A pepper oleoresin and its preparation method

By controlling the content of neo-8-hydroxy-piperidine and total polyphenols in Sichuan pepper oleoresin, and combining supercritical extraction and low molecular weight alcohol treatment, the problems of bitterness and poor oil solubility of Sichuan pepper oleoresin were solved, and high-quality Sichuan pepper oil products were achieved.

CN116602390BActive Publication Date: 2025-12-02CHENGUANG BIOTECH GRP CO LTD +1
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Patent Information

Application Number
CN202310811540.7
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-07-04
Publication Date
2025-12-02
Estimated Expiration
2043-07-04

AI Technical Summary

Technical Problem

Existing technologies for Sichuan pepper oleoresin have problems such as obvious bitterness, poor oil solubility, affecting the quality of seasonings, and insignificant removal of bitter substances.

Method used

By controlling the mass percentage of neo-8-hydroxy-sanshool in Sichuan pepper oleoresin within the range of 0.1-0.2% and the total polyphenol content within the range of 50-80 mg/g, and combining supercritical extraction and low molecular weight alcohol treatment, bitterness was significantly reduced and oil solubility was improved.

Benefits of technology

It significantly reduces the bitterness of Sichuan pepper oleoresin, enhances the numbing sensation, improves oil solubility, and significantly improves product quality, making it suitable for seasoning oils and spicy snack foods.

✦ Generated by Eureka AI based on patent content.

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Patent Text Reader

Abstract

This invention relates to the field of plant extract technology, specifically to a Sichuan pepper oleoresin and its preparation method. In the Sichuan pepper oleoresin of this invention, the mass percentage of neo-8-hydroxy-sanshool is 0.1-0.2%, and the total polyphenol content is 50-80 mg / g. The Sichuan pepper oleoresin and its products of this invention exhibit significantly eliminated bitterness, provide a rapid and prolonged numbing sensation, and demonstrate good oil solubility and no precipitation when blended with salad oil and other oils. This significantly improves product quality and better meets the needs of seasoning oils, spicy foods, and other fields.
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Description

Technical Field

[0001] This invention relates to the field of plant extract technology, and in particular to a pepper oleoresin and its preparation method. Background Technology

[0002] Sichuan pepper (Zanthoxylum bungeanum) is the dried, mature pericarp of plants belonging to the genus Zanthoxylum bungeanum in the Rutaceae family. It is an important spice and medicinal plant. Sichuan pepper is renowned for its aroma and numbing sensation. Its pericarp contains a large amount of volatile components, generally referred to as volatile oils or essential oils, including terpenes, alcohols, ketones, and esters, which give Sichuan pepper its unique aromatic flavor. The pericarp also contains abundant unsaturated fatty acid amides, with sanshool as a representative, possessing a strong stimulating effect. These amides contribute to the numbing sensation of Sichuan pepper. However, Sichuan pepper also has a bitter taste. This bitterness is an internal quality characteristic of Sichuan pepper. After extraction and concentration, the bitterness of Sichuan pepper oleoresin becomes more pronounced. This means that when a large amount of Sichuan pepper oleoresin is added to seasonings, the bitterness becomes more pronounced, and its poor oil solubility leads to precipitation, seriously affecting the quality of the seasonings.

[0003] Sichuan pepper oleoresin is generally extracted using methods such as supercritical fluid extraction, steam distillation, and solvent extraction. However, the Sichuan pepper oleoresin obtained by these commonly used methods all have a noticeable bitter taste and poor oil solubility when diluted with salad oil, resulting in precipitation. This limits the application of blended Sichuan pepper oil in the food and condiment industries. Currently, there are few Sichuan pepper oleoresin and related products that are low in bitterness, high in numbing flavor, and have good oil solubility. Summary of the Invention

[0004] This invention provides a pepper oleoresin and its preparation method.

[0005] Sichuan pepper oil is obtained by blending Sichuan pepper oleoresin and Sichuan pepper essential oil in a certain proportion. The flavor of Sichuan pepper oil is mainly contributed by Sichuan pepper essential oil, while Sichuan pepper oleoresin is the main source of the numbing and bitter taste of Sichuan pepper oil. Sichuan pepper oleoresin is mainly composed of fatty acid amides such as hydroxy-sanshool, sanshool, and sanshool, lignin, flavonoids, fatty acids, diglycerides (DG), and triglycerides (TG). Currently, research on the substances that produce bitterness in Sichuan pepper oleoresin is still limited, which increases the difficulty of removing bitterness from Sichuan pepper oleoresin. In the process of developing low-bitterness Sichuan pepper oleoresin, this invention unexpectedly discovered that by controlling the mass percentage of neo-8-hydroxy-sanshool within the range of 0.1-0.2% and the total polyphenol content within the range of 50-80 mg / g, the bitterness of Sichuan pepper oleoresin can be significantly reduced. However, when the content of neo-8-hydroxy-sanshool and total polyphenols exceeds the above range, the bitterness of Sichuan pepper oleoresin is significantly increased. The above findings were made by the applicant through a large-sample study during the long-term research and development and production of pepper oleoresin, and have good universality.

[0006] Specifically, the present invention provides the following technical solutions:

[0007] This invention provides a pepper oil resin, wherein the pepper oil resin contains 0.1-0.2% by mass of neo-8-hydroxy-piperazine and 50-80 mg / g of total polyphenols.

[0008] In this invention, the structural formula of the novel 8-hydroxy-piperidine is shown in formula (I), and its molecular formula is C1. 16 H 27 NO5 has a molecular weight of 313.1889.

[0009]

[0010] Preferably, the zanthoxylum oleoresin contains 0.12-0.2% by mass of neo-8-hydroxy-piperidine and 50-70 mg / g of total polyphenols.

[0011] In the aforementioned Sichuan pepper oleoresin, the mass percentage of thiamethoxam is 0.2-0.5% (preferably 0.3-0.5%). Controlling the thiamethoxam content within the above range can significantly improve the numbing flavor of the Sichuan pepper oleoresin, while also making it easier to control the bitterness.

[0012] By simultaneously controlling the contents of the new 8-hydroxy-sanshool, total polyphenols, and sanshoolamide within the above-mentioned range, the bitterness of sanshool oleoresin can be significantly reduced, the numbing sensation of sanshool oleoresin can be enhanced, and sanshool oleoresin can be given a good flavor and taste.

[0013] The present invention provides a method for preparing the above-mentioned pepper oleoresin, the method comprising: first removing the seeds and pressing the pepper raw material into tablets, then performing supercritical extraction to obtain crude pepper oleoresin, mixing the crude pepper oleoresin with a low molecular weight alcohol, and collecting the pepper oleoresin layer by separation.

[0014] Currently, methods for removing bitterness from natural extracts mainly include water treatment, brine treatment, and additive methods. However, brine and water treatment methods are not very effective in removing bitterness from Sichuan pepper oleoresin. This invention has explored various methods for removing bitterness from Sichuan pepper oleoresin and found that after pressing the raw Sichuan pepper into tablets, supercritical extraction followed by low-molecular-weight alcohol treatment not only controls the content of neo-8-hydroxy-sanshool and total polyphenols within the aforementioned ranges, significantly reducing the bitterness of the obtained Sichuan pepper oleoresin, but also retains more of the numbing substances in the oleoresin, significantly reducing the loss of numbing substances. However, if low-molecular-weight alcohol extraction is performed before supercritical extraction, the removal of bitterness and the retention of numbing flavor are significantly reduced.

[0015] In the above method, the moisture content of the Sichuan pepper raw material after tableting is 5-10%. This invention has found that when the moisture content of the Sichuan pepper raw material used for supercritical extraction is too high, bitter substances (such as neo-8-hydroxy-sanshool) in the Sichuan pepper raw material will be extracted into the Sichuan pepper oleoresin, increasing the bitterness of the oleoresin and resulting in poor oil solubility. Conversely, when the moisture content is too low, the extraction efficiency of the Sichuan pepper oleoresin decreases, and the yield of ephedrine is low. By controlling the moisture content of the Sichuan pepper raw material to the range of 5-10% through pretreatment, the extraction of bitter substances can be reduced, and the oil solubility of the resin can be increased.

[0016] In the above method, the seed content of the pepper raw material after seed removal is ≤5%.

[0017] In the above method, the supercritical extraction pressure is 20-25 MPa, the extraction temperature is 54-56℃, and the extraction time is 1-4 h.

[0018] In the above method, the separation pressure of the supercritical extraction is 6-9 MPa, the separation temperature is 44-46℃, and the carbon dioxide flow rate is 280-300 L / h.

[0019] By controlling the supercritical extraction conditions within the above range, bitter substances in Sichuan pepper oleoresin can be significantly removed, and the oil solubility of the product can be improved. In particular, compared with extraction using higher pressure (such as 28-35 MPa, extraction for 1-4 hours), low-pressure extraction using 20-25 MPa is more conducive to controlling the content of new 8-hydroxy-piperidine and polyphenols that cause bitterness in Sichuan pepper oleoresin, significantly reducing bitterness, and improving the oil solubility of the product.

[0020] In the above method, the low molecular weight alcohol is one or more of methanol, ethanol, and isopropanol.

[0021] Preferably, the concentration of the low molecular weight alcohol is 20-50%. This invention has found that treating supercritical fluid extracted Sichuan pepper oleoresin with low molecular weight alcohol within the above concentration range can significantly improve the numbing sensation of the Sichuan pepper oleoresin, while also facilitating the further removal of bitter substances (such as neo-8-hydroxy-sanshool and polyphenols).

[0022] More preferably, the low molecular weight alcohol is ethanol with a concentration of 25-35°.

[0023] In the above method, the crude pepper oleoresin is mixed with a low molecular weight alcohol and stirred at 40-50℃ for 20-40 minutes, and the pepper oleoresin layer is collected.

[0024] The aforementioned low-molecular-weight alcohol treatment step works well in conjunction with the supercritical extraction step to reduce the content of bitter substances in Sichuan pepper oleoresin, alleviate its bitterness, and at the same time increase the content of ephedrine, ensuring a high degree of numbing sensation and resin extraction yield.

[0025] After collecting the pepper oil resin layer, the method further includes a step of concentrating and desolventizing the collected pepper oil resin layer.

[0026] Preferably, the solvent concentration and removal is carried out at a temperature of 55-60°C and a pressure of -0.08 to -0.09 MPa until the solvent content is below 50 ppm.

[0027] By mixing the pepper oil resin of the present invention with pepper essential oil, a pepper oil product with both pepper numbing and aroma can be obtained.

[0028] This invention provides a Sichuan pepper oil product, which includes the Sichuan pepper oil resin described above, and also includes Sichuan pepper essential oil.

[0029] Preferably, in the pepper oil product, the mass ratio of pepper oleoresin to pepper essential oil is 1:(1-2).

[0030] Preferably, the pepper oil product contains 0.05-0.2% by mass of neo-8-hydroxy-piperazine and 50-80 mg / g of total polyphenols.

[0031] This invention provides the application of the above-described pepper oil resin or pepper oil product in the preparation of food or seasonings.

[0032] The present invention also provides a method for reducing the bitterness of Sichuan pepper oleoresin, the method comprising: adjusting the mass percentage content of neo-8-hydroxy-piperazine in Sichuan pepper oleoresin to 0.1-0.2%, and the content of total polyphenols to 50-80 mg / g.

[0033] Preferably, the method further includes adjusting the mass percentage content of zanubrutinib in the zanubrutinib oleoresin to 0.2-0.5%.

[0034] The beneficial effects of the present invention are as follows: the bitterness of the pepper oil resin and its products is significantly eliminated, the numbing sensation is quick and long-lasting, and the pepper oil resin and its products have good oil solubility and no precipitation after being mixed with salad oil and other oils, thus significantly improving the product quality and better meeting the needs of the fields of seasoning oil, spicy snack food, etc.

[0035] The method for preparing pepper oleoresin of the present invention results in pepper oleoresin and its products with significantly eliminated bitterness, rapid and long-lasting numbing sensation, and good oil solubility with salad oil and other oils after blending, without precipitation. This method has the advantages of simple process flow, low cost, and easy implementation of continuous industrial production. Detailed Implementation

[0036] To make the objectives, technical solutions, and advantages of this invention clearer, the technical solutions of this invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of this invention, not all embodiments. Based on the embodiments of this invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this invention.

[0037] In the following examples and comparative examples, the bitterness and numbing sensation of Sichuan pepper oil were evaluated using a quantitative descriptive analysis method. Sensory evaluation personnel were trained according to GB / T1629.1-2012 "General Guidelines for the Selection, Training and Management of Sensory Evaluators Part 1: Selection of Evaluators," and a sensory evaluation team of 10 individuals aged 25 to 30 (5 males and 5 females) was established. The indoor temperature was 25±2℃ and the humidity was 40±3%. Sichuan pepper oil was diluted with sunflower seed oil to a numbing level of 1.5 and placed in tasting cups. Samples were randomly numbered using Arabic numbing numbers, and sensory attributes of the samples were scored, including bitterness intensity, speed of bitterness onset, and duration of bitterness. The intensity, speed of bitterness onset, and duration of bitterness were all scored on a 5-point scale. The data results were analyzed using analysis of variance.

[0038] In the following examples and comparative examples, the content of neo-8-hydroxy-sanshool was determined by Q-TOF-LC / MS, the total polyphenol content was determined by spectrophotometry, and the sanshoolamide was detected by ultraviolet spectrophotometry.

[0039] The Sichuan peppercorns used in the following examples and comparative examples are from the same batch and source.

[0040] Example 1

[0041] This embodiment provides a pepper oil resin, wherein the mass percentage of neo-8-hydroxy-piperidine is 0.15%, the total polyphenol content is 63 mg / g, and the mass percentage of pepper amide is 0.35%.

[0042] This embodiment also provides a method for preparing the above-mentioned pepper oleoresin, the steps of which are as follows:

[0043] (1) The pepper raw material was deseeded and pressed into tablets. After processing, the pepper raw material had a seed content of 3% and a moisture content of 6%.

[0044] (2) Extract the pepper raw material after step (1) under a pressure of 22 MPa and a temperature of 55°C for 2 hours, and then separate it under a pressure of 8 MPa, a temperature of 45°C and a carbon dioxide flow rate of 280 L / h, and collect the pepper oil resin in the separation vessel.

[0045] (3) Mix the pepper oil resin collected in step (2) with 25° ethanol, stir at 45° for 30 min, collect the pepper oil resin layer, and obtain 15.9g of pepper oil resin layer.

[0046] (4) The pepper oil resin layer from step (3) is concentrated and the solvent is removed at a temperature of 55°C and a pressure of -0.09MPa until the solvent content is below 50ppm to obtain pepper oil resin.

[0047] Tests showed that the pepper oleoresin prepared by the above method had a 2.5% increase in unit numbing effect and an extraction yield of 95.98%.

[0048] This embodiment also provides a pepper oil product obtained by blending the pepper oleoresin obtained above with pepper essential oil at a mass ratio of 1:1.15.

[0049] The Sichuan pepper oil product prepared in this embodiment was subjected to sensory evaluation. The Sichuan pepper oil was diluted with sunflower seed oil to 1.5 degrees of numbing sensation for evaluation. The results showed (see Table 1, where "before treatment" refers to Sichuan pepper raw materials that were directly processed by pressing, and "after treatment" refers to Sichuan pepper oil products prepared by the method of this embodiment). The bitterness of the Sichuan pepper oil product was significantly reduced, with almost no bitterness. The numbing sensation was quick to develop and lasted for a long time.

[0050] Table 1. Sensory evaluation results of Sichuan pepper oil before and after treatment.

[0051]

[0052] Furthermore, the pepper oleoresin prepared in this embodiment was diluted with salad oil at a mass ratio of 1:60. The results showed that no precipitation was produced after dilution, and the solution was clear and transparent.

[0053] Example 2

[0054] This embodiment provides a pepper oil resin, wherein the mass percentage of neo-8-hydroxy-piperidine is 0.18%, the total polyphenol content is 70 mg / g, and the mass percentage of pepper amide is 0.39%.

[0055] This embodiment also provides a method for preparing the above-mentioned pepper oleoresin, the steps of which are as follows:

[0056] (1) The pepper raw material was deseeded and pressed into tablets. After processing, the pepper raw material had a seed content of 3% and a moisture content of 10%.

[0057] (2) Extract the pepper raw material after step (1) under a pressure of 24 MPa and a temperature of 54°C for 2 hours, and then separate it under a pressure of 8.5 MPa, a temperature of 44°C and a carbon dioxide flow rate of 290 L / h, and collect the pepper oil resin in the separation vessel.

[0058] (3) Mix the pepper oil resin collected in step (2) with 25° ethanol, stir at 45° for 30 min, collect the pepper oil resin layer, and obtain 15.5g of pepper oil resin layer.

[0059] (4) The pepper oil resin layer from step (3) is concentrated and the solvent is removed at a temperature of 55°C and a pressure of -0.09MPa until the solvent content is below 50ppm to obtain pepper oil resin.

[0060] Tests showed that the pepper oleoresin prepared by the above method increased the unit numbing effect by 2.7%, and the extraction yield was 96.37%.

[0061] This embodiment also provides a pepper oil product obtained by blending the pepper oleoresin obtained above with pepper essential oil at a mass ratio of 1:1.13.

[0062] The Sichuan pepper oil product prepared in this embodiment was subjected to sensory evaluation. The Sichuan pepper oil was diluted with sunflower seed oil to 1.5 degrees of numbing sensation for evaluation. The results showed (see Table 2, where "before treatment" refers to Sichuan pepper raw materials that were directly processed by pressing, and "after treatment" refers to Sichuan pepper oil products prepared by the method of this embodiment). The bitterness of the Sichuan pepper oil product was significantly reduced, with almost no bitterness. The numbing sensation was quick to develop and lasted for a long time.

[0063] Table 2. Sensory evaluation results of Sichuan pepper oil before and after treatment.

[0064]

[0065] Furthermore, the pepper oleoresin prepared in this embodiment was diluted with salad oil at a mass ratio of 1:60. The results showed that no precipitation was produced after dilution, and the solution was clear and transparent.

[0066] Example 3

[0067] This embodiment provides a pepper oil resin, wherein the mass percentage of neo-8-hydroxy-piperidine is 0.13%, the total polyphenol content is 55 mg / g, and the mass percentage of pepper amide is 0.42%.

[0068] This embodiment also provides a method for preparing the above-mentioned pepper oleoresin, the steps of which are as follows:

[0069] (1) The pepper raw material was deseeded and pressed into tablets. After processing, the pepper raw material had a seed content of 3% and a moisture content of 10%.

[0070] (2) Extract the pepper raw material after step (1) under a pressure of 22 MPa and a temperature of 55°C for 2 hours, and then separate it under a pressure of 8 MPa, a temperature of 45°C and a carbon dioxide flow rate of 280 L / h, and collect the pepper oil resin in the separation vessel.

[0071] (3) Mix the pepper oil resin collected in step (2) with 35° ethanol, stir at 50° for 20 min, collect the pepper oil resin layer, and obtain 14.5g of pepper oil resin layer.

[0072] (4) The pepper oil resin layer from step (3) is concentrated and the solvent is removed at a temperature of 55°C and a pressure of -0.09MPa until the solvent content is below 50ppm to obtain pepper oil resin.

[0073] Tests showed that the pepper oleoresin prepared by the above method increased the unit numbing effect by 2.9%, and the extraction yield was 95.22%.

[0074] This embodiment also provides a pepper oil product obtained by blending the pepper oleoresin obtained above with pepper essential oil at a mass ratio of 1:1.1.

[0075] The Sichuan pepper oil product prepared in this embodiment was subjected to sensory evaluation. The Sichuan pepper oil was diluted with sunflower seed oil to 1.5 degrees of numbing sensation for evaluation. The results showed (see Table 3, where "before treatment" refers to Sichuan pepper raw materials that were directly processed by pressing, and "after treatment" refers to Sichuan pepper oil products prepared by the method of this embodiment). The bitterness of the Sichuan pepper oil product was significantly reduced, with almost no bitterness. The numbing sensation was quick to develop and lasted for a long time.

[0076] Table 3. Sensory evaluation results of Sichuan pepper oil before and after treatment.

[0077]

[0078]

[0079] Furthermore, the pepper oleoresin prepared in this embodiment was diluted with salad oil at a mass ratio of 1:60. The results showed that no precipitation was produced after dilution, and the solution was clear and transparent.

[0080] Comparative Example 1

[0081] This comparative example provides a pepper oil resin, wherein the mass percentage of neo-8-hydroxy-piperidine is 0.35%, the total polyphenol content is 85 mg / g, and the mass percentage of pepper amide is 0.42%.

[0082] This comparative example also provides a method for preparing the above-mentioned pepper oleoresin, the steps of which are as follows:

[0083] (1) The pepper raw material was deseeded and pressed into tablets. After processing, the pepper raw material had a seed content of 3% and a moisture content of 6%.

[0084] (2) Extract the pepper raw material after step (1) under pressure of 28 MPa and temperature of 55℃ for 2 hours, and separate it under pressure of 8 MPa, temperature of 45℃ and carbon dioxide flow rate of 280 L / h, and collect the pepper oil resin in the separation vessel.

[0085] (3) Mix the pepper oil resin collected in step (2) with 25° ethanol, stir at 45° for 30 min, collect the pepper oil resin layer, and obtain 17g of pepper oil resin layer.

[0086] (4) The pepper oil resin layer from step (3) is concentrated and the solvent is removed at a temperature of 55°C and a pressure of -0.09MPa until the solvent content is below 50ppm to obtain pepper oil resin.

[0087] Tests showed that the pepper oleoresin prepared by the above method increased the unit numbing effect by 1.5%, and the extraction yield was 96.95%.

[0088] This comparative example also provides a Sichuan pepper oil product obtained by blending the Sichuan pepper oleoresin obtained above with Sichuan pepper essential oil at a mass ratio of 1:1.15.

[0089] Sensory evaluation was conducted on the Sichuan pepper oil products prepared in this comparative example. The Sichuan pepper oil was diluted with sunflower seed oil to 1.5 degrees of numbing sensation for evaluation. The results showed (see Table 4, where "before treatment" refers to Sichuan pepper raw materials that have been directly processed by pressing, and "after treatment" refers to Sichuan pepper oil products prepared by the method of this comparative example) that the Sichuan pepper oil products have a distinct bitter taste, and the bitterness is quick to develop and lasts for a long time.

[0090] Table 4. Sensory evaluation results of Sichuan pepper oil before and after treatment.

[0091]

[0092] Furthermore, the pepper oleoresin prepared in this comparative example was diluted with salad oil at a mass ratio of 1:60. The results showed that the diluted product was not clear and transparent.

[0093] Comparative Example 2

[0094] This comparative example provides a pepper oil resin, wherein the mass percentage of neo-8-hydroxy-piperidine is 0.30%, the total polyphenol content is 95 mg / g, and the mass percentage of pepper amide is 0.39%.

[0095] This comparative example also provides a method for preparing the above-mentioned pepper oleoresin, the steps of which are as follows:

[0096] (1) The pepper raw material was deseeded and pressed into tablets. After processing, the pepper raw material had a seed content of 3% and a moisture content of 20%.

[0097] (2) Extract the pepper raw material after step (1) under a pressure of 22 MPa and a temperature of 55°C for 2 hours, and then separate it under a pressure of 8 MPa, a temperature of 45°C and a carbon dioxide flow rate of 280 L / h, and collect the pepper oil resin in the separation vessel.

[0098] (3) Mix the pepper oil resin collected in step (2) with 25° ethanol, stir at 45° for 30 min, collect the pepper oil resin layer, and obtain 18g of pepper oil resin layer.

[0099] (4) The pepper oil resin layer from step (3) is concentrated and the solvent is removed at a temperature of 55°C and a pressure of -0.09MPa until the solvent content is below 50ppm to obtain pepper oil resin.

[0100] Tests showed that the pepper oleoresin prepared by the above method increased the unit numbing effect by 2.0%, and the extraction yield was 97.32%.

[0101] This comparative example also provides a Sichuan pepper oil product obtained by blending the Sichuan pepper oleoresin obtained above with Sichuan pepper essential oil at a mass ratio of 1:1.15.

[0102] Sensory evaluation was conducted on the Sichuan pepper oil products prepared in this comparative example. The Sichuan pepper oil was diluted with sunflower seed oil to 1.5 degrees of numbing sensation for evaluation. The results showed (see Table 5, where "before treatment" refers to Sichuan pepper raw materials that have been directly processed by pressing, and "after treatment" refers to Sichuan pepper oil products prepared by the method of this comparative example) that the Sichuan pepper oil products had obvious bitterness and the bitterness lasted for a long time.

[0103] Table 5. Sensory evaluation results of Sichuan pepper oil before and after treatment.

[0104]

[0105] Furthermore, the pepper oleoresin prepared in this comparative example was diluted with salad oil at a mass ratio of 1:60. The results showed that some sediment was produced after dilution, and the product was not clear and transparent.

[0106] Comparative Example 3

[0107] This comparative example provides a pepper oil resin, wherein the mass percentage of neo-8-hydroxy-piperidine is 0.35%, the total polyphenol content is 95 mg / g, and the mass percentage of pepper amide is 0.36%.

[0108] This comparative example also provides a method for preparing the above-mentioned pepper oleoresin, the steps of which are as follows:

[0109] (1) The pepper raw material was deseeded and pressed into tablets. After processing, the pepper raw material had a seed content of 3% and a moisture content of 6%.

[0110] (2) Extract the pepper raw material after step (1) under a pressure of 22 MPa and a temperature of 55°C for 2 hours, and then separate it under a pressure of 8 MPa, a temperature of 45°C and a carbon dioxide flow rate of 280 L / h, and collect the pepper oil resin in the separation vessel.

[0111] (3) Mix the pepper oil resin collected in step (2) with 10° ethanol, stir at 45° for 30 min, collect the pepper oil resin layer, and obtain 18.5g of pepper oil resin layer.

[0112] (4) The pepper oil resin layer from step (3) is concentrated and the solvent is removed at a temperature of 55°C and a pressure of -0.09MPa until the solvent content is below 50ppm to obtain pepper oil resin.

[0113] Tests showed that the pepper oleoresin prepared by the above method had a 1.2% increase in unit numbing effect and an extraction yield of 96.53%.

[0114] This comparative example also provides a Sichuan pepper oil product obtained by blending the Sichuan pepper oleoresin obtained above with Sichuan pepper essential oil at a mass ratio of 1:1.15.

[0115] Sensory evaluation was conducted on the Sichuan pepper oil products prepared in this comparative example. The Sichuan pepper oil was diluted with sunflower seed oil to 1.5 degrees of numbing sensation for evaluation. The results showed (see Table 6, where "before treatment" refers to Sichuan pepper raw materials that have been directly processed by pressing, and "after treatment" refers to Sichuan pepper oil products prepared by the method of this comparative example) that the Sichuan pepper oil products have a distinct bitter taste, and the bitterness is quick to develop and lasts for a long time.

[0116] Table 6. Sensory evaluation results of Sichuan pepper oil before and after treatment.

[0117]

[0118] Furthermore, the pepper oleoresin prepared in this comparative example was diluted with salad oil at a mass ratio of 1:60. The results showed that the diluted product was clear and transparent.

[0119] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A pepper oil resin, characterized in that, The zanthoxylum oleoresin contains 0.1-0.2% neo-8-hydroxy-piperazine by mass, 50-80 mg / g total polyphenols, and 0.2-0.5% zanthoxylum amide by mass. The preparation method of the pepper oleoresin includes: first removing the seeds and pressing the pepper raw material into tablets, then extracting it with supercritical carbon dioxide to obtain crude pepper oleoresin, mixing the crude pepper oleoresin with low molecular weight alcohol, stirring at 40-50℃ for 20-40 minutes, separating and collecting the pepper oleoresin layer, and concentrating the collected pepper oleoresin layer to remove the solvent. The moisture content of the Sichuan peppercorn raw material after pressing is 5-10%. The supercritical carbon dioxide extraction is performed at an extraction pressure of 20-25 MPa, an extraction temperature of 54-56℃, and an extraction time of 1-4 h; the supercritical carbon dioxide extraction is performed at a separation pressure of 6-9 MPa, a separation temperature of 44-46℃, and a carbon dioxide flow rate of 280-300 L / h. The low molecular weight alcohol is 25-35° ethanol.

2. The method for preparing the Sichuan pepper oleoresin according to claim 1, characterized in that, The method includes: first removing the seeds and pressing the raw pepper into tablets, then extracting it with supercritical carbon dioxide to obtain crude pepper oleoresin; mixing the crude pepper oleoresin with low molecular weight alcohol and stirring at 40-50℃ for 20-40 minutes; separating and collecting the pepper oleoresin layer; and concentrating the collected pepper oleoresin layer to remove the solvent. The moisture content of the Sichuan peppercorn raw material after pressing is 5-10%. The supercritical carbon dioxide extraction is performed at an extraction pressure of 20-25 MPa, an extraction temperature of 54-56℃, and an extraction time of 1-4 h; the supercritical carbon dioxide extraction is performed at a separation pressure of 6-9 MPa, a separation temperature of 44-46℃, and a carbon dioxide flow rate of 280-300 L / h. The low molecular weight alcohol is 25-35° ethanol.

3. A Sichuan pepper oil product, characterized in that, The pepper oil product comprises the pepper oil resin as described in claim 1, and also comprises pepper essential oil.

4. The Sichuan pepper oil product according to claim 3, characterized in that, In the aforementioned Sichuan pepper oil product, the mass ratio of Sichuan pepper oleoresin to Sichuan pepper essential oil is 1:(1-2).

5. The use of the pepper oil resin of claim 1 or the pepper oil product of claim 3 or 4 in the preparation of food or seasonings.

Citation Information

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