A pepper oleoresin, its preparation method and application

Abstract

This invention relates to the field of material extraction technology, specifically disclosing a Sichuan pepper oleoresin, its preparation method, and its application. The method for preparing the Sichuan pepper oleoresin includes the step of extracting Sichuan pepper raw materials using supercritical carbon dioxide fluid. In the extraction, medium-chain fatty acid triglycerides are used as a carrier for the first stage extraction at an extraction temperature of 36-46℃ and an extraction pressure of 25-29 MPa. The extracted material is then separated into a first Sichuan pepper oleoresin by passing it through a distillation column. The distillation column has a pressure of 9-21 MPa and is divided into three sections. The extracted material enters the distillation column from bottom to top, with the first section at a temperature of 40-45℃, the second section at 50-55℃, and the third section at 60-65℃. Using this method, high-quality Sichuan pepper oleoresin with low bitterness and low precipitation can be obtained. Furthermore, the Sichuan pepper residue after the first stage extraction can be subjected to a second extraction, improving the overall resource utilization rate of the Sichuan pepper raw materials.

Description

Technical Field

[0001] This invention relates to the field of material extraction technology, and more specifically, to a pepper oleoresin, its preparation method, and its application. Background Technology

[0002] In the process of natural selection and long-term evolution, Sichuan pepper has synthesized some natural antitoxins to resist pests and diseases, such as alkaloids, flavonoids, phenols, terpenes, and coumarins (derived products). However, most of these secondary metabolites have a bitter taste, which to some extent limits the application and deep processing of Sichuan pepper and its extracts.

[0003] Most existing technologies for preparing Sichuan pepper oleoresin rely on single processes such as solvent extraction or supercritical CO2 extraction. Solvent extraction is generally costly, complex, and prone to issues like excessive solvent residues in the product. Supercritical extraction, conducted at a constant temperature, typically uses highly polar solvents like ethanol as carriers, resulting in resins with a higher proportion of polar components. This leads to unresolved problems such as poor oil solubility, high bitterness, and high levels of precipitation.

[0004] In addition, although Chinese patent CN110338233A uses enzymatic hydrolysis to destroy bitter substances, then adds bitterness inhibitors, and finally removes bitter substances by low-temperature centrifugation, the enzymatic hydrolysis substrate in this scheme is pepper oleoresin, rather than producing low-bitter pepper oleoresin from pepper raw materials in one step. Its enzymatic hydrolysis reaction time is long and the cost is high, which increases the cost of industrial production.

[0005] Therefore, it is necessary to further develop the refining process for low-bitter Sichuan pepper oleoresin. Summary of the Invention

[0006] One of the objectives of this invention is to provide a new method for large-scale production of high-quality Sichuan pepper oleoresin with low bitterness and low precipitation.

[0007] This invention provides a method for preparing Sichuan pepper oleoresin, which includes the step of extracting Sichuan pepper raw material with supercritical carbon dioxide fluid; in the extraction, medium-chain fatty acid triglycerides are used as carriers for the first stage extraction, followed by distillation to separate the first Sichuan pepper oleoresin.

[0008] The conditions for the first stage of extraction are: extraction temperature 36-46℃, extraction pressure 25-29 MPa;

[0009] During the first stage of extraction, extraction and distillation are carried out simultaneously. The extracted material is separated into the first pepper oil resin through a distillation column. The pressure of the distillation column is 9-21 MPa. The distillation column is divided into three sections. The extracted material enters the distillation column from bottom to top. The temperature of the first section is 40-45℃, the temperature of the second section is 50-55℃, and the temperature of the third section is 60-65℃.

[0010] This invention has discovered that when Sichuan pepper raw materials are extracted and distilled under specific conditions with a specific carrier, high-quality Sichuan pepper oleoresin with low bitterness and low precipitation can be obtained. The operation is simple and suitable for large-scale industrial production.

[0011] This invention, through a combination of specific fractional extraction and distillation processes, can better remove impurities (such as some large molecular precipitates that are not easy to separate) and bitter components from materials, and minimize the formation of new bitter components during the distillation stage.

[0012] In the method of the present invention, the distillation column contains conventional packing materials in the art (such as ceramic corrugated packing with a pore size of 5-10 micrometers or stainless steel wire mesh corrugated packing) to increase the contact area of ​​the liquid and facilitate the efficient separation of pepper oil resin and other components.

[0013] The method of the present invention preferably further includes a second stage of extraction on the Sichuan pepper raw material after the first stage of extraction, followed by a step of distillation to separate the second Sichuan pepper oleoresin; the conditions for the second stage of extraction are: extraction temperature 55-65℃, extraction pressure 25-29 MPa; the method for distillation to separate the second Sichuan pepper oleoresin is the same as the method for distillation to separate the first Sichuan pepper oleoresin.

[0014] This invention involves a second stage of extraction using specific conditions on the remaining pepper pulp after the first stage extraction to prepare high-quality pepper oleoresin. This process yields pepper oleoresin with a pepper amide content of 21-27%, resulting in a high overall pepper amide content yield. This process not only produces a high-quality product but also improves the overall utilization rate of the raw materials.

[0015] In the method of the present invention, in the first stage of extraction, the required carbon dioxide fluid flow rate is 10-50 L / h per kilogram of Sichuan pepper raw material; the required mass of the carrier is 1-5% of the mass of the Sichuan pepper raw material; in the second stage of extraction, the required carbon dioxide fluid flow rate is 10-50 L / h per kilogram of Sichuan pepper raw material.

[0016] In the method of the present invention, the medium-chain fatty acid triglyceride is one substance or a mixture of multiple medium-chain fatty acid triglycerides, and the medium-chain fatty acid triglyceride is preferably one or more of caprylic acid triglyceride, capric acid triglyceride and lauric acid triglyceride.

[0017] In the method of the present invention, the extraction time of the first stage is 1-2 hours; the extraction time of the second stage is 2-3 hours.

[0018] The method of the present invention further includes a step of separating the remaining materials after separating the first pepper oil resin and the second pepper oil resin in a separation vessel, wherein the pressure of the separation vessel is 3-7 MPa and the temperature is 30-40℃.

[0019] After the remaining materials of this invention are separated in a separation vessel, pepper essential oil (which can be used to formulate pepper resin), pepper oleoresin with low pepper amide content, and gaseous carbon dioxide (which can be recycled and reused) can be obtained.

[0020] Overall, the total content of zanthoxylum bungeanum oleoresin with low bitterness obtained from the first stage of extraction and separated from the distillation column, the second stage of extraction and separated from the distillation column, and the zanthoxylum bungeanum oleoresin separated from the separation vessel after both stages of extraction account for more than 95% of the total zanthoxylum bungeanum oleoresin content in the raw zanthoxylum bungeanum.

[0021] The method of the present invention further includes a step of pre-treating the Sichuan pepper raw material before the first stage extraction; the pre-treatment includes deseeding, crushing or breaking.

[0022] The thickness of the rolled peppercorn raw material is 0.2-0.8 mm;

[0023] The crushed Sichuan pepper raw material has a passing rate of 60%-90% through a 20-mesh standard sieve.

[0024] Preferably, the processing temperature during rolling or crushing is 25-40°C.

[0025] Crushing can be done using an automatic crusher with a screen mesh of 10-20 mesh.

[0026] As a preferred embodiment, the supercritical extraction process of pepper oleoresin of the present invention includes: (1) pretreatment of pepper raw materials; (2) supercritical fluid treatment: extraction in an extraction vessel, distillation by a supercritical distillation column, and finally passing through a supercritical separation vessel.

[0027] Specifically, after extraction, the extract is discharged from the extraction vessel and enters a supercritical distillation column for distillation through the feed inlet. Distillation and supercritical extraction are carried out simultaneously. Afterward, the material enters a supercritical separation vessel from the top of the distillation column. The extract obtained after the first-stage extraction conditions is processed by the distillation column. After depressurization, the high-quality Sichuan pepper oleoresin (first Sichuan pepper oleoresin) with low bitterness and low precipitation is released from the distillation column. The Sichuan pepper oleoresin released after the extract obtained after the second-stage extraction conditions is the ordinary product (second Sichuan pepper oleoresin). The Sichuan pepper essential oil released from the separation vessel can be used for product blending. Carbon dioxide can be recovered and reused through pipelines. The Sichuan pepper oleoresin with low Sichuan pepper amide content can be used for blending Sichuan pepper oil products of different content specifications.

[0028] The present invention also provides a pepper oil resin, which is prepared by the above method; preferably, the pepper oil resin is the first pepper oil resin, the first pepper oil resin has a pepper amide content of 20-25%, and the precipitate mass ratio is 0.1-0.3%.

[0029] This invention can prepare pepper oleoresin with virtually no bitterness and few precipitates (good oil solubility). Compared with ordinary pepper oleoresin, it is more suitable for application in food and condiments, avoiding the generation of unpleasant flavors.

[0030] Generally, the content of pepper amide in raw pepper is 2.0-2.5%, and the pepper oleoresin prepared by this invention significantly increases the content of this active ingredient.

[0031] The present invention also provides the application of the above method or pepper oleoresin in the preparation of seasonings.

[0032] The present invention also provides a seasoning comprising the above-mentioned pepper oil resin, preferably comprising the first pepper oil resin.

[0033] The beneficial effects of this invention are at least as follows:

[0034] The method provided by this invention can efficiently extract high-quality pepper oleoresin from pepper raw materials, which basically eliminates bitterness, greatly reduces precipitate content (good oil solubility), is simple to operate, and is suitable for large-scale industrial production. Detailed Implementation

[0035] The preferred embodiments of the present invention will now be described in detail with reference to specific examples. It should be understood that the following examples are given for illustrative purposes only and are not intended to limit the scope of the invention. Those skilled in the art can make various modifications and substitutions to the present invention without departing from its spirit and essence.

[0036] Unless otherwise specified, the experimental methods used in the following examples are conventional methods. Unless otherwise specified, the materials and reagents used in the following examples are commercially available or prepared according to conventional methods in the art.

[0037] In the specific embodiments section of this invention, the detection method for xanthanamide in Sichuan pepper raw materials and Sichuan pepper oleoresin is described in GH / T 1291-2020. The packing material in the distillation column is macroporous ceramic composite corrugated packing with a pore size of 8 micrometers.

[0038] Example 1

[0039] This embodiment provides a 1500L supercritical extraction process for Sichuan pepper oleoresin, as detailed below:

[0040] (1) Pretreatment: 400 kg of Sichuan Jinyang seedless green pepper raw material (pepper amide content 2.5%) was rolled into sheets using a rolling mill at a rolling temperature of 32℃ and a sheet thickness of 0.5 mm.

[0041] (2) After pretreatment, the material is fed into the supercritical extraction vessel. Carbon dioxide is continuously pumped in through a high-pressure pump at a speed of 12000 L / h. 12 kg of carrier (capital-capric triglyceride, capric triglyceride, and lauric triglyceride in a mass ratio of 1:1:1) is pumped in using a carrier pump at a speed of 8 kg / h. The pressure in the extraction vessel is 27 MPa. The first stage of extraction is carried out at an extraction temperature of 41℃ for 1.5 h. Extraction and distillation are carried out simultaneously. The extracted material enters the distillation column and passes through the first stage temperature zone of 42℃, the second stage temperature zone of 52℃, and the third stage temperature zone of 62℃ from bottom to top under a pressure of 15 MPa. Afterward, it is fed into the separation vessel (the pressure in the separation vessel is 5 MPa and the temperature is 35℃) from the top of the distillation column. After the distillation column is depressurized, low-bitter pepper oil resin is collected, weighing 32.2 kg, with a pepper amide content of 21.9%.

[0042] Second-stage extraction: The extraction vessel was heated to 60℃, and the Sichuan pepper raw material after the first-stage extraction was extracted again for 2.5 hours under the same carbon dioxide conditions (i.e., consistent pump speed and extraction pressure). The extracted material was sequentially fed into a distillation column and a separation vessel (the pressure and temperature conditions of the distillation column and separation vessel were consistent with the first stage). After depressurization of the distillation column, 3.7 kg of Sichuan pepper oleoresin with a Sichuan pepper amide content of 22.8% was collected. After depressurization of the separation vessel, 51.8 kg of Sichuan pepper oleoresin with a Sichuan pepper amide content of 3.2% was collected. The overall Sichuan pepper amide content yield was 95.5% (the percentage of total Sichuan pepper amide content in the Sichuan pepper oleoresin collected from the distillation column after the first-stage extraction, the Sichuan pepper oleoresin collected from the distillation column after the second-stage extraction, and the Sichuan pepper oleoresin collected from the separation vessel after both stages of extraction, relative to the total Sichuan pepper amide content in the raw material). The carbon dioxide used was recycled back to the storage tank through a recovery system.

[0043] Example 2

[0044] This embodiment provides a 1500L supercritical extraction process for Sichuan pepper oleoresin, as detailed below:

[0045] (1) Pretreatment: 400 kg of Sichuan Jinyang deseeded pepper raw material (pepper amide content 2.5%) was rolled into sheets using a rolling mill at a rolling temperature of 25℃ and a sheet thickness of 0.2 mm.

[0046] (2) After pretreatment, the material is fed into the supercritical extraction vessel. Carbon dioxide is continuously pumped in through a high-pressure pump at a speed of 20,000 L / h. 20 kg of caprylic glycerol ester is pumped in using a carrier pump at a speed of 20 kg / h. The pressure in the extraction vessel is 29 MPa. The first stage of extraction is carried out at an extraction temperature of 36°C for 1 hour. Extraction and distillation are carried out simultaneously. The extracted material enters the distillation column from bottom to top and passes through the first stage temperature zone of 40°C, the second stage temperature zone of 50°C, and the third stage temperature zone of 60°C under a pressure of 9 MPa. Then, it is passed into the separation vessel from the top of the distillation column (the pressure in the separation vessel is 3 MPa and the temperature is 30°C). After the distillation column is depressurized, the low-bitter pepper oil resin is collected, weighing 31.5 kg, with a pepper amide content of 21.0%.

[0047] Second-stage extraction: The extraction vessel was heated to 55°C, and the Sichuan pepper raw material extracted in the first stage was further extracted for 3 hours under the same carbon dioxide conditions (i.e., consistent pump speed and extraction pressure). The extracted material was then sequentially fed into a distillation column and a separation vessel (the pressure and temperature conditions of the distillation column and separation vessel were consistent with the first stage). After depressurization of the distillation column, 8.6 kg of Sichuan pepper oleoresin was collected, with a Sichuan pepper amide content of 22.3%. After depressurization of the separation vessel, 55.4 kg of Sichuan pepper oleoresin was collected, with a Sichuan pepper amide content of 1.9%. The overall Sichuan pepper amide content yield was 95.9%. The carbon dioxide used was recycled back to the storage tank through a recovery system.

[0048] Example 3

[0049] This embodiment provides a 1500L supercritical extraction process for Sichuan pepper oleoresin, as detailed below:

[0050] (1) Pretreatment: 400 kg of Sichuan Jinyang deseeded pepper raw material (pepper amide content 2.5%) was rolled into sheets using a rolling mill at a rolling temperature of 40℃ and a sheet thickness of 0.8 mm.

[0051] (2) After pretreatment, the material is fed into the supercritical extraction vessel. Carbon dioxide is continuously pumped in through a high-pressure pump at a speed of 4000 L / h. 4 kg of decanoic acid glyceride is pumped in using a carrier pump at a speed of 2 kg / h. The pressure in the extraction vessel is 25 MPa. The first stage of extraction is carried out at a temperature of 46℃ for 2 hours. Extraction and distillation are performed simultaneously. The extracted material enters the distillation column from bottom to top and passes through the first stage temperature zone of 45℃, the second stage temperature zone of 55℃, and the third stage temperature zone of 65℃ under a pressure of 21 MPa. Afterward, it is fed into the separation vessel (the pressure in the separation vessel is 7 MPa and the temperature is 40℃). After the distillation column is depressurized, low-bitter pepper oil resin is collected, weighing 20.8 kg, with a pepper amide content of 24.5%.

[0052] Second-stage extraction: The extraction vessel was heated to 65℃, and the Sichuan pepper raw material extracted in the first stage was further extracted for 2 hours under the same carbon dioxide conditions (i.e., consistent pump speed and extraction pressure). The extracted material was then sequentially fed into a distillation column and a separation vessel (the pressure and temperature conditions of the distillation column and separation vessel were consistent with the first stage). After depressurization of the distillation column, 3.6 kg of Sichuan pepper oleoresin was collected, with a Sichuan pepper amide content of 26.7%. After depressurization of the separation vessel, 54.1 kg of Sichuan pepper oleoresin was collected, with a Sichuan pepper amide content of 6.4%. The overall Sichuan pepper amide content yield was 95.2%. The carbon dioxide used was recycled back to the storage tank through a recovery system.

[0053] Example 4

[0054] This embodiment provides a 1500L supercritical extraction process for Sichuan pepper oleoresin, which is basically the same as the process in Example 1, except that the carrier used is trilauric acid triglyceride. All other conditions are the same as in Example 1. Finally, after the first stage extraction and depressurization of the distillation column, low-bitter Sichuan pepper oleoresin was collected, weighing 32.1 kg, with a Sichuan pepper amide content of 22.0%.

[0055] In the second stage of extraction, after depressurizing the distillation column, 3.6 kg of pepper oleoresin with a pepper amide content of 22.9% was collected. After depressurizing the separation vessel, 51.9 kg of pepper oleoresin with a pepper amide content of 3.1% was collected. The overall pepper amide content yield was 94.95%.

[0056] Example 5

[0057] This embodiment provides a 1500L supercritical extraction process for Sichuan pepper oleoresin, which is basically the same as the process in Example 1, except that the raw material used is Chongqing Jiangjin green deseeded Sichuan pepper (Sichuan pepper amide content 2.0%). All other conditions are the same as in Example 1.

[0058] Finally, after the first stage of extraction and depressurization of the distillation column, low-bitter Sichuan pepper oil resin was collected, weighing 25.2 kg, with a Sichuan pepper amide content of 21.5%.

[0059] In the second stage of extraction, after depressurizing the distillation column, 3.5 kg of pepper oleoresin with a pepper amide content of 21.9% was collected. After depressurizing the separation vessel, 53.2 kg of pepper oleoresin with a pepper amide content of 2.7% was collected. The overall pepper amide content yield was 95.26%.

[0060] Comparative Example 1

[0061] This comparative example provides a supercritical extraction process for Sichuan pepper oleoresin, which is basically the same as that in Example 1, except that the supercritical extraction temperature in the first stage is 55°C, and the carrier and carbon dioxide pumping rates, as well as the distillation and separation methods, are the same as in Example 1. After depressurizing the first-stage distillation column, 32.5 kg of Sichuan pepper oleoresin with a Sichuan pepper amide content of 22.1% was collected. After depressurizing the second-stage distillation column, 3.6 kg of Sichuan pepper oleoresin with a Sichuan pepper amide content of 22.5% was collected. After depressurizing the separation vessel, 51.4 kg of Sichuan pepper oleoresin with a Sichuan pepper amide content of 3.1% was collected. The overall Sichuan pepper amide content yield is 95.9%.

[0062] Comparative Example 2

[0063] This comparative example provides a supercritical extraction process for Sichuan pepper oleoresin, which is basically the same as that in Example 1, except that no carrier is added. After depressurization of the first-stage distillation column, 32.4 kg of Sichuan pepper oleoresin with a Sichuan pepper amide content of 21.7% was collected. After depressurization of the second-stage distillation column, 3.8 kg of Sichuan pepper oleoresin with a Sichuan pepper amide content of 22.6% was collected. After depressurization of the separation vessel, 38.7 kg of Sichuan pepper oleoresin with a Sichuan pepper amide content of 4.2% was collected. The overall Sichuan pepper amide yield was 95.2%.

[0064] Comparative Example 3

[0065] This comparative example provides a supercritical extraction process for Sichuan pepper oleoresin, which is basically the same as that in Example 1, except that triacetin is used as the carrier. After depressurization of the first-stage distillation column, 32.3 kg of Sichuan pepper oleoresin with a Sichuan pepper amide content of 22.2% is collected. After depressurization of the second-stage distillation column, 3.5 kg of Sichuan pepper oleoresin with a Sichuan pepper amide content of 22.8% is collected. After depressurization of the separation vessel, 51.6 kg of Sichuan pepper oleoresin with a Sichuan pepper amide content of 3.0% is collected. The overall Sichuan pepper amide yield is 95.2%.

[0066] Comparative Example 4

[0067] This comparative example provides a supercritical extraction process for Sichuan pepper oleoresin, which is basically the same as that in Example 1, except that 95% ethanol is used as the carrier. After depressurization of the first-stage distillation column, 32.6 kg of Sichuan pepper oleoresin with a Sichuan pepper amide content of 21.5% is collected. After depressurization of the second-stage distillation column, 3.6 kg of Sichuan pepper oleoresin with a Sichuan pepper amide content of 22.7% is collected. After depressurization of the separation vessel, 40.3 kg of Sichuan pepper oleoresin with a Sichuan pepper amide content of 4.3% is collected. The overall Sichuan pepper amide yield is 95.6%.

[0068] Comparative Example 5

[0069] This comparative example provides a supercritical extraction process for Sichuan pepper oleoresin, which is basically the same as that in Example 1, except that the distillation column temperature is 50°C and no temperature gradient is set. After depressurization of the first stage distillation column, 33.0 kg of Sichuan pepper oleoresin with a Sichuan pepper amide content of 21.4% is collected. After depressurization of the second stage distillation column, 3.2 kg of Sichuan pepper oleoresin with a Sichuan pepper amide content of 22.4% is collected. After depressurization of the separation vessel, 51.4 kg of Sichuan pepper oleoresin with a Sichuan pepper amide content of 3.3% is collected. The overall Sichuan pepper amide yield is 94.8%.

[0070] Comparative Example 6

[0071] This comparative example provides a supercritical extraction process for Sichuan pepper oleoresin, which is basically the same as that in Example 1, except that the distillation column is set at 50°C in the first stage, 60°C in the second stage, and 70°C in the third stage. After depressurization of the first stage distillation column, 30.5 kg of Sichuan pepper oleoresin with a Sichuan pepper amide content of 23.2% is collected. After depressurization of the second stage distillation column, 3.3 kg of Sichuan pepper oleoresin with a Sichuan pepper amide content of 23.8% is collected. After depressurization of the separation vessel, 53.2 kg of Sichuan pepper oleoresin with a Sichuan pepper amide content of 3.0% is collected. The overall Sichuan pepper amide yield is 94.6%.

[0072] Comparative Example 7

[0073] This comparative example provides a supercritical extraction process for Sichuan pepper oleoresin, as detailed below:

[0074] (1) Pretreatment: 400 kg of deseeded pepper raw material (pepper amide content 2.5%) was rolled into sheets using a rolling mill at a rolling temperature of 58℃ and a sheet thickness of 0.5 mm;

[0075] (2) After pretreatment, the material is fed into the supercritical extraction vessel through the feed port. Carbon dioxide is continuously pumped in through a high-pressure pump at a speed of 12000 L / h. The extraction vessel pressure is 28 MPa, the extraction temperature is 60℃, and the extraction time is 4 h. The extracted material enters the distillation column at a pressure of 10 MPa and a temperature of 50℃. After passing through the distillation column, the material enters the separation vessel at a pressure of 5 MPa and a temperature of 50℃. After depressurization of the distillation column, 40.8 kg of pepper oleoresin with a pepper amide content of 20.8% is collected. After depressurization of the separation vessel, 33.5 kg of pepper oleoresin with a pepper amide content of 2.9% is collected. The overall pepper amide content yield is 94.6%. The carbon dioxide used is recycled back to the storage tank through the recovery system.

[0076] Experimental Example

[0077] This experimental example tested the products of each embodiment and comparative example, as follows:

[0078] 1. Bitterness evaluation

[0079] Evaluation Method: A Sichuan pepper oil product with 12% Sichuan pepper amide content and 40% essential oil content was prepared by blending Sichuan pepper oleoresin with Sichuan pepper essential oil and sunflower seed oil. This product was then further diluted with sunflower seed oil to a Sichuan pepper amide content of 0.15%. Ten sensory evaluators were selected. When evaluating bitterness, each evaluator used a 1mL disposable dropper to add 3 drops of the diluted oil to the center of their tongue. The evaluators then recorded the bitterness score according to a bitterness evaluation form. The average score of the ten evaluators was used as the bitterness score for that sample (using Sichuan pepper oleoresin, which had the highest bitterness in the comparative sample, as a control; a bitterness score of 5 was given, and a bitterness score of 0 was given for sunflower seed oil; the higher the score, the more bitter the sample). After tasting one sample, the evaluators rinsed their mouths with purified water, and waited 10 minutes before evaluating the next sample.

[0080] 2. Sedimentation rate

[0081] Test method: Mix the pepper oil resin with an equal weight of pepper essential oil. First, weigh a 15mL centrifuge tube and record the weight as m0. Then, weigh 9.00g of the mixed pepper oil resin into a 15mL centrifuge tube and record the total weight of the mixed pepper oil resin and the centrifuge tube as m1. Centrifuge at 4000rpm for 30min using a high-speed centrifuge. Gently pour off the upper layer of the mixed pepper oil resin from the test tube, then invert the test tube for 2 hours. Weigh the precipitate and the total weight of the test tube and record the weight as m2. Calculate the precipitate percentage as (m2-m0) / (m1-m0)×100%, which is the precipitation rate.

[0082] The test results of each specific embodiment and comparative example are shown in Table 1 (the test results of comparative example 7 are obtained by collecting pepper oil resin after depressurization of the distillation column).

[0083] Table 1

[0084]

[0085] Although the present invention has been described in detail above with general descriptions and specific embodiments, modifications or improvements can be made to it, which will be obvious to those skilled in the art. Therefore, all such modifications or improvements made without departing from the spirit of the present invention fall within the scope of protection claimed by the present invention.

Claims

1. A method of preparing a zanthoxyli resinum, characterized in that, The method comprises the steps of: extracting pepper raw materials with carbon dioxide supercritical fluid; in the extraction, medium-chain fatty acid triglyceride is used as a carrier agent to perform first-stage extraction, and then first-stage pepper oleoresin is separated by rectification; The first-stage extraction is performed at an extraction temperature of 36-46 ℃ and an extraction pressure of 25-29 MPa; In the first-stage extraction, extraction and rectification are performed synchronously, and the extracted material is separated from the first-stage pepper oleoresin by passing through a rectification column; the rectification column has a pressure of 9-21 MPa, and is divided into three sections; the extracted material enters the rectification column from bottom to top; the temperature of the first section is 40-45 ℃, the temperature of the second section is 50-55 ℃, and the temperature of the third section is 60-65 ℃; The medium-chain fatty acid triglyceride is one or more of caprylic acid triglyceride, capric acid triglyceride and lauric acid triglyceride.

2. The method of claim 1, wherein, The method further comprises the steps of: continuing to perform second-stage extraction on the pepper raw materials after the first-stage extraction, and then separating second-stage pepper oleoresin by rectification; the second-stage extraction is performed at an extraction temperature of 55-65 ℃ and an extraction pressure of 25-29 MPa; and the method for separating the second-stage pepper oleoresin by rectification is the same as the method for separating the first-stage pepper oleoresin by rectification.

3. The method of claim 2, wherein, In the first-stage extraction, the carbon dioxide fluid flow required for each kilogram of pepper raw materials is 10-50 L / h; and the mass of the carrier agent required is 1-5% of the mass of the pepper raw materials; in the second-stage extraction, the carbon dioxide fluid flow required for each kilogram of pepper raw materials is 10-50 L / h.

4. The method according to claim 2 or 3, characterized in that, The first-stage extraction is performed for 1-2 h; and the second-stage extraction is performed for 2-3 h.

5. The method according to claim 2 or 3, characterized in that, The method further comprises the steps of: performing separation kettle separation on the remaining material after the first-stage pepper oleoresin and the second-stage pepper oleoresin are separated, respectively; the separation kettle has a pressure of 3-7 MPa and a temperature of 30-40 ℃.

6. The method of claim 4, wherein, The method further comprises the steps of: performing separation kettle separation on the remaining material after the first-stage pepper oleoresin and the second-stage pepper oleoresin are separated, respectively; the separation kettle has a pressure of 3-7 MPa and a temperature of 30-40 ℃.

7. The method according to any of claims 1 to 3, 6, characterized in that, The method further comprises the step of pretreating the pepper raw materials before the first-stage extraction; the pretreatment comprises seed removal, flaking or crushing; The thickness of the flaked pepper raw materials is 0.2-0.8 mm; The 20-mesh standard sieve passing rate of the crushed pepper raw materials is 60%-90%.

8. The method of claim 4, wherein, The method further comprises the step of pretreating the pepper raw materials before the first-stage extraction; the pretreatment comprises seed removal, flaking or crushing; The thickness of the flaked pepper raw materials is 0.2-0.8 mm; The 20-mesh standard sieve passing rate of the crushed pepper raw materials is 60%-90%.

9. The method of claim 5, wherein, The method further comprises the step of pretreating the pepper raw materials before the first-stage extraction; the pretreatment comprises seed removal, flaking or crushing; The thickness of the flaked pepper raw materials is 0.2-0.8 mm; The 20-mesh standard sieve passing rate of the crushed pepper raw materials is 60%-90%.

10. A Zanthoxylum oil resin characterized by, The method is prepared by any one of claims 1-9.

11. The prickly ash oleoresin according to claim 10, characterized in that, The zanthoxyli resina is the first zanthoxyli resina, the first zanthoxyli resina has a zanthoxylum amide content of 20-25%, and a precipitate mass ratio of 0.1-0.3%.

12. Use of the zanthoxyli resina according to any one of claims 1 to 9 or according to claim 10 or 11 for the preparation of a condiment.

13. A condiment, characterized in that, The zanthoxyli resina according to claim 10 or 11. The zanthoxyli resina according to claim 10 or 11.

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