Supercritical extraction method for preventing zanthoxylum oil resin from crystallizing

Abstract

The invention relates to the technical field of deep processing of agricultural products, and particularly discloses a supercritical extraction method for preventing zanthoxylum oleoresin from crystallizing, which comprises the following steps of: storing zanthoxylum oleoresin through a vacuum bag by virtue of multiple dehydration and separation procedures, and performing low-temperature separation on the zanthoxylum oleoresin in the vacuum bag to obtain zanthoxylum oleoresin. The zanthoxylum oil resin containing no water and amide substances and the zanthoxylum oil resin product containing pure amide substances are obtained, the zanthoxylum oil resin containing no volatile oil and the zanthoxylum oil resin product containing pure amide substances are independently subjected to cavitation treatment, the stability of the volatile oil content is guaranteed, and the problem that the zanthoxylum oil resin is crystallized in a traditional method is solved. In the process of vacuumizing and re-pressing the zanthoxylum oleoresin to perform cavitation on the zanthoxylum oleoresin, not only is the amide substances subjected to mechanical collapse, but also the content of volatile oil substances is reduced, and the flavor of the zanthoxylum oleoresin is reduced.

Description

Technical Field

[0001] This application relates to the field of agricultural product deep processing technology, and specifically discloses a supercritical extraction method for preventing the crystallization of pepper oleoresin. Background Technology

[0002] Sichuan pepper has a wide range of uses and high economic value, with applications in the food, medical, and industrial fields. Sichuan pepper oleoresin, as a deep-processed product of Sichuan pepper, is a viscous, brown, fluid substance extracted from Sichuan pepper fruits using solvent extraction or supercritical fluid extraction methods.

[0003] However, pepper oleoresin products are prone to freezing at low temperatures, severely affecting their usability. Therefore, existing technologies employ supercritical carbon dioxide extraction methods to prevent pepper oleoresin crystallization, such as the method described in Chinese Patent Publication No. CN113801732B. The method for supercritical extraction crystallization of Sichuan pepper oleoresin includes sequential operations such as distillation to remove water, centrifugation, vacuuming and repressurization to reduce the water content in the Sichuan pepper oleoresin and separate macromolecules such as pectin and polysaccharides. Then, the Sichuan pepper oleoresin is depressurized under constant temperature conditions to induce cavitation, causing the amide substances produced in the Sichuan pepper oleoresin to undergo mechanical collapse and produce irreversible changes. By repeating the operation multiple times, the precipitation of amide substances at low temperatures is prevented, thus allowing the Sichuan pepper oleoresin to be stored for a long time without crystallization.

[0004] However, in the process of vacuuming and repressurizing the pepper oil resin to cavitate it, the volatile nature of the volatile oil in the pepper oil resin not only causes the amide substances to undergo mechanical collapse, but also reduces the content of volatile oil substances and the flavor of the pepper oil resin.

[0005] Therefore, in view of this, the inventors have provided a supercritical extraction method to prevent the crystallization of pepper oleoresin, in order to solve the above-mentioned problems. Summary of the Invention

[0006] The purpose of this invention is to solve the problem that traditional methods for preventing the crystallization of Sichuan pepper oil resin, which involve vacuuming and repressurizing the Sichuan pepper oil resin to cavitate it, not only cause mechanical collapse of amide substances but also reduce the content of volatile oil substances and the flavor of Sichuan pepper oil resin.

[0007] To achieve the above objectives, the basic solution of the present invention provides a supercritical extraction method for preventing the crystallization of Sichuan pepper oleoresin, comprising the following steps: Step S1: Remove impurities from the peppercorn granules, dry them, and then grind them into peppercorn powder; Step S2: Weigh out a quantitative amount of Sichuan pepper powder into the extractor and continuously pass it through a supercritical fluid. The pepper oil resin was obtained by extraction; Step S3: Collect the pepper oleoresin and separate the oil and water in a flowing state to obtain pepper oleoresin free of water. Step S4: The pepper oil resin obtained in step S3 is introduced into a vacuum bag for collection, resulting in bagged pepper oil resin. Step S5: Place the bagged pepper oil resin in a low temperature environment of 0-5℃ to precipitate amide substances and solidify. Discharge the unsolidified pepper oil resin on the top layer separately and store it independently to obtain pepper oil resin without amide substances. Step S6: Place the solidified amide substance in a sealed container, heat it up and make the solidified amide substance flow, evacuate the air in the sealed container to create a negative pressure in the sealed container, stop evacuating when the negative pressure reaches -0.05Mpa, and then instantly restore normal pressure. Repeat the above operation 1-2 times to obtain pure amide substance pepper oil resin. Step S7: Mix pepper oil resin without amides and pepper oil resin with pure amides to obtain the desired pepper oil resin.

[0008] Furthermore, the implementation of step S3 includes the following steps: Step S31: Place filter barrel one, with several filter holes at the bottom of filter barrel one and an oil-water separation filter membrane laid on it. Pour pepper oil resin into filter barrel one, heat filter barrel one to keep the pepper oil resin inside in a flowing state and let it stand, to obtain anhydrous pepper oil resin.

[0009] Furthermore, the implementation of step S3 also includes the following steps: Step S32: Insert a filter tube into the pepper oil resin separated in filter barrel 1, export the pepper oil resin from the bottom of filter barrel 1 and perform tubular centrifugation, collect the top material after centrifugation, and obtain refined pepper oil resin. Step S32: Place filter barrel two. The bottom of filter barrel two has several filter holes and is covered with an oil-water separation filter membrane. Pour refined pepper oil resin into filter barrel two. Heat the inside of filter barrel two to keep the refined pepper oil resin in a flowing state and let it stand to obtain water-free refined pepper oil resin.

[0010] Furthermore, step S4 is specifically implemented as follows: a conduit is inserted into the refined pepper oil resin separated in the second filter barrel, and the refined pepper oil resin is discharged from the bottom of the second filter barrel into a vacuum bag for collection, thereby obtaining bagged pepper oil resin.

[0011] Furthermore, in step S2, the pepper powder is extracted in an extractor at 35°C, 25 MPa, and a carbon dioxide flow rate of 30 ml / min for 2 hours to obtain pepper oleoresin.

[0012] The basic solution of the present invention provides a vacuum bag to realize the supercritical extraction method for preventing the crystallization of pepper oil resin as described above. It includes a vacuum bag body and a feed port opened on one side of the vacuum bag body and connected to a feed pipe. The feed pipe is equipped with a valve. An air hole is opened on one side of the vacuum bag body and is covered by an air cap. When the air cap covers the air hole, the bottom of the air cap is continuous with the inner wall of the vacuum bag.

[0013] The principle and effect of this solution are as follows: Compared with existing technologies, this invention obtains anhydrous Sichuan pepper oil resin through a dehydration separation process, stores the Sichuan pepper oil resin in a vacuum bag, and then performs low-temperature separation on the Sichuan pepper oil resin in the vacuum bag to obtain anhydrous Sichuan pepper oil resin without amide substances and pure amide Sichuan pepper oil resin products. The pure amide Sichuan pepper oil resin without volatile oil is separately subjected to cavitation treatment to ensure the stability of volatile oil content. This solves the problem of traditional methods for preventing Sichuan pepper oil resin crystallization. In the process of vacuuming and repressurizing Sichuan pepper oil resin to perform cavitation, not only does the amide substance undergo mechanical collapse, but it also reduces the content of volatile oil substances and the flavor of Sichuan pepper oil resin. Attached Figure Description

[0014] To more clearly illustrate the technical solutions in the embodiments of this application, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the accompanying drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0015] Figure 1 A flowchart of a supercritical extraction method for preventing the crystallization of Sichuan pepper oleoresin according to an embodiment of this application is shown; Figure 2 The diagram shows the contents of amide substances and volatile oils in the samples and control samples proposed in the embodiments of this application. Figure (a) is a schematic diagram of the contents of amide substances and volatile oils in the three groups of samples, and Figure (b) is a schematic diagram of the contents of amide substances and volatile oils in the three groups of control samples. Detailed Implementation

[0016] To further illustrate the technical means and effects of the present invention in achieving its intended purpose, the following detailed description of the specific implementation methods, structures, features, and effects of the present invention, in conjunction with the accompanying drawings and preferred embodiments, is provided below.

[0017] A supercritical extraction method for preventing the crystallization of Sichuan pepper oleoresin, Example 1 as follows: Figure 1 As shown: Includes the following steps: Step S1: Remove impurities from the peppercorn granules, dry them, and then grind them into peppercorn powder; Step S2: Weigh out a quantitative amount of Sichuan pepper powder into the extractor and continuously pass it through a supercritical fluid. The pepper oil resin was obtained by extraction; Step S3: Collect the pepper oleoresin and separate the oil and water in a flowing state to obtain pepper oleoresin free of water. Step S4: The pepper oil resin obtained in step S3 is introduced into a vacuum bag for collection, resulting in bagged pepper oil resin. Step S5: Place the bagged pepper oil resin in a low temperature environment of 0-5℃ to precipitate amide substances and solidify. Discharge the unsolidified pepper oil resin on the top layer separately and store it independently to obtain pepper oil resin without amide substances. Step S6: Place the solidified amide substance in a sealed container, heat it up and make the solidified amide substance flow, evacuate the air in the sealed container to create a negative pressure in the sealed container, stop evacuating when the negative pressure reaches -0.05Mpa, and then instantly restore normal pressure. Repeat the above operation 1-2 times to obtain pure amide substance pepper oil resin. Step S7: Mix pepper oil resin without amides and pepper oil resin with pure amides to obtain the desired pepper oil resin.

[0018] The implementation of step S3 includes the following steps: Step S31: Place filter barrel one, with several filter holes at the bottom of filter barrel one and an oil-water separation filter membrane laid on it. Pour pepper oil resin into filter barrel one, heat filter barrel one to keep the pepper oil resin inside in a flowing state and let it stand, to obtain anhydrous pepper oil resin.

[0019] The implementation of step S3 also includes the following steps: Step S32: Insert a filter tube into the pepper oil resin separated in filter barrel 1, export the pepper oil resin from the bottom of filter barrel 1 and perform tubular centrifugation, collect the top material after centrifugation, and obtain refined pepper oil resin. Step S32: Place filter barrel two. The bottom of filter barrel two has several filter holes and is covered with an oil-water separation filter membrane. Pour refined pepper oil resin into filter barrel two. Heat the inside of filter barrel two to keep the refined pepper oil resin in a flowing state and let it stand to obtain water-free refined pepper oil resin.

[0020] The specific implementation of step S4 is as follows: insert a conduit into the refined pepper oil resin separated in the second filter barrel, and export the refined pepper oil resin from the bottom of the second filter barrel into a vacuum bag for collection to obtain bagged pepper oil resin. In step S4, the vacuum bag used has the following structure: it includes a vacuum bag body and an inlet port on one side of the vacuum bag body connected to an inlet pipe. A valve is installed on the inlet pipe. An air hole is opened on one side of the vacuum bag body and sealed with an air cap. Specifically, a sealing tube with an internal thread is installed on the air hole, and an external thread that engages with the internal thread is opened on the outer wall of the air cap. After the air cap is screwed into the sealing tube, the bottom of the air cap is continuous with the inner wall of the vacuum bag. In this embodiment, the air cap not only seals the vacuum bag body, but also allows for the separation of refined pepper oil resin. By unscrewing the air cap and inserting a straw into the air hole, the end of the straw is placed under the unsolidified pepper oil resin to absorb the unsolidified pepper oil resin, which is then collected through another vacuum bag.

[0021] Furthermore, in step S2, the Sichuan pepper powder is extracted in an extractor at 35°C, 25 MPa, and a carbon dioxide flow rate of 30 ml / min for 2 hours to obtain Sichuan pepper oleoresin.

[0022] In this embodiment, the desired pepper oleoresin obtained in step S7 was tested according to the detection methods in: GH / T 1290—2020 Determination of Total Pepper Amide Content in Sichuan Pepper and Processed Sichuan Pepper Products by Ultraviolet Spectrophotometry, GH / T 1291—2020 Determination of Total Pepper Amide Content in Sichuan Pepper and Processed Sichuan Pepper Products by High Performance Liquid Chromatography, and GB / T 30385—2013 Determination of Volatile Oil Content in Spices and Seasonings. Three sets of samples were collected, and the contents of amide substances and volatile oils in the three sets of samples are as follows. Figure 2 As shown in Figure (a).

[0023] Comparative Example 1: This includes the pepper oleoresin prepared using the following steps: The pepper oil resin obtained in step S2 is centrifuged in a tubular centrifuge. The top layer of material after centrifugation is collected to obtain refined pepper oil. The refined pepper oil is directly placed into a sealed tank. The air in the sealed tank is evacuated to create a negative pressure in the sealed tank. When the negative pressure reaches -0.05 MPa, the evacuation is stopped, and then the pressure is instantly restored to normal. The above operation is repeated 1-2 times to obtain pepper oil resin.

[0024] Three sets of samples were collected as control samples (Sample 1, Sample 2, and Sample 3). The contents of amide substances and volatile oils in the obtained control samples are as follows: Figure 2 As shown in Figure (b).

[0025] contrast Figure 2As can be seen from Figures (a) and (b) in this paper, the desired pepper oleoresin prepared by the supercritical extraction method for preventing crystallization of pepper oleoresin provided by the present invention contains a significantly higher volatile oil content than pepper oleoresin prepared by conventional methods, and is therefore practical.

[0026] Furthermore, the supercritical extraction method provided by this invention can also obtain pepper oleoresin products without amide substances, pure amide substances, and anhydrous pepper oleoresin products during the preparation of pepper oleoresin, and can obtain a variety of by-products.

[0027] Furthermore, in step S32, the present invention performs secondary dehydration of the refined Sichuan pepper oil, so that the refined Sichuan pepper oil resin collected in the vacuum bag is water-free, and the Sichuan pepper oil resin without amide substances and the pure amide substances obtained by bagging the Sichuan pepper oil resin are both water-free, thus obtaining 100% anhydrous Sichuan pepper oil resin.

[0028] Furthermore, this invention collects pepper oil resin through a vacuum bag and precipitates amide substances at low temperature. The amide substances precipitate at the bottom of the vacuum bag until they are completely separated, yielding pepper oil resin without amide substances and pepper oil resin with pure amide substances. This can be directly separated and obtained without multiple processing steps.

[0029] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some modifications or alterations to the above-disclosed technical content to create equivalent embodiments without departing from the scope of the present invention. Any simple modifications, equivalent changes and alterations made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention shall still fall within the scope of the present invention.

Claims

1. A supercritical extraction method for preventing the crystallization of Sichuan pepper oleoresin, characterized in that, Includes the following steps: Step S1: Remove impurities from the peppercorn granules, dry them, and then grind them into peppercorn powder; Step S2: Weigh out a quantitative amount of Sichuan pepper powder into the extractor and continuously pass it through a supercritical fluid. The pepper oil resin was obtained by extraction; Step S3: Collect the pepper oleoresin and separate the oil and water in a flowing state to obtain pepper oleoresin free of water. Step S4: The pepper oil resin obtained in step S3 is introduced into a vacuum bag for collection, resulting in bagged pepper oil resin. Step S5: Place the bagged pepper oil resin in a low temperature environment of 0-5℃ to precipitate amide substances and solidify. Discharge the unsolidified pepper oil resin on the top layer separately and store it independently to obtain pepper oil resin without amide substances. Step S6: Place the solidified amide substance in a sealed container, heat it up and make the solidified amide substance flow, evacuate the air in the sealed container to create a negative pressure in the sealed container, stop evacuating when the negative pressure reaches -0.05Mpa, and then instantly restore normal pressure. Repeat the above operation 1-2 times to obtain pure amide substance pepper oil resin. Step S7: Mix pepper oil resin without amides and pepper oil resin with pure amides to obtain the desired pepper oil resin.

2. The supercritical extraction method for preventing the crystallization of Sichuan pepper oleoresin according to claim 1, characterized in that, The implementation of step S3 includes the following steps: Step S31: Place filter barrel one, with several filter holes at the bottom of filter barrel one and an oil-water separation filter membrane laid on it. Pour pepper oil resin into filter barrel one, heat filter barrel one to keep the pepper oil resin inside in a flowing state and let it stand, to obtain anhydrous pepper oil resin.

3. The supercritical extraction method for preventing the crystallization of Sichuan pepper oleoresin according to claim 2, characterized in that, The implementation of step S3 also includes the following steps: Step S32: Insert a filter tube into the pepper oil resin separated in filter barrel 1, export the pepper oil resin from the bottom of filter barrel 1 and perform tubular centrifugation, collect the top material after centrifugation, and obtain refined pepper oil resin. Step S32: Place filter barrel two. The bottom of filter barrel two has several filter holes and is covered with an oil-water separation filter membrane. Pour refined pepper oil resin into filter barrel two. Heat the inside of filter barrel two to keep the refined pepper oil resin in a flowing state and let it stand to obtain water-free refined pepper oil resin.

4. The supercritical extraction method for preventing the crystallization of Sichuan pepper oleoresin according to claim 3, characterized in that, The specific implementation of step S4 is as follows: insert a conduit into the refined pepper oil resin separated in the second filter barrel, and guide the refined pepper oil resin from the bottom of the second filter barrel into a vacuum bag for collection to obtain bagged pepper oil resin.

5. The supercritical extraction method for preventing the crystallization of Sichuan pepper oleoresin according to claim 1, characterized in that, In step S2, Sichuan pepper powder is extracted in an extractor at 35°C, 25 MPa, and a carbon dioxide flow rate of 30 ml / min for 2 hours to obtain Sichuan pepper oleoresin.

6. A vacuum bag for implementing the supercritical extraction method for preventing the crystallization of Sichuan pepper oleoresin as described in claim 1, characterized in that, It includes a vacuum bag body and a feed port opened on one side of the vacuum bag body and connected to a feed pipe. The feed pipe is equipped with a valve. An air hole is opened on one side of the vacuum bag body and is covered by an air cover. When the air cover covers the air hole, the bottom of the air cover is continuous with the inner wall of the vacuum bag.

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