Zanthoxylum oil resin as well as preparation method and application thereof

Abstract

The invention relates to the technical field of substance extraction, and particularly discloses zanthoxylum oil resin as well as a preparation method and application thereof. The method for preparing the zanthoxylum oil resin comprises the following steps: extracting a zanthoxylum raw material with a carbon dioxide supercritical fluid; in the extraction, medium-chain fatty acid triglyceride is used as a carrying agent, first-stage extraction is carried out, the extraction temperature is 36-46 DEG C, and the extraction pressure is 25-29 Mpa; separating first zanthoxylum oil resin from the extracted material through a rectifying column; the pressure of a rectifying column is 9-21 Mpa, the rectifying column is divided into three sections, the extracted material enters the rectifying column from bottom to top, the temperature of the first section is 40-45 DEG C, the temperature of the second section is 50-55 DEG C, and the temperature of the third section is 60-65 DEG C. The high-quality zanthoxylum oil resin with low bitterness and low precipitate can be obtained by using the method disclosed by the invention, and the zanthoxylum meal after the first-stage extraction can also be subjected to secondary extraction, so that the overall resource utilization rate of the zanthoxylum raw material is improved.

Description

Technical Field

[0001] The invention relates to the technical field of material extraction, in particular to a prickly ash oleoresin and a preparation method and application thereof. Background Art

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

[0003] Most of the existing technologies for preparing Zanthoxylum bungeanum oleoresin are based on solvent extraction or supercritical CO 2 The extraction process is a single process. Solvent extraction is generally costly, complex, and has problems such as excessive residual solvent in the product. Supercritical extraction is carried out at a constant temperature. The carriers generally used are highly polar solvents such as ethanol. The resin obtained by extraction has more highly polar components, and there are unsolvable problems such as poor oil solubility, high bitterness, and high sedimentation.

[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 Zanthoxylum bungeanum oleoresin, rather than producing low-bitter Zanthoxylum bungeanum oleoresin from the Zanthoxylum bungeanum raw material in one step. The 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 refined production technology of low-bitter Zanthoxylum bungeanum oleoresin. Summary of the invention

[0006] One of the purposes of the present invention is to provide a new method for mass-producing high-quality Zanthoxylum bungeanum oleoresin with low bitterness and low sediment.

[0007] The present invention provides a method for preparing pepper oleoresin, comprising 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 to perform first-stage extraction, and then the first pepper oleoresin is separated by rectification; The conditions of the first stage extraction are: extraction temperature 36-46°C, extraction pressure 25-29Mpa; During the first stage of extraction, extraction and distillation are carried out simultaneously, and the extracted material is separated into the first prickly ash oleoresin through a distillation column; the pressure of the distillation column is 9-21Mpa, and 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°C, the temperature of the second section is 50-55°C, and the temperature of the third section is 60-65°C.

[0008] The present invention has found that when the Zanthoxylum bungeanum raw material is extracted and distilled under specific conditions in the presence of a specific carrier, high-quality Zanthoxylum bungeanum oleoresin with low bitterness and low precipitation can be obtained. The operation is simple and suitable for industrial large-scale production.

[0009] The present invention can better remove impurities (such as some macromolecular precipitates that are not easy to separate) and bitter components in the material through the combination of specific segmented extraction and distillation processes, and try to avoid the formation of new bitter components in the distillation stage.

[0010] In the method of the present invention, the distillation column contains conventional fillers in the art (e.g., ceramic corrugated fillers or stainless steel wire mesh corrugated fillers with a pore size of 5-10 microns) to increase the effective area of ​​the feed liquid, which is conducive to the efficient separation of Zanthoxylum bungeanum oleoresin and other components.

[0011] The method of the present invention preferably also includes the step of subjecting the Zanthoxylum bungeanum raw material subjected to the first-stage extraction to a second-stage extraction, and then distilling and separating a second Zanthoxylum bungeanum oleoresin; the conditions of the second-stage extraction are: extraction temperature 55-65° C., extraction pressure 25-29 MPa; the method for distilling and separating the second Zanthoxylum bungeanum oleoresin is the same as the method for distilling and separating the first Zanthoxylum bungeanum oleoresin.

[0012] The present invention extracts the remaining pepper meal after the high-quality pepper oleoresin is prepared by the first-stage extraction under specific conditions in the second stage, so as to obtain pepper oleoresin with a pepper amide content of 21-27%, so that the overall pepper amide content yield is high, and while obtaining high-quality products, the overall utilization rate of raw materials is improved.

[0013] In the method of the present invention, in the first stage of extraction, the carbon dioxide fluid flow rate required for each kilogram of pepper raw material is 10-50L / h; the required mass of the carrying agent is 1-5% of the mass of the pepper raw material; in the second stage of extraction, the carbon dioxide fluid flow rate required for each kilogram of pepper raw material is 10-50L / h.

[0014] In the method of the present invention, the medium-chain fatty acid triglyceride is a 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 triglyceride, capric triglyceride and lauric triglyceride.

[0015] In the method of the present invention, the time of the first stage extraction is 1-2 hours; the time of the second stage extraction is 2-3 hours.

[0016] The method of the present invention also includes the step of separating the remaining materials after separating the first and second prickly ash oleoresins in a separation kettle, wherein the pressure of the separation kettle is 3-7 MPa and the temperature is 30-40°C.

[0017] After the residual materials of the present invention are separated by a separation kettle, prickly ash essential oil (which can be used for the preparation of prickly ash resin), prickly ash oleoresin with low prickly ash amide content and gaseous carbon dioxide (which can be recycled and reused) can be obtained.

[0018] Overall, the total content of prickly ash amide in the low-bitter first prickly ash oleoresin separated from the distillation column after the first stage extraction, the second prickly ash oleoresin separated from the distillation column after the second stage extraction, and the prickly ash oleoresin separated from the separation kettle after the two stages of extraction accounts for more than 95% of the total content of prickly ash amide in the prickly ash raw material.

[0019] The method of the present invention further comprises the step of pre-treating the raw material of Sichuan pepper before the first stage extraction; the pre-treatment comprises deseeding, flaking or crushing; The thickness of the Zanthoxylum bungeanum raw material after slicing is 0.2-0.8 mm; The crushed pepper raw material has a passing rate of 60%-90% on a 20-mesh standard sieve.

[0020] Preferably, the processing temperature during flaking or crushing is 25-40°C.

[0021] Crushing can be done using an automatic crusher with a screen size of 10-20 meshes.

[0022] As a specific preferred embodiment, the supercritical extraction process of Zanthoxylum bungeanum oleoresin of the present invention comprises: (1) pre-treating the Zanthoxylum bungeanum raw material; (2) supercritical fluid treatment: extracting in an extraction kettle, distilling through a supercritical distillation column, and finally passing through a supercritical separation kettle.

[0023] Specifically, after extraction, the extract is discharged from the extraction kettle and enters the supercritical distillation column through the feed port for distillation treatment. The distillation and supercritical extraction are carried out simultaneously, and then the material enters the supercritical separation kettle from the upper port of the distillation column. The extract obtained after the first stage extraction condition treatment is treated by the distillation column, and the high-quality pepper oil resin (first pepper oil resin) with low bitterness and low sediment is released from the distillation column after pressure relief. The pepper oil resin released by the distillation column treatment of the extract obtained after the second stage extraction condition treatment is a common product (second pepper oil resin). The pepper essential oil released from the separation kettle can be used for product preparation, and the carbon dioxide can be recycled and used through the pipeline. The pepper oil resin with low pepper amide content can be used for the preparation of pepper oil products with different content specifications.

[0024] The present invention also provides a Zanthoxylum bungeanum oleoresin, which is prepared by the above method; preferably, the Zanthoxylum bungeanum oleoresin is the first Zanthoxylum bungeanum oleoresin, the content of prickly ash amide in the first Zanthoxylum bungeanum oleoresin is 20-25%, and the mass proportion of the precipitate is 0.1-0.3%.

[0025] The method can prepare Zanthoxylum bungeanum oleoresin which is substantially free of bitterness and has little sediment (good oil solubility). Compared with common Zanthoxylum bungeanum oleoresin, the method can be more convenient to be applied to food and condiments and avoid the generation of unpleasant flavors.

[0026] Generally speaking, the content of prickly ash amide in raw materials is 2.0-2.5%. The prickly ash oleoresin prepared by the present invention significantly increases the content of this active ingredient.

[0027] The invention also provides an application of the method or the prickly ash oleoresin in preparing condiments.

[0028] The present invention also provides a condiment, which comprises the above-mentioned Zanthoxylum bungeanum oleoresin, preferably comprises the first Zanthoxylum bungeanum oleoresin.

[0029] The beneficial effects of the present invention are at least: The method provided by the present invention can efficiently extract high-quality Zanthoxylum bungeanum oleoresin from Zanthoxylum bungeanum raw materials, the bitterness of which is basically eliminated, the sediment content is greatly reduced (oil solubility is good), the operation is simple, and the method is suitable for industrial large-scale production. DETAILED DESCRIPTION

[0030] The preferred embodiments of the present invention will be described in detail below in conjunction with examples. It should be understood that the following examples are provided only for the purpose of illustration and are not intended to limit the scope of the present invention. Those skilled in the art may make various modifications and substitutions to the present invention without departing from the purpose and spirit of the present invention.

[0031] The experimental methods used in the following examples are conventional methods unless otherwise specified. The materials, reagents, etc. used in the following examples are commercially available or prepared according to conventional methods in the art unless otherwise specified.

[0032] In the specific implementation of the present invention, the detection method of prickly ash amide in prickly ash raw material and prickly ash oleoresin refers to GH / T 1291-2020. The filler in the distillation column is a macroporous ceramic composite corrugated filler with a pore size of 8 microns.

[0033] Example 1 This embodiment provides a 1500L supercritical extraction process for Zanthoxylum bungeanum oleoresin, which is as follows: (1) Pretreatment: 400 kg of Sichuan Jinyang deseeded green pepper raw material (with a content of 2.5% of prickly ash) was rolled using a flake mill at a temperature of 32°C and a thickness of 0.5 mm; (2) After pretreatment, feed the material from the feeding port of the supercritical extraction kettle, and continuously pump carbon dioxide through a high-pressure pump at a pumping speed of 12000L / h. Use a carrying agent pump to pump in 12kg of carrying agent (caprylic acid triglyceride, capric acid triglyceride and lauric acid triglyceride with a mass ratio of 1:1:1) at a pumping speed of 8kg / h. The pressure of the extraction kettle is 27MPa, the first stage extraction: the extraction temperature is 41℃, the extraction time is 1.5h, the extraction and distillation are carried out simultaneously, and 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 at a pressure of 15Mpa, and then passes into the separation kettle from the upper port of the distillation column (the pressure in the separation kettle is 5MPa and the temperature is 35℃). After the distillation column is depressurized, the low-bitter prickly ash oil resin is collected, weighing 32.2kg, and the prickly ash amide content is 21.9%; Second stage extraction: The extraction kettle continues to heat up to 60°C, and the pepper raw material after the first stage extraction continues to be extracted under the same carbon dioxide conditions (i.e., the pump speed and extraction pressure are consistent) for 2.5 hours, and the extracted materials enter the distillation column and the separation kettle in turn (the pressure and temperature conditions of the distillation column and the separation kettle are consistent with the first stage). After the distillation column is depressurized, 3.7 kg of pepper oleoresin is collected, with a pepper amide content of 22.8%, and after the separation kettle is depressurized, 51.8 kg of pepper oleoresin is collected, with a pepper amide content of 3.2%. The overall pepper amide content yield is 95.5% (the total pepper amide content in the pepper oleoresin collected from the distillation column after the first stage extraction, the pepper oleoresin collected from the distillation column after the second stage extraction, and the pepper oleoresin collected from the separation kettle after the two stages of extraction accounts for the total pepper amide content in the pepper raw material). The used carbon dioxide is returned to the storage tank through the recovery system for recycling.

[0034] Example 2 This embodiment provides a 1500L supercritical extraction process for Zanthoxylum bungeanum oleoresin, which is as follows: (1) Pretreatment: 400 kg of Sichuan Jinyang deseeded pepper raw material (with a pepper amide content of 2.5%) was rolled using a flake rolling machine at a temperature of 25°C and a thickness of 0.2 mm; (2) After pretreatment, feed the material from the feeding port of the supercritical extraction kettle, and continuously pump carbon dioxide into the kettle through a high-pressure pump at a pumping speed of 20,000 L / h. Use a carrying agent pump to pump in 20 kg of carrying agent caprylic acid glyceride at a pumping speed of 20 kg / h. The pressure of the extraction kettle is 29 MPa, the first stage extraction: the extraction temperature is 36 ° C, the extraction time is 1 hour, the extraction and distillation are carried out simultaneously, and 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 at a pressure of 9 MPa. Then, it is passed into the separation kettle from the upper port of the distillation column (the pressure in the separation kettle is 3 MPa and the temperature is 30 ° C). After the distillation column is depressurized, the low-bitter prickly ash oil resin is collected and obtained, with a weight of 31.5 kg and a prickly ash amide content of 21.0%; Second stage extraction: The extraction kettle continues to heat up to 55°C, and the pepper raw material after the first stage extraction continues to be extracted for 3 hours under the same carbon dioxide conditions (i.e., the pump speed and extraction pressure are consistent). The extracted materials enter the distillation column and the separation kettle in turn (the pressure and temperature conditions of the distillation column and the separation kettle are consistent with the first stage). After the distillation column is depressurized, 8.6 kg of pepper oleoresin is collected and the pepper amide content is 22.3%. After the separation kettle is depressurized, 55.4 kg of pepper oleoresin is collected and the pepper amide content is 1.9%. The overall pepper amide content yield is 95.9%. The used carbon dioxide is returned to the storage tank through the recovery system for recycling.

[0035] Example 3 This embodiment provides a 1500L supercritical extraction process for Zanthoxylum bungeanum oleoresin, which is as follows: (1) Pretreatment: 400 kg of Sichuan Jinyang deseeded pepper raw material (with a pepper amide content of 2.5%) was rolled using a flake mill at a temperature of 40°C and a thickness of 0.8 mm; (2) After pretreatment, feed the material from the feeding port of the supercritical extraction kettle, and continuously pump carbon dioxide through a high-pressure pump at a pumping speed of 4000L / h. Use a carrying agent pump to pump in 4kg of carrying agent capric glyceride at a pumping speed of 2kg / h. The pressure of the extraction kettle is 25MPa, the first stage extraction: the extraction temperature is 46℃, the extraction time is 2h, the extraction and distillation are carried out simultaneously, and 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℃ at a pressure of 21Mpa, and then passes into the separation kettle from the upper port of the distillation column (the pressure in the separation kettle is 7MPa and the temperature is 40℃). After the distillation column is depressurized, the low-bitter prickly ash oil resin is collected and obtained, with a weight of 20.8kg and a prickly ash amide content of 24.5%; Second stage extraction: The extraction kettle continues to heat up to 65°C, and the pepper raw material after the first stage extraction continues to be extracted for 2 hours under the same carbon dioxide conditions (i.e., the pump speed and extraction pressure are consistent). The extracted materials enter the distillation column and the separation kettle in turn (the pressure and temperature conditions of the distillation column and the separation kettle are consistent with the first stage). After the distillation column is depressurized, 3.6 kg of pepper oleoresin is collected and the pepper amide content is 26.7%. After the separation kettle is depressurized, 54.1 kg of pepper oleoresin is collected and the pepper amide content is 6.4%. The overall pepper amide content yield is 95.2%. The used carbon dioxide is returned to the storage tank through the recovery system for recycling.

[0036] Example 4 This embodiment provides a 1500L supercritical extraction process for pepper oleoresin, which is basically the same as the process in Example 1, except that the carrier used is lauric acid triglyceride. The remaining conditions are the same as in Example 1. Finally, in the first stage of extraction, the distillation column is depressurized and collected to obtain low-bitter pepper oleoresin, weighing 32.1 kg and having a pepper amide content of 22.0%; In the second stage of extraction, 3.6 kg of prickly ash oleoresin was collected after the distillation column was depressurized, and the prickly ash amide content was 22.9%. After the separation kettle was depressurized, 51.9 kg of prickly ash oleoresin was collected, and the prickly ash amide content was 3.1%. The overall prickly ash amide content yield was 94.95%.

[0037] Example 5 This embodiment provides a 1500L supercritical extraction process for Zanthoxylum bungeanum oleoresin, which is basically the same as the process in Example 1, except that the raw material used is Chongqing Jiangjin green deseeded green Zanthoxylum bungeanum (with a content of 2.0% of prickly ash). The remaining conditions are the same as those in Example 1.

[0038] Finally, after the first stage of extraction, the low-bitter Zanthoxylum oleoresin was collected after the distillation column was depressurized, weighing 25.2 kg and containing 21.5% Zanthoxylum amide; In the second stage of extraction, 3.5 kg of prickly ash oleoresin was collected after the distillation column was depressurized, and the prickly ash amide content was 21.9%. 53.2 kg of prickly ash oleoresin was collected after the separation kettle was depressurized, and the prickly ash amide content was 2.7%. The overall prickly ash amide content yield was 95.26%.

[0039] Comparative Example 1 This comparative example provides a supercritical extraction process for pepper oleoresin, which is basically the same as Example 1, except that the supercritical extraction temperature in the first stage is 55°C, the pumping speed of the carrying agent and carbon dioxide, and the distillation and separation treatment methods are the same as those in Example 1. After the first stage distillation column is depressurized, 32.5 kg of pepper oleoresin with a pepperamide content of 22.1% are collected, and after the second stage distillation column is depressurized, 3.6 kg of pepper oleoresin with a pepperamide content of 22.5% are collected, and after the separation kettle is depressurized, 51.4 kg of pepper oleoresin with a pepperamide content of 3.1% are collected. The overall pepperamide content yield is 95.9%.

[0040] Comparative Example 2 This comparative example provides a supercritical extraction process for pepper oleoresin, which is basically the same as Example 1, except that no carrying agent is added, 32.4 kg of pepper oleoresin is collected after the first stage distillation column is depressurized, and the pepper amide content is 21.7%, 3.8 kg of pepper oleoresin is collected after the second stage distillation column is depressurized, and the pepper amide content is 22.6%, and 38.7 kg of pepper oleoresin is collected after the separation kettle is depressurized, and the pepper amide content is 4.2%. The overall pepper amide content yield is 95.2%.

[0041] Comparative Example 3 This comparative example provides a supercritical extraction process for pepper oleoresin, which is basically the same as Example 1, except that triacetin is used as a carrier, 32.3 kg of pepper oleoresin is collected after the first stage distillation column is depressurized, and the pepper amide content is 22.2%, 3.5 kg of pepper oleoresin is collected after the second stage distillation column is depressurized, and the pepper amide content is 22.8%, and 51.6 kg of pepper oleoresin is collected after the separation kettle is depressurized, and the pepper amide content is 3.0%. The overall pepper amide content yield is 95.2%.

[0042] Comparative Example 4 This comparative example provides a supercritical extraction process for pepper oleoresin, which is basically the same as Example 1, except that 95% ethanol is used as a carrier, 32.6 kg of pepper oleoresin is collected after the first stage distillation column is depressurized, and the pepper amide content is 21.5%, 3.6 kg of pepper oleoresin is collected after the second stage distillation column is depressurized, and the pepper amide content is 22.7%, and 40.3 kg of pepper oleoresin is collected after the separation kettle is depressurized, and the pepper amide content is 4.3%. The overall pepper amide content yield is 95.6%.

[0043] Comparative Example 5 This comparative example provides a supercritical extraction process for pepper oleoresin, which is basically the same as Example 1, except that the temperature of the distillation column is 50°C, and no temperature gradient is set. After the first stage distillation column is depressurized, 33.0 kg of pepper oleoresin with a pepperamide content of 21.4% is collected, and after the second stage distillation column is depressurized, 3.2 kg of pepper oleoresin with a pepperamide content of 22.4% is collected, and after the separation kettle is depressurized, 51.4 kg of pepper oleoresin with a pepperamide content of 3.3% is collected. The overall pepperamide content yield is 94.8%.

[0044] Comparative Example 6 This comparative example provides a supercritical extraction process for pepper oleoresin, which is basically the same as Example 1, except that the temperature zone of the first stage of the distillation column is 50°C, the temperature zone of the second stage is 60°C, and the temperature zone of the third stage is 70°C. After the first stage distillation column is depressurized, 30.5 kg of pepper oleoresin with a pepper amide content of 23.2% is collected, and after the second stage distillation column is depressurized, 3.3 kg of pepper oleoresin with a pepper amide content of 23.8% is collected, and after the separation kettle is depressurized, 53.2 kg of pepper oleoresin with a pepper amide content of 3.0% is collected. The overall pepper amide content yield is 94.6%.

[0045] Comparative Example 7 This comparative example provides a supercritical extraction process for Zanthoxylum bungeanum oleoresin, which is as follows: (1) Pretreatment: 400 kg of deseeded pepper raw material (with a pepper amide content of 2.5%) was rolled using a flake mill at a temperature of 58°C and a thickness of 0.5 mm; (2) After pretreatment, feed the material from the feeding port of the supercritical extraction kettle, and continuously pump carbon dioxide into the supercritical extraction kettle through a high-pressure pump at a pump speed of 12000L / h, an extraction kettle pressure of 28MPa, an extraction temperature of 60℃, and an extraction time of 4h. The extracted material enters the distillation column at a pressure of 10Mpa and a temperature of 50℃. After passing through the distillation column, the material enters the separation kettle at a pressure of 5Mpa and a temperature of 50℃. After the distillation column is depressurized, 40.8kg of prickly ash oil resin is collected, with a prickly ash amide content of 20.8%. After the separation kettle is depressurized, 33.5kg of prickly ash oil resin is collected, with a prickly ash amide content of 2.9%. The overall prickly ash amide content yield is 94.6%. The used carbon dioxide is returned to the storage tank through the recovery system for recycling.

[0046] Experimental example This experimental example tests the products of each embodiment and comparative example, as follows: 1. Bitterness evaluation Evaluation method: Pepper oleoresin is mixed with pepper essential oil and sunflower oil to prepare a pepper oil product with a pepper amide content of 12% and an essential oil content of 40%. The pepper oil product is then further diluted with sunflower oil to a pepper amide content of 0.15%. Ten sensory evaluators are selected. When evaluating the bitterness, each evaluator uses a 1mL disposable dropper to drop 3 drops of diluted oil to the middle of the tongue each time. The evaluators then record the bitterness score according to the bitterness evaluation form. The average score of the 10 people is used as the bitterness score of the sample (using the pepper oleoresin with the greatest bitterness in the comparative example as a control, the bitterness score is 5 points, and the sunflower oil bitterness score is 0 points. The larger the score, the more bitter the sample). After tasting a sample, rinse your mouth with pure water and evaluate the next sample after an interval of 10 minutes.

[0047] 2. Sedimentation rate Detection method: Mix the pepper oleoresin with the same weight of pepper essential oil. Then weigh the weight of the 15mL centrifuge tube and record it as m 0 ; Then weigh 9.00g of the mixed prickly ash oleoresin in a 15mL centrifuge tube, and record the total weight of the mixed prickly ash oleoresin and the centrifuge tube m 1 Use a high-speed centrifuge to centrifuge at 4000 rpm for 30 min, gently pour out the mixed Zanthoxylum oleoresin on the upper layer of the test tube, then invert the test tube for 2 h, weigh the total weight of the sediment and the test tube, and record it as m 2 , according to (m 2 -m 0 ) / (m 1 -m 0 )×100% to calculate the percentage of sediment, which is the sedimentation rate.

[0048] The test results of the specific embodiments and comparative examples are shown in Table 1 (Comparative Example 7 is a test of collecting the Zanthoxylum bungeanum oleoresin after depressurizing the distillation column).

[0049] Table 1 Although the present invention has been described in detail above with general descriptions and specific embodiments, it is obvious to those skilled in the art that some modifications or improvements may be made thereto based on the present invention. Therefore, these modifications or improvements made without departing from the spirit of the present invention all fall within the scope of protection claimed by the present invention.

Claims

1. A method for preparing Zanthoxylum bungeanum oleoresin, characterized in that: The method comprises the steps of extracting the raw material of Sichuan pepper with a carbon dioxide supercritical fluid; in the extraction, medium-chain fatty acid triglyceride is used as a carrier to perform a first-stage extraction, and then a first Sichuan pepper oleoresin is separated by rectification; The conditions of the first stage extraction are: extraction temperature 36-46°C, extraction pressure 25-29Mpa; During the first stage of extraction, extraction and distillation are carried out simultaneously, and the extracted material is separated into the first prickly ash oleoresin through a distillation column; the pressure of the distillation column is 9-21Mpa, and 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°C, the temperature of the second section is 50-55°C, and the temperature of the third section is 60-65°C.

2. The method according to claim 1, characterized in that The method also includes the step of subjecting the Zanthoxylum bungeanum raw material subjected to the first-stage extraction to a second-stage extraction, and then distilling and separating a second Zanthoxylum bungeanum oleoresin; the conditions for the second-stage extraction are: extraction temperature 55-65° C., extraction pressure 25-29 MPa; and the method for distilling and separating the second Zanthoxylum bungeanum oleoresin is the same as the method for distilling and separating the first Zanthoxylum bungeanum oleoresin.

3. The method according to claim 2, characterized in that In the first stage of extraction, the required carbon dioxide fluid flow rate per kilogram of pepper raw material is 10-50 L / h; the mass of the required carrying agent is 1-5% of the mass of the pepper raw material; in the second stage of extraction, the required carbon dioxide fluid flow rate per kilogram of pepper raw material is 10-50 L / h; And / or, 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 triglyceride, capric triglyceride and lauric triglyceride.

4. The method according to claim 2 or 3, characterized in that: The extraction time of the first stage is 1-2 hours; the extraction time of the second stage is 2-3 hours.

5. The method according to any one of claims 2 to 4, characterized in that: The method also includes the steps of separating the remaining materials after separating the first Zanthoxylum bungeanum oleoresin and the second Zanthoxylum bungeanum oleoresin by using a separation kettle, wherein the pressure of the separation kettle is 3-7 MPa and the temperature is 30-40°C.

6. The method according to any one of claims 1 to 5, characterized in that: The method also includes the step of pre-treating the raw material of Sichuan pepper before the first stage extraction; the pre-treatment includes deseeding, flaking or crushing; The thickness of the Zanthoxylum bungeanum raw material after slicing is 0.2-0.8 mm; The crushed pepper raw material has a passing rate of 60%-90% on a 20-mesh standard sieve.

7. A Zanthoxylum bungeanum oleoresin, characterized in that The method is prepared by any one of claims 1 to 6.

8. The Zanthoxylum bungeanum oleoresin according to claim 7, characterized in that The Zanthoxylum bungeanum oleoresin is the first Zanthoxylum bungeanum oleoresin, the first Zanthoxylum bungeanum oleoresin has a prickly ash amide content of 20-25%, and a precipitate mass proportion of 0.1-0.3%.

9. Use of the method according to any one of claims 1 to 6 or the Zanthoxylum bungeanum oleoresin according to claim 7 or 8 in preparing condiments.

10. A seasoning, characterized in that: Including the Zanthoxylum bungeanum oleoresin according to claim 7 or 8.

Images