation bottle, the distillation is stopped.

[0037] The application has the following beneficial effects:

[0038] From the perspective of industrial application, the equipment used in the application is conventional experimental equipment, which does not need to be specially customized, and has good technical transplantability and large-scale potential. Through parameter optimization and process integration, the method significantly reduces the energy consumption and solvent consumption per unit output while maintaining high-quality product output, and has significant economic and environmental advantages, providing a feasible technical solution for the high-quality and large-scale production of Zanthoxylum bungeanum essential oil.

[0039] The Zanthoxylum bungeanum essential oil extraction method provided by the application uses the method of ultrasonic-assisted simultaneous distillation extraction to extract Zanthoxylum bungeanum essential oil, which is cheap and easy to obtain, has low cost, simple process, mild reaction conditions and low energy consumption.

[0040] The Zanthoxylum bungeanum essential oil extraction method provided by the application has the synergistic effect of ultrasonic cavitation and simultaneous distillation extraction, which improves the extraction rate of Zanthoxylum bungeanum essential oil, and the yield and quality of the product are high.

[0041] The Zanthoxylum bungeanum essential oil extraction method provided by the application has strong universality, and the ultrasonic cleaner, electric heating jacket, rotary evaporator and other equipment used are conventional laboratory or industrial equipment, without the need for special devices, reducing the cost of industrialization.

[0042] The Zanthoxylum bungeanum essential oil extraction method provided by the application has low solvent residue, and the petroleum ether is efficiently removed by a rotary evaporator, so that the solvent residue of the finished product is less than 10 mg / kg, meeting the safety standards of the food and pharmaceutical fields.

[0043] (1) The expected income and commercial value of the technical solution of the application after transformation are:

[0044] The core technical value of the application lies in achieving the best balance of efficiency, cost and quality through process innovation and equipment cooperation.

[0045] On the production side, the comprehensive cost is significantly reduced and the efficiency is improved:

[0046] Yield improvement directly reduces raw material cost: The data of the examples show that the yield of essential oil (8.37%) of the present application is improved by more than 40% compared with the traditional steam distillation method (5.96%). This means that to obtain the same yield of essential oil, a large amount of raw material can be saved, directly reducing the core raw material cost per unit of product.

[0047] Energy consumption and solvent cost control: Ultrasonic assistance shortens the dissolution time of active ingredients, reducing energy consumption for maintaining long-time distillation. At the same time, since simultaneous distillation extraction (SDE) is carried out in a closed system, the solvent (petroleum ether) can be efficiently recycled, combined with the optimization of the rotary evaporation step, the final solvent residue is very low (<10 mg / kg), reducing the solvent consumption and subsequent processing cost.

[0048] Light investment in equipment, easy to industrialize and replicate: The ultrasonic cleaning machine, electric heating jacket, rotary evaporator and other equipment used are mature and general laboratory or industrial equipment, without the need to invest in high-priced special customized equipment (such as supercritical CO2 extraction device), which greatly reduces the initial investment threshold and technical adaptation difficulty of enterprises, and is conducive to the rapid popularization and application of technology.

[0049] On the product side, create core competitiveness of high quality and high safety:

[0050] Sensory and functional ingredients are retained intact: Mild ultrasonic pretreatment (10-20°C) and subsequent efficient condensation capture (condensation temperature 10-20°C) in the SDE system maximize the prevention of the destruction and oxidation of heat-sensitive aroma ingredients, resulting in a light yellow and transparent essential oil with a rich and pure pepper and sesame aroma, superior to the product of traditional high-temperature methods.

[0051] Food safety is guaranteed: Strict solvent removal process ensures that the final product meets or even exceeds the relevant safety standards in the food and pharmaceutical fields, which provides a key access advantage for the product to enter the high-value health food, natural cosmetics and traditional Chinese medicine market.

[0052] On the market side, it has strong competitive barriers and potential for value chain extension:

[0053] This technical solution provides an efficient, green and scalable solution for the deep processing of Zanthoxylum bungeanum Maxim, which not only improves the added value of Zanthoxylum bungeanum Maxim raw materials and drives income growth on the planting side, but also provides stable and high-quality essential oil raw materials for downstream enterprises.

[0054] The expected revenue model is diverse, including technology licensing, production line cooperation, and direct sales of high-end essential oil products. Under the trend of natural and healthy consumption, the high-quality Zanthoxylum bungeanum Maxim essential oil produced by the present application has strong market competitiveness, broad business prospects, and a considerable investment return rate.

[0055] (2) The technical solution of the present application fills the technical gap in the industry at home and abroad:

[0056] There is a clear "technical gap" in the current extraction technology field of Chinese prickly ash essential oil: high efficiency extraction, high quality retention and low cost operation are difficult to balance.

[0057] Limitations of the existing technology:

[0058] Although the traditional method (steam distillation, solvent extraction) has lower cost, it has obvious shortcomings in yield and solvent residue.

[0059] Advanced methods (supercritical CO2, ultrahigh pressure extraction) may have advantages in quality and yield, but their high equipment cost and complex operation and maintenance will exclude many small and medium-sized enterprises, and the scale application is limited.

[0060] Although single ultrasonic assisted extraction can improve the dissolution efficiency of intracellular substances, it is insufficient in capturing volatile components, resulting in the inability to maximize the overall extraction efficiency.

[0061] The gap filled by the present application:

[0062] The present application first systematically integrates and optimizes ultrasonic pretreatment and simultaneous distillation extraction (SDE) technology, forming a complete and efficient technical closed loop. This is not just a simple superposition of two methods, but through specific process parameters (such as ultrasonic power 200W, solid-liquid ratio 1:15, and staged heating control), a synergistic effect of "1+1>2" is achieved:

[0063] Ultrasonic wave acts as a "wall-breaking pioneer": efficiently destroys the oil cell structure of Chinese prickly ash under mild conditions, and releases essential oil precursors.

[0064] The SDE system acts as a "capture network": distills and condenses the released volatile components in a closed environment to prevent their escape or degradation.

[0065] Therefore, the present application successfully fills the gap in the extraction technology of Chinese prickly ash essential oil suitable for large-scale production, with high yield and high quality, and controllable investment cost, providing a new solution with strong universality and excellent comprehensive performance for the industry.

[0066] (3) The technical solution of the present application solves the technical problems that people have been eager to solve but have failed to succeed:

[0067] This technical solution accurately solves the three core problems that have long plagued the industrial extraction of Chinese prickly ash essential oil:

[0068] Problem one: how to break through the "yield ceiling" without sacrificing quality?

[0069] Traditional dilemma: Higher yield often requires more severe conditions (such as higher temperature, longer time or stronger solvent), but this will also cause the destruction of heat-sensitive components and distortion of aroma.

[0070] The solution of the present application: The physical wall breaking is realized at the cell level by using the ultrasonic cavitation effect, which fundamentally improves the dissolution rate and degree of the target, and lays the foundation for high yield. The subsequent SDE process avoids the destruction of components by long-term high-temperature soaking through immediate capture, thereby improving the yield while ensuring the pure quality of essential oil.

[0071] Problem two: How to completely eliminate the safety hazards of solvent residues while ensuring extraction efficiency?

[0072] Traditional dilemma: Solvent extraction method inevitably faces the problem of solvent residue, affecting product safety.

[0073] The solution of the present application: The present application uses petroleum ether (60-90℃) with moderate boiling point range as the extraction solvent, which has good volatility. By optimizing the rotary evaporation parameters (40-50℃ water bath, 0.08-0.09Mpa vacuum degree), the solvent can be efficiently and completely removed within 5-6 minutes, reducing the residual amount to below 10mg / kg, and perfectly solving the contradiction between safety and extraction efficiency.

[0074] Problem three: How to make high-efficiency extraction technology get rid of the dependence on expensive and special equipment and realize large-scale popularization?

[0075] Traditional dilemma: Although supercritical extraction and other technologies are good, they are difficult to be widely popularized in the industry due to their "aristocratic" equipment properties.

[0076] The solution of the present application: The present application is based on the innovative combination and parameter optimization of conventional equipment, and constructs a set of high-efficiency extraction system. This enables the majority of small and medium-sized food and spice enterprises to upgrade their production processes without making revolutionary equipment investment, and fundamentally solves the industrialization problem of high-efficiency technology "applauding but not attending".

[0077] (4) The technical solution of the present application overcomes technical bias:

[0078] There are some inherent technical biases in the field, which hinder the combination of ultrasonic and SDE technology:

[0079] Bias one: It is believed that "although the cavitation effect of ultrasonic can help extraction, it may cause unnecessary component decomposition or change, which is not conducive to preserving the true aroma of natural products."

[0080] The invention overcomes: Through systematic experiments, a safe window of 200W power and low-temperature ultrasound of 10-20℃ is determined. Under this parameter, the main role of ultrasound is mechanical wall breaking rather than triggering violent chemical changes. The essential oil obtained in the example has rich and pure aroma, and the yield is significantly improved. The successful practice proves that under the optimized conditions, the ultrasound pretreatment has no adverse effect on the structure of the main components of the pepper essential oil, but rather better preserves the overall flavor profile by improving the extraction efficiency.

[0081] Bias two: believes that "simultaneous distillation extraction (SDE) is essentially a high-temperature process, which inevitably leads to the loss of heat-sensitive aroma components, and is not suitable for the preparation of high-end fragrances."

[0082] The invention overcomes: The invention resolves this bias through ingenious device design and temperature control. First, the raw material bottle is only kept in a slightly boiling state, not in a violent boiling state, reducing heat shock. Second, and most importantly, an efficient condensation system (condensation temperature 10-20℃) is set up, so that the volatile essential oil components distilled out can be condensed instantly, greatly shortening their residence time in the high-temperature gas phase, thereby effectively avoiding the destruction of heat-sensitive components and aroma distortion. This "front-end gentle wall breaking, back-end rapid condensation" synergistic design overcomes people's stereotyped impression of SDE technology as "not friendly to high temperature". BRIEF DESCRIPTION OF DRAWINGS

[0083] Figure 1 is the process flow chart of the method for extracting pepper essential oil by ultrasonic-assisted simultaneous distillation extraction provided by the embodiment of the invention.

[0084] Figure 2 is the process flow chart provided by the embodiment of the invention.

[0085] Figure 3 is the GC-MS thermodynamic analysis chart for comparison between the traditional water extraction method and the UAE-SDE method provided by the embodiment of the invention. DETAILED DESCRIPTION

[0086] To make the purpose, technical solutions and advantages of the embodiments of the invention clearer, the technical solutions in the embodiments of the invention will be described clearly and completely below. Obviously, the described embodiments are part of the embodiments of the invention, not all the embodiments. Based on the embodiments in the invention, all other embodiments obtained by those of ordinary skill in the art without creative labor fall within the scope of protection of the invention.

[0087] The present application realizes the two-stage mass transfer enhancement of volatile aromatic components in Chinese prickly ash by coupling ultrasonic pretreatment with simultaneous distillation extraction process. The ultrasonic treatment causes micro-scale rupture of cell walls, making the aromatic oil glands open and forming internal micro-channel structure conducive to subsequent steam removal. Compared with the traditional simultaneous distillation extraction process which only relies on heating steam to drive the migration of volatile components, the ultrasonic cavitation pretreatment of the present application significantly reduces the internal diffusion resistance, so that the raw material can quickly reach gas-liquid equilibrium under micro-boiling conditions, thereby shortening the extraction time and improving the actual extraction rate of essential oil.

[0088] Under the condition of maintaining stable evaporation of the solvent bottle, the bubbles generated by micro-boiling of the raw material bottle are more easily entered into the tissue rupture, thereby forming a synergistically enhanced steam migration channel, so that the rate of water vapor carrying volatile components is greatly improved, showing a significant nonlinear improvement effect. This effect is not taught in the comparative documents, and is a technical effect that cannot be expected by those skilled in the art.

[0089] In addition, the ultrasonic pretreatment also improves the phase separation behavior in the subsequent liquid separation and rotary evaporation steps, and the resin impurities in the essential oil are less, so that the product is light yellow and transparent, and the quality stability is significantly better than that of the method described in the comparative documents. Through the above-mentioned synergistic technical chain, the overall extraction efficiency, product purity and process stability of the present application are better than those of the prior art, and have obvious technical progress.

[0090] The technical solution of the present application realizes controllable rupture of cell wall structure by accurately controlling the power density and action time of the ultrasonic treatment stage, avoiding the dissolution of impurities caused by excessive crushing. In the simultaneous distillation extraction stage, by optimizing the heating mode and temperature parameters of the raw material bottle and the solvent bottle, a stable steam equilibrium system is established, ensuring efficient transfer and capture of volatile components. This process design not only improves the extraction efficiency of essential oil, but also effectively protects the chemical integrity of heat-sensitive components by reducing the process temperature and shortening the heating time.

[0091] The present application changes the migration path and mass transfer kinetics of volatile components at the molecular level through the systematic cooperation of ultrasonic pretreatment and simultaneous distillation extraction. Ultrasonic cavitation not only creates a physical mass transfer channel, but also reduces the energy barrier of essential oil components across the phase interface by changing the permeability of cell walls. This enables the essential oil components to transfer between phases with lower activation energy in the subsequent distillation process, thereby achieving a qualitative leap in extraction efficiency while maintaining the natural configuration of essential oil.

[0092] As shown in Figure 1 , Figure 2 , the method for extracting essential oil from Chinese prickly ash by ultrasonic-assisted simultaneous distillation extraction according to the present embodiment 1 comprises the following steps:

[0093] S1, the selected high-quality pepper is crushed, then sieved, and the undersize material is collected as the extraction raw material and stored in separate containers.

[0094] S2, 25 g of the treated raw material is loaded into a round-bottom flask, mixed with distilled water at a material-to-liquid ratio of 1:15 g / ml, and placed in an ultrasonic cleaner for ultrasonic treatment.

[0095] S3, the simultaneous distillation and extraction device is set up, the raw material flask and the solvent flask after ultrasonic treatment are connected to the device, the device is started, heating is started, the raw material flask is kept at a slight boil, and the solvent flask is kept at a stable evaporation state, simultaneous distillation and extraction is carried out, and the process lasts for 2 hours.

[0096] S4, after the extraction is completed, the collected mixture is transferred to a separatory funnel, and the mixture is separated from water.

[0097] S5, the separated petroleum ether-essential oil mixture is connected to a rotary evaporator for rotary evaporation, and then a light yellow transparent pepper essential oil is obtained.

[0098] The selection conditions of high-quality pepper in S1 are as follows: uniform and bright color, emitting a strong and pure pepper aroma, and the particles are full, oil cells are dense, opening rate is high, dryness is moderate, hand feeling is crisp, impurities are few, and there are no signs of mildew, insect damage, and rancid smell.

[0099] In S1, the crushing is performed using a crusher, and then a 50-mesh standard sieve is used for sieving to ensure uniform particle size of the raw material.

[0100] The storage method in S1 is to store the obtained sample in a 4℃ refrigerator.

[0101] In S2, the ultrasonic treatment by the ultrasonic cleaner is performed at a power of 200W, an ultrasonic temperature of 10℃, an ultrasonic time of 1 hour, and a water level of 3cm above the liquid level of the round-bottom flask.

[0102] In S3, the solvent in the solvent flask is petroleum ether (analytical pure, 60-90℃), and the solvent dosage is 50ml.

[0103] In S3, the raw material flask and the solvent flask are located on the left and right sides of the simultaneous distillation and extraction device respectively. In the device, the position of the raw material flask is lower than that of the solvent flask.

[0104] In S3, the heating devices of the raw material flask and the solvent flask are different. The raw material flask is heated by an electric heating jacket, and the voltage of the electric heating jacket is set to 150V. The solvent flask is heated by a water bath, and the water bath temperature is set to 90℃.

[0105] In S3, the condenser tube of the simultaneous distillation and extraction device is connected to circulating cooling water to ensure that the condensation temperature is maintained at 20℃, ensuring efficient condensation of the steam.

[0106] The method for separating the mixture from water in S4 is as follows: After the mixture in the collection bottle has cooled to room temperature, it is transferred to a separatory funnel and allowed to stand for 45 minutes. The oil and water are separated by density difference. The lower aqueous phase is discarded, and the upper petroleum ether-essential oil mixture is collected in a rotary evaporator flask.

[0107] The parameters of the rotary evaporator in S5 are set as follows: rotation speed 30 rpm / min, water bath temperature 40℃, and vacuum degree 0.09 MPa.

[0108] The rotary evaporation time in S5 is 5 minutes. During the distillation process, observe in real time and stop distillation when there is no obvious solvent dripping out of the rotary evaporation flask.

[0109] like Figure 1 , Figure 2 As shown in Example 2, a method for extracting Sichuan pepper essential oil using ultrasound-assisted simultaneous distillation includes the following steps:

[0110] S1. Crush the selected high-quality peppercorns, then sieve them, collect the sieved material as the extraction raw material, and package and store it.

[0111] S2. Put 25g of the processed raw material into a round-bottom flask, mix it with distilled water at a material-to-liquid ratio of 1:15g / ml, and place it in an ultrasonic cleaner for ultrasonic treatment.

[0112] S3. Set up the simultaneous distillation and extraction apparatus, connect the ultrasonically treated raw material bottle and solvent bottle into the apparatus, start the apparatus, start heating, maintain the raw material bottle at a slight boil and the solvent bottle at a stable evaporation state, and carry out simultaneous distillation and extraction for 2.5 hours.

[0113] S4. After extraction, transfer the collected mixture to a separatory funnel to separate the mixture from the water.

[0114] S5. The separated petroleum ether-essential oil mixture is fed into a rotary evaporator for rotary evaporation, and then a pale yellow transparent pepper essential oil is obtained.

[0115] The selection criteria for high-quality Sichuan peppercorns in S1 are: bright and uniform color, rich and pure Sichuan pepper aroma, plump grains, dense oil cells, high opening rate, moderate dryness, crispy feel, and very few impurities, ensuring no signs of spoilage such as mold, insect infestation, or rancidity.

[0116] In S1, the grinding process involves using a pulverizer, followed by sieving through a 50-mesh standard sieve to ensure uniform particle size.

[0117] The storage method in S1 is as follows: the obtained sample is stored in a refrigerator at 4°C.

[0118] The power of ultrasonic treatment in the ultrasonic cleaner in S2 is 200 W, the ultrasonic temperature is 10℃, and the ultrasonic time is 1 hour, and the water level is 3 cm higher than the liquid level of the round-bottom flask.

[0119] The solvent in the solvent bottle in S3 is petroleum ether (analytical pure, 60-90℃), and the solvent usage is 50 ml.

[0120] The raw material bottle and the solvent bottle in S3 are located on the left and right sides of the simultaneous distillation and extraction device respectively. In the device, the position of the raw material bottle is lower than that of the solvent bottle.

[0121] The heating devices of the raw material bottle and the solvent bottle in S3 are different. The raw material bottle is heated by an electric heating jacket, and the voltage of the electric heating jacket is set to 150 V. The solvent bottle is heated by a water bath, and the water bath temperature is set to 90℃.

[0122] The condenser tube of the simultaneous distillation and extraction device in S3 is connected to circulating cooling water to ensure that the condensation temperature is maintained at 20℃, ensuring efficient condensation of steam.

[0123] In S4, the mixture is separated from water by cooling the mixture in the collection bottle to room temperature, transferring it to a separatory funnel, standing for 45 minutes, and using the density difference between oil and water to achieve layering. The lower water phase is discarded, and the upper petroleum ether-essential oil mixture is collected in a rotary evaporation flask.

[0124] In S5, the parameters of the rotary evaporator are set as follows: rotation speed 30 rpm / min, water bath temperature 40℃, and vacuum degree 0.09 Mpa.

[0125] In S5, the rotary evaporation time is 5 min, and the distillation process is observed in real time. When there is no obvious solvent dripping from the rotary evaporation flask, stop the distillation.

[0126] As shown in Figure 1 , Figure 2 , the method for extracting Zanthoxylum bungeanum essential oil by ultrasonic-assisted simultaneous distillation and extraction in Embodiment 3 includes the following steps:

[0127] In S1, the selected high-quality Zanthoxylum bungeanum is crushed, then sieved, and the undersize material is collected as the extraction raw material and stored separately.

[0128] In S2, 25 g of the treated raw material is placed in a round-bottom flask, mixed with distilled water according to the solid-liquid ratio of 1:20 g / ml, and subjected to ultrasonic treatment in an ultrasonic cleaner.

[0129] In S3, the simultaneous distillation and extraction device is set up, the ultrasonic-treated raw material bottle and the solvent bottle are connected to the device, the device is started, heating is started, and the state of micro-boiling of the raw material bottle and stable evaporation of the solvent bottle is maintained, and simultaneous distillation and extraction is carried out for 2.5 hours.

[0130] S4, after extraction, the collected mixture was transferred to a separatory funnel, the mixture was separated from water.

[0131] S5, the separated petroleum ether-essential oil mixture was connected to a rotary evaporator for rotary evaporation, and a light yellow transparent Zanthoxylum oil was obtained.

[0132] The selection conditions of high-quality Zanthoxylum in S1 are as follows: uniform color, strong and pure pepper and sesame aroma, full particles, dense oil cells, high opening rate, moderate dryness, crisp hand feeling, and few impurities, ensuring no mold, insect damage, and halitosis.

[0133] In S1, the crushing was performed using a crusher, and then a 50-mesh standard sieve was used for screening to ensure uniform particle size of the raw materials.

[0134] The storage method in S1 is to store the obtained sample in a 4℃ refrigerator.

[0135] The ultrasonic treatment power of the ultrasonic cleaner in S2 is 200W, the ultrasonic temperature is 20℃, the ultrasonic time is 1 hour, and the water level is 3cm higher than the liquid level of the round-bottom flask.

[0136] The solvent in the solvent bottle in S3 is petroleum ether (analytical pure, 60-90℃), and the solvent dosage is 50ml.

[0137] The raw material bottle and the solvent bottle in S3 are located on the left and right sides of the simultaneous distillation and extraction device respectively. In the device, the position of the raw material bottle is lower than that of the solvent bottle.

[0138] The heating devices of the raw material bottle and the solvent bottle in S3 are different. The raw material bottle is heated by an electric heating jacket with a voltage setting of 150V; the solvent bottle is heated by a water bath with a water bath temperature setting of 90℃.

[0139] The condenser tube of the simultaneous distillation and extraction device in S3 is connected to circulating cooling water to ensure that the condensation temperature is maintained at 20℃, ensuring efficient condensation of steam.

[0140] The method of separating the mixture from water in S4 is as follows: after the mixture in the collection bottle is cooled to room temperature, it is transferred to a separatory funnel, and left to stand for 45 minutes. The oil and water are separated by their density difference, the lower water phase is discarded, and the upper petroleum ether-essential oil mixture is collected in a rotary evaporation flask.

[0141] The parameter settings of the rotary evaporator in S5 are as follows: rotary speed 30rpm / min, water bath temperature 40℃, and vacuum degree 0.09Mpa.

[0142] The rotary evaporation time in S5 is 5min, and the distillation process is observed in real time. When there is no obvious solvent dripping from the rotary evaporation flask, the distillation is stopped.

[0143] The method of ultrasonic-assisted simultaneous distillation and extraction of Zanthoxylum bungeanum essential oil in this embodiment is mainly based on the comprehensive mechanism of "sonic chemical enhanced mass transfer" and "synchronous distillation-solvent trapping synergistic effect". When ultrasonic waves propagate in the liquid, cavitation bubbles are formed. When the bubbles burst, high-temperature and high-pressure micro-jets and shock waves are generated, which can break the plant cell wall and promote the rapid release of essential oil from the oil-containing glands. At the same time, this micro-disturbance can also enhance the contact area between the raw material particles and water, accelerate the diffusion of effective components to the vapor phase, and provide more volatile material basis for subsequent simultaneous distillation.

[0144] In the distillation stage, the Zanthoxylum bungeanum and water in the raw material bottle are heated to a micro-boiling state after mixing. The water vapor carries the volatile essential oil components released from the Zanthoxylum bungeanum and is brought out during the continuous rising process, forming an oil-water vapor mixture. Unlike traditional steam distillation, this method sets petroleum ether as the extraction solvent, so that the vapor is immediately condensed into the solvent phase after condensation, realizing a continuous process of "vapor carrying-condensation dissolution-oil phase trapping", thereby significantly reducing the loss of essential oil in the condensed water phase, improving the yield and extraction efficiency.

[0145] The structure layout of the device plays a key role in the mass and heat transfer process. The raw material bottle is positioned lower than the solvent bottle, so that the petroleum ether vapor can be condensed into the Zanthoxylum bungeanum vapor path area, enhancing the meeting and mixing effect of the two-phase gas flow. Different heating methods (electric heating jacket and water bath) ensure that the raw material bottle maintains micro-boiling and the solvent bottle evaporates stably, preventing solvent from boiling or condensation efficiency from decreasing. At the same time, the constant temperature cooling water circulation of the condenser tube is maintained at 20°C, which can effectively condense the vapor and quickly separate the layers, helping the essential oil to be enriched with petroleum ether phase.

[0146] In the separation stage, the oil-water separation relies on the density difference between the two phases. By standing, the water phase sinks and the oil phase floats, further purifying the essential oil and solvent mixture. This process not only avoids the emulsification caused by mechanical stirring, but also reduces the loss of essential oil. Finally, the petroleum ether solvent is removed by rotary evaporation, which takes advantage of vacuum to reduce the boiling point and gentle evaporation to prevent the destruction of heat-sensitive components (such as terpenes, aldehydes and ketones) in the essential oil, ensuring that the product has a light yellow and transparent color and a pure aroma.

[0147] This method uses ultrasonic to enhance the wall breaking and synchronous distillation-solvent trapping synergy to achieve the goal of "low temperature, fast and efficient" extraction. Ultrasonic promotes the release of essential oil, while simultaneous distillation and extraction reduces secondary loss and thermal degradation. The synergistic effect of the two strengthening mechanisms makes the essential oil yield, purity and aroma retention significantly better than simple steam distillation or traditional extraction, providing an efficient, green and popular process path for the extraction of aromatic plant essential oils such as Zanthoxylum bungeanum.

[0148] The application provides a method for extracting zanthoxylum bungeanum essential oil through ultrasonic-assisted simultaneous distillation and extraction, and the zanthoxylum bungeanum essential oil obtained has high quality, high yield and low solvent residue, and can be widely applied to the following fields as a key natural raw material and functional component, and can derive various related products.

[0149] 1. Food industry field

[0150] High-end condiments and food additives:

[0151] Product: Compound seasoning oil, hot pot base material, spicy snack food (such as spicy strips, dried bean curd), sauce, pickling material and the like.

[0152] Application value: The zanthoxylum bungeanum essential oil extracted has pure aroma and sufficient spiciness, can effectively improve the flavor level and intensity of products, replaces or partially replaces traditional zanthoxylum bungeanum powder, makes the flavor more stable and uniform, and has no solid residue, and improves the taste and appearance of food.

[0153] Natural food preservative:

[0154] Product: Applied to the preservation of cooked meat, cakes, noodles and the like.

[0155] Application value: The zanthoxylum bungeanum essential oil has been shown to have broad-spectrum antibacterial and antioxidant activity. As a natural and safe biological preservative, it can replace or reduce the use of chemical preservatives, and meet the clean label (Clean Label) consumption trend.

[0156] Functional food and beverage:

[0157] Product: Functional beverage, oral liquid, health capsule and the like with spiciness experience.

[0158] Application value: The active ingredients (such as zanthoxylum bungeanum spicin) in the zanthoxylum bungeanum essential oil have specific physiological functions, and can be used for developing innovative food and beverage with unique sensory experience or specific health claims.

[0159] 2. Daily chemical and perfume field

[0160] Personal care and washing product:

[0161] Product: Shampoo (for scalp care), shower gel, toothpaste, functional soap with “warm feeling” or “relieving” effect.

[0162] Application value: The zanthoxylum bungeanum essential oil can produce unique tingling and warm feeling, and can be added to personal care products to provide novel use experience and claimed effect. Meanwhile, its antibacterial property is also suitable for acne-removing and oil-controlling products.

[0163] Characteristic fragrance product:

[0164] Product: High-end salon perfumes, indoor aromatherapy, essential oil diffusion, etc.

[0165] Application value: The unique "pepper and numbness" aroma of Zanthoxylum bungeanum can be used as a distinctive note in fragrance creation, creating innovative fragrance products with personality and memory points such as oriental and woody notes.

[0166] Oral care products:

[0167] Product: Mouthwash, breath freshening spray, etc.

[0168] Application value: Utilizing its antibacterial and breath freshening properties, it provides a natural source of oral care solution.

[0169] 3. Medicine and health field

[0170] Traditional Chinese medicine modernization and external preparation:

[0171] Product: Plaster, patch, liniment, massage oil, etc.

[0172] Application value: In traditional Chinese medicine theory, Zanthoxylum bungeanum has the effects of warming the center, stopping pain, killing insects and stopping itching. The high-purity essential oil obtained by the invention can be used as a standardized raw material for the development of external medicines or medical devices for treating symptoms such as rheumatic pain, muscle soreness and skin itching.

[0173] Adjuvant therapy products:

[0174] Product: Transdermal drug delivery carrier, local anesthetic adjuvant.

[0175] Application value: The local anesthetic and transdermal promoting effect of Zanthoxylum bungeanum makes it have potential application value in the development of transdermal drug delivery systems.

[0176] 4. Agriculture and animal husbandry field

[0177] Green plant source pesticide:

[0178] Product: Insecticide, repellent for organic agriculture.

[0179] Application value: Zanthoxylum bungeanum essential oil has repellent and killing effects on a variety of pests, and can be developed into environmentally friendly biological pesticides to reduce chemical pesticide residues and pollution.

[0180] Feed additive:

[0181] Product: Feed additive for livestock and poultry.

[0182] Application value: As a natural antibacterial and flavoring substance, it can be added to feed to improve animal intestinal health, reduce antibiotic use, and possibly improve meat flavor.

[0183] Second, the technical effects of the embodiments of the present application are related to the evidence.

[0184] The technical effects of the present application are fully verified by comparing the objective data of the embodiments with the comparative examples. These evidences not only include macro yield data, but also micro component analysis revealing the inherent quality advantages, which together constitute a complete and three-dimensional evidence system.

[0185] Core evidence one: significant improvement in extraction efficiency-yield data

[0186] Evidence source: performance test of Example 1 (inventive method) and Comparative Example 1 (traditional steam distillation method).

[0187] Specific data:

[0188] The yield of Zanthoxylum bungeanum essential oil obtained by the UAE-SDE method of the present application is 8.37%.

[0189] The yield of traditional steam distillation method is 5.96%.

[0190] Evidence power:

[0191] The extraction efficiency of the inventive method is absolutely improved by 2.41 percentage points, and the relative improvement rate is more than 40%.

[0192] This directly proves that the present application has a revolutionary advantage in breaking the yield bottleneck and reducing raw material waste.

[0193] Core evidence two: outstanding product quality-GC-MS component analysis

[0194] Evidence source: GC-MS (gas chromatography-mass spectrometry) thermogram and component list comparison of the inventive method (UAE-SDE) and traditional water extraction method.

[0195] Specific data and findings:

[0196] In the provided GC-MS component list, a series of known key flavor and active components of Zanthoxylum bungeanum, including "α-Phellandrene", "D-Limonene", "Caryophyllene", etc. were detected.

[0197] Key findings: Compared with the traditional water extraction method, the UAE-SDE method of the present application obtains essential oil with more abundant and representative volatile components. This indicates that the present method can more comprehensively capture the complete aroma profile and active substance spectrum of Zanthoxylum bungeanum.

[0198] Evidence power:

[0199] More complete retention of components: GC-MS data directly show that the method of the present application can effectively transfer and retain more types of flavor components, especially volatile ones, in the final product, due to the combination of ultrasonic cell wall breaking and immediate condensation capture by SDE.

[0200] More pure and high-quality flavor: The richer component spectrum is the material basis for the stronger aroma of essential oil and the closer to the original flavor of natural Zanthoxylum bungeanum. This scientifically analyzes the excellent effect of the present application in "retaining heat-sensitive components and preventing distortion of aroma", which perfectly confirms the sensory description of "light yellow transparent and strong and pure aroma" in the examples.

[0201] Core evidence three: guarantee of product safety-solvent residue control

[0202] Evidence source: "beneficial effects" part of the invention and process parameters in the specific embodiment.

[0203] Specific commitment and process guarantee:

[0204] The present application promises that the "solvent residue in the finished essential oil is less than 10mg / kg".

[0205] The result is ensured by optimized rotary evaporation parameters (water bath 40-50℃, vacuum degree 0.08-0.09Mpa), which can efficiently remove petroleum ether under mild conditions.

[0206] Evidence effectiveness: This index is direct evidence that the product of the present application meets the safety standards in the fields of food and medicine.

[0207] Core evidence four: economic efficiency and universality of the process-equipment and energy consumption

[0208] Evidence source: "beneficial effects" and specific embodiments in the invention.

[0209] General equipment: It is explicitly stated that "ultrasonic cleaner, electric heating jacket, rotary evaporator and other conventional laboratory or industrial equipment" are used.

[0210] Optimized time consumption: The total extraction time (ultrasonic 1h+SDE 2-3h) is shorter than that of traditional methods, and the yield is higher, which means higher production efficiency and energy efficiency.

[0211] Evidence effectiveness: This constitutes strong evidence that the present application is "easy to industrialize, low investment threshold, and controllable comprehensive operating cost".

[0212] Comparative example 1

[0213] The Zanthoxylum bungeanum essential oil extraction method provided by this comparative example is: water vapor distillation method to extract Zanthoxylum bungeanum essential oil.

[0214] Performance test

[0215] The yield of the obtained pepper essential oil in example 1, example 2, example 3 and comparative example 1 was detected, and the obtained data was recorded in the following table:

[0216]

[0217] Through the experimental results in the above table, we found that the yield of the pepper essential oil in example 1 reached 8.37%, which was significantly higher than 5.96% in comparative example 1. This showed that the ultrasonic-assisted simultaneous distillation and extraction process was superior to the traditional steam distillation method in extraction efficiency. In addition, the yields of example 2 and example 3 were 6.75% and 5.99% respectively, which were also higher than that of comparative example 1, further verifying the stability and effectiveness of the process. In summary, the method of extracting pepper essential oil provided by the present application has good extraction effect and high market promotion and application value.

[0218] The above description is only a preferred embodiment of the present application and is not intended to limit the present application. Any modification, equivalent replacement and improvement made by any person skilled in the art within the technical scope disclosed by the present application shall be covered within the protection scope of the present application.

Claims

1. A method of extracting essential oil from Zanthoxylum bungeanum Maxim. by ultrasonic-assisted simultaneous distillation and extraction, characterized in that, The method comprises the following steps: S1, crushing and screening the selected high-quality Zanthoxylum bungeanum, and collecting the undersize as the extraction raw material; S2, loading the extraction raw material into a round-bottom flask, mixing with distilled water according to the solid-liquid ratio of 1:15 g / ml, and then placing in an ultrasonic cleaner for ultrasonic treatment, so that the raw material is subjected to cell wall microscale rupture under ultrasonic cavitation; S3, connecting the raw material bottle and the solvent bottle to a simultaneous distillation extraction device, maintaining the raw material bottle in a micro-boiling state and the solvent bottle in a stable evaporation state, and performing simultaneous distillation extraction for 2-3 hours to realize mass transfer migration of volatile aromatic components in the raw material; S4, transferring the mixture obtained after extraction to a separatory funnel to separate water, and obtaining a petroleum ether-essential oil mixture; S5, connecting the petroleum ether-essential oil mixture to a rotary evaporator for rotary evaporation to obtain a light yellow transparent Zanthoxylum bungeanum essential oil.

2. The method of claim 1, wherein, In the step S1, the high-quality Zanthoxylum bungeanum selected by artificial selection and meeting the predetermined sensory and physical standards is first crushed by a shearing crusher in an intermittent and low-speed operation mode; the macroscopic organizational structure of the Zanthoxylum bungeanum is destroyed by controllable mechanical force, and the integrity of the oil gland cells rich in essential oil inside the Zanthoxylum bungeanum is maximally preserved, thereby avoiding pre-loss of volatile components caused by excessive crushing or instantaneous high temperature; In the step S1, the crushed product is classified and screened through a 50-mesh standard screen, and the undersize with optimal particle size uniformity passing through the screen is accurately collected as the raw material for this extraction; this pretreatment process accurately controls the particle size and specific surface area of the raw material, thereby laying a crucial physical foundation for uniform and efficient action of ultrasonic energy and solvent medium in the subsequent steps; The ultrasonic treatment in the step S2 opens the aromatic oil glands by cavitation effect, forming an internal microchannel structure conducive to subsequent vapor carrying of volatile components, thereby reducing the internal diffusion resistance in the process of simultaneous distillation extraction; The ultrasonic treatment in the step S2 precisely acts on the cell wall structure of the Zanthoxylum bungeanum raw material, selectively causing microscale rupture and porosity, thereby efficiently releasing the intracellular oil gland contents without causing significant thermal degradation, and dispersing the contents in the aqueous phase to prepare a high-concentration precursor for the subsequent simultaneous distillation extraction step; In the step S3, the device adopts an asymmetric heating system: the raw material bottle is heated by an electric heating jacket to maintain its contents in a micro-boiling state, and the solvent bottle is controlled by a constant-temperature water bath to ensure that the petroleum ether is in a stable and continuous evaporation state; In the step S3, in this synergistic system, the pre-processed material in the raw material bottle can be efficiently penetrated by water vapor and carry the released volatile essential oil components out due to the microchannel network constructed inside; at the same time, the petroleum ether vapor evaporated from the solvent bottle meets the water vapor and essential oil components in the middle part of the device, and efficient mass transfer is completed at the gas-liquid interface, and the essential oil components are selectively extracted into the petroleum ether phase. The process in step S3 lasts for 2 to 3 hours, ensuring sufficient and complete mass transfer; the entire system is maintained at a low temperature environment of 10-20℃ by circulating cooling water at the condensation section, aiming to achieve immediate condensation of the steam backflow, and maximize the residence time of the heat-sensitive components in the high-temperature zone; The process in step S3 is under the synergistic conditions of micro-boiling of the raw material bottle and stable evaporation of the solvent bottle, which makes it easier for water vapor to enter the ultrasonically broken tissue structure, and realizes the enhancement of nonlinear migration of volatile components, so as to improve the actual extraction rate of essential oil and improve the phase separation behavior in the subsequent liquid separation and rotary evaporation process; The separation process in step S4 benefits from the optimization of the cell structure of the raw material by the previous ultrasonic pretreatment, and the content of resin macromolecules and hydrophilic impurities in the obtained extraction phase is significantly reduced, so that the oil-water interface is more clear, and the occurrence of emulsification is effectively avoided; in the separation operation, the lower water phase is accurately discarded, and the upper clear petroleum ether-essential oil mixed solution is precisely collected and transferred to a dedicated rotary evaporation bottle for subsequent treatment; The optimization of parameters in step S5 aims to realize the efficient and rapid evaporation of petroleum ether, while maximizing the avoidance of the escape or chemical structure damage of heat-sensitive aromatic components in essential oil; through the constant rotation of the rotary bottle, a uniform film is formed on the wall of the bottle.

3. The method for extracting Sichuan pepper essential oil using ultrasound-assisted simultaneous distillation and extraction as described in claim 1, characterized in that, The selection conditions of high-quality Zanthoxylum bungeanum in S1: bright and uniform color, emitting rich and pure pepper and sesame aroma, and the particles are full, oil cell is dense, opening rate is high, dryness is moderate, hand feeling is crisp, impurities are few, and there are no signs of mildew, insect damage, and rancid smell; The crushing in S1 is performed by using a crusher, and then a 50-mesh standard sieve is selected for screening, to ensure uniformity of the raw material particles.

4. The method for extracting Sichuan pepper essential oil using ultrasound-assisted simultaneous distillation extraction as described in claim 1, characterized in that, The storage method in S1 is to store the obtained sample in a 4℃ refrigerator.

5. The method of claim 1, wherein the ultrasonic-assisted simultaneous distillation and extraction of the Zanthoxylum bungeanum essential oil is performed at a temperature of 200-300 °C and a pressure of 0.001-0.1 MPa. The ultrasonic treatment by the ultrasonic cleaner in S2 has a power of 200W, an ultrasonic temperature of 10-20℃, and an ultrasonic time of 1 hour, and the water level is preferably 2-3cm higher than the liquid level of the round-bottom flask.

6. The method of claim 1, wherein the ultrasonic-assisted simultaneous distillation and extraction of the Zanthoxylum bungeanum essential oil is performed at a temperature of 200-300 °C and a pressure of 0.001-0.1 MPa. The solvent in the solvent bottle in S3 is petroleum ether (analytical pure, 60-90℃), and the solvent dosage is just enough to cover the raw material. The raw material bottle and the solvent bottle in S3 are respectively located on the left and right sides of the simultaneous distillation and extraction device, and in the device, the position of the raw material bottle is lower than that of the solvent bottle. The heating devices of the raw material bottle and the solvent bottle in S3 are different, the raw material bottle is heated by an electric heating jacket, and the voltage of the electric heating jacket is set to 100-150V; the solvent bottle is heated by a water bath, and the water bath temperature is set to 80-90℃.

7. The method of claim 1, wherein the ZDEx is performed at a temperature of 40- 60°C, a pressure of 0.1-0.5 torr, and a frequency of 20-40 kHz. The condenser tube of the simultaneous distillation and extraction device in S3 is connected to circulating cooling water to ensure that the condensation temperature is maintained at 10-20℃, ensuring efficient condensation of the steam.

8. The method for extracting Sichuan pepper essential oil using ultrasound-assisted simultaneous distillation and extraction as described in claim 1, characterized in that, The method for separating the mixture from water in S4: after the mixture in the collection bottle is cooled to room temperature, it is transferred to a separatory funnel, and is left to stand for 30-45 minutes, and the separation is realized by the density difference between oil and water, the lower water phase is discarded, and the upper petroleum ether-essential oil mixed solution is collected into a rotary evaporation bottle.

9. The method for extracting Sichuan pepper essential oil using ultrasound-assisted simultaneous distillation and extraction as described in claim 1, characterized in that, The parameter settings of the rotary evaporator in S5 are as follows: the rotation speed is 30-40 r / min, the water bath temperature is 40-50 DEG C, and the vacuum degree is 0.08-0.09 Mpa.

10. The method for extracting Sichuan pepper essential oil using ultrasound-assisted simultaneous distillation extraction as described in claim 1, characterized in that, The rotary evaporation time in S5 is 5-6 min, and the distillation process is observed in real time. When there is no obvious solvent drop in the rotary evaporation bottle, stop distillation.

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