Preparation method of zanthoxylum oil

Abstract

The invention relates to a preparation method of zanthoxylum oil. Specifically, the invention provides a method for increasing the content of active ingredients in zanthoxylum oil and improving the fragrance, taste and / or oxidation stability of the zanthoxylum oil, and the method comprises the following steps: mixing and emulsifying grease and water, extracting whole dry zanthoxylum by using emulsified oil, and filtering out the zanthoxylum to obtain supernate, namely the zanthoxylum oil; wherein in the emulsified oil, the mass of the water is 4-19% of the mass of the grease. According to the method, the volatile oil and the zanthoxylum amide in the zanthoxylum bungeanum can be completely extracted on the premise that the zanthoxylum bungeanum is not crushed, the content of the zanthoxylum amide and representative volatile oil components linalool and limonene in the prepared zanthoxylum bungeanum oil is high, the zanthoxylum bungeanum oil shows rich fragrance and strong numb taste, and the oxidation stability is high.

Description

Technical Field

[0001] This invention relates to condiment processing technology, specifically to a method for preparing Sichuan pepper oil. Background Technology

[0002] Sichuan pepper is a common spice plant, mainly growing in Asia, and is highly sought after for its unique aroma and taste. The flavor compounds of Sichuan pepper are mainly composed of its numbing and aromatic components. The numbing components are primarily salinomycin-like substances, represented by sanshool, which give Sichuan pepper its unique numbing and spicy sensation, causing a tingling or numbing sensation in the mouth and skin, and possessing antibacterial, antioxidant, and anti-inflammatory biological activities. The aromatic components of Sichuan pepper are mainly its volatile oils, which include various olefinic compounds and oxygenated organic hydrocarbons, such as limonene, linalool, linalyl acetate, ocimene, myrcene, and geraniol.

[0003] Edible seasoning oil refers to condiments made from edible vegetable oil, in which flavoring and aromatic substances extracted from edible plants or their seeds are dissolved in the oil. Sichuan pepper oil is a typical example of edible seasoning oil. The main methods for preparing Sichuan pepper oil include oil maceration, solvent extraction, and supercritical carbon dioxide extraction. Among these, oil maceration is currently the mainstream process for large-scale Sichuan pepper oil production due to its simplicity and low cost. However, this method still faces some problems. For example, the grinding of Sichuan pepper and the hot maceration process result in varying degrees of loss of volatile oils, leading to insufficient aroma in the oil. Furthermore, high temperatures can also cause the loss of active ingredients in the Sichuan pepper oil.

[0004] Therefore, there is an urgent need in the field for a method to better extract the active ingredients from Sichuan pepper oil without crushing the peppercorns. Summary of the Invention

[0005] This invention first provides a method for increasing the content of active ingredients in Sichuan pepper oil, improving the aroma and taste of Sichuan pepper oil, and / or its oxidative stability. The method includes: mixing and emulsifying oil and water, extracting whole dried Sichuan peppercorns with the emulsified oil, filtering out the Sichuan peppercorns, and obtaining a supernatant, which is Sichuan pepper oil; wherein, in the emulsified oil, the mass of water is 4-19% of the mass of oil.

[0006] In one or more embodiments, the oil in the emulsified oil is a vegetable oil, preferably selected from one or more of rice bran oil, refined cottonseed oil, palm oil, rapeseed oil, soybean oil, corn oil, peanut oil, sunflower seed oil, flaxseed oil, sesame oil, olive oil, and evening primrose oil, and more preferably from one or more of rapeseed oil, soybean oil, corn oil, and rice bran oil. In one or more embodiments, the oil is one or more of rapeseed oil, soybean oil, corn oil, and rice bran oil. In one or more embodiments, the vegetable oil is a refined vegetable oil, including grade 1, grade 2, grade 3, or grade 4 oil.

[0007] In one or more embodiments, ultrasonic emulsification is used.

[0008] In one or more embodiments, the intensity of ultrasonic emulsification is 0.5–5.0 W / cm. 3 Preferably, it is 1.0–4.0 W / cm². 3 1.5~3.5W / cm 3 Or 2.0~2.7W / cm 3 .

[0009] In one or more embodiments, the ultrasonic emulsification time is 0.5 to 5 min, preferably 0.5 to 1 min or 1 to 3 min.

[0010] In one or more embodiments, the ultrasonic frequency is 15–40 kHz, preferably 15–20 kHz or 20–30 kHz.

[0011] In one or more embodiments, the extraction is carried out in an inert atmosphere at a temperature of 45–55°C.

[0012] In one or more embodiments, the mass of the dried Sichuan peppercorns is 10-20 wt% of the mass of the emulsified oil, preferably 10-12 wt%; or, the mass ratio of the dried Sichuan peppercorns to the oil in the emulsified oil is 1:(5-8), preferably 1:(7-8).

[0013] In one or more embodiments, the extraction is performed using ultrasound.

[0014] In one or more embodiments, the intensity of the ultrasonic extraction is greater than 1.5 W / cm. 3 And less than 4W / cm 3 .

[0015] In one or more embodiments, the frequency of the ultrasonic extraction is 15–30 kHz, preferably 15–20 kHz or 20–30 kHz.

[0016] In one or more embodiments, the ultrasonic extraction time is 5 to 30 minutes, for example 5 to 20 minutes, 25 to 30 minutes, or 15 to 20 minutes.

[0017] In one or more embodiments, the intensity of the ultrasonic extraction is 2.0–3.5 W / cm². 3 2.0~2.7W / cm 3 Or 2.7~3.5W / cm 3 .

[0018] In one or more embodiments, the Sichuan pepper is Qin pepper, Shu pepper, Sichuan pepper or mountain pepper.

[0019] In one or more embodiments, the refining includes at least one step selected from filtration, degumming, dewaxing, deacidification, decolorization, deodorization, degreasing, transesterification, and hydrogenation.

[0020] In one or more embodiments, the method further includes a raw material processing step: screening and / or impurity removal.

[0021] A second aspect of the present invention provides Sichuan pepper oil or an oil composition containing said Sichuan pepper oil prepared by the method as described in any embodiment herein.

[0022] In one or more embodiments, the Sichuan pepper oil contains at least 1.00 mg / mL of linalool, preferably 1.00–2.50 mg / mL; at least 2.50 mg / mL of limonene, preferably 2.50–5.00 mg / mL; at least 6.80 mg / g of limonene, preferably 6.80–8.00 mg / g; and / or has an OSI value of at least 10.00 h, preferably 10.00–15.00 h, at 110°C.

[0023] In one or more embodiments, the oil composition further comprises a vegetable oil, which may be the same as or different from the oil in the emulsified oil, preferably selected from one or more of rice bran oil, refined cottonseed oil, palm oil, rapeseed oil, soybean oil, corn oil, peanut oil, sunflower seed oil, flaxseed oil, sesame oil, olive oil, and evening primrose oil, and more preferably one or more of rapeseed oil, soybean oil, corn oil, and rice bran oil. In one or more embodiments, the vegetable oil is a refined vegetable oil, including grade I, grade II, grade III, or grade IV oil.

[0024] A third aspect of the present invention provides the application of the method described in any embodiment herein in the preparation of Sichuan pepper oil.

[0025] In one or more embodiments, the active ingredients in the Sichuan pepper oil include one or more of the numbing and aromatic components of Sichuan pepper oil.

[0026] In one or more embodiments, the active ingredients in the Sichuan pepper oil include, but are not limited to, one or more of sapinene, limonene, linalool, leaf alcohol, benzaldehyde, linalyl acetate, ocimene, myrcene, geraniol, and zanubrutinamide. Detailed Implementation

[0027] To enable those skilled in the art to understand the features and effects of the present invention, the terms and expressions used in the specification and claims are explained and defined in general below. Unless otherwise specified, all technical and scientific terms used herein have the ordinary meaning understood by those skilled in the art regarding the present invention, and in case of conflict, the definitions in this specification shall prevail.

[0028] The theories or mechanisms described and disclosed herein, whether right or wrong, should not in any way limit the scope of the invention, that is, the contents of the invention can be implemented without being limited by any particular theory or mechanism.

[0029] In this document, the terms “contains,” “includes,” “containing,” and similar terms encompass the meanings of “basically composed of” and “composed of.” For example, when this document discloses “A contains B and C,” “A is basically composed of B and C” and “A is composed of B and C” should be considered as having been disclosed in this document.

[0030] In this document, all features defined by numerical ranges or percentage ranges, such as numerical values, quantities, contents, and concentrations, are for the sake of brevity and convenience only. Accordingly, descriptions of numerical ranges or percentage ranges should be considered as covering and specifically disclosing all possible sub-ranges and individual numerical values ​​(including integers and fractions) within those ranges.

[0031] In this article, "whole dried peppercorns" refers to whole, uncrushed dried peppercorn grains.

[0032] Unless otherwise specified, percentages refer to mass percentages and proportions refer to mass ratios in this article.

[0033] In this article, the sum of the percentages of all components in the composition is 100%.

[0034] In this document, when describing embodiments or examples, it should be understood that it is not intended to limit the invention to those embodiments or examples. Rather, all alternatives, modifications, and equivalents of the methods and materials described herein are covered within the scope defined by the claims.

[0035] For the sake of brevity, not all possible combinations of the technical features in each implementation scheme or embodiment are described herein. Therefore, as long as there is no contradiction in the combination of these technical features, the technical features in each implementation scheme or embodiment can be combined arbitrarily, and all possible combinations should be considered within the scope of this specification.

[0036] The volatile oil in Sichuan peppercorns is lost to varying degrees during the crushing and hot soaking processes, resulting in the loss of active ingredients, including aroma components (such as linalool and limonene) and flavor compounds (such as xanthanamide). However, the inventors have discovered that using water-emulsified oil extraction to prepare Sichuan peppercorn oil allows for better extraction of the volatile oil and its representative volatile oil components, including xanthanamide, linalool, and limonene, without breaking the peppercorns. This enhances the aroma and numbing sensation of the Sichuan peppercorn oil and improves its oxidative stability. This invention thus completes the present invention.

[0037] Sichuan pepper oil and its preparation method

[0038] The present invention first provides a method for preparing Sichuan pepper oil, the method comprising: extracting whole dried Sichuan peppercorns with emulsified oil, filtering out the Sichuan peppercorns, and obtaining the supernatant as Sichuan pepper oil.

[0039] In this article, the emulsified oil is a milky white or pale yellow liquid with no obvious layering, sedimentation or impurities, and uniform color and transparency.

[0040] The method described herein may also include the step of mixing and emulsifying oils and water to obtain an emulsified oil.

[0041] The present invention does not impose any particular limitation on the oils in the emulsified oil; they can be commonly used vegetable oils in the art. These vegetable oils can be refined vegetable oils, including Grade 1, Grade 2, Grade 3, or Grade 4 oils. The oil types include, but are not limited to, one or more of rice bran oil, refined cottonseed oil, palm oil, rapeseed oil, soybean oil, corn oil, peanut oil, sunflower seed oil, flaxseed oil, sesame oil, olive oil, and evening primrose oil, preferably one or more of rapeseed oil, soybean oil, corn oil, and rice bran oil. The present invention does not impose any particular limitation on the refined vegetable oils; they can be some commonly used refined vegetable oils in the art. The refining process includes at least one step selected from filtration, degumming, dewaxing, deacidification, decolorization, deodorization, degreasing, transesterification, and hydrogenation. Further, the refining process may also include the step of treating the vegetable oil with an oxidizing agent, adsorbent, reducing agent, acidic and / or alkaline reagent. In an exemplary embodiment, dried Sichuan peppercorns are selected for preparation with refined Grade 1 rapeseed oil or refined Grade 1 soybean oil.

[0042] In emulsified oils, more water facilitates emulsification; however, excessive water can negatively impact extraction efficiency and the oxidative stability of the extracted oil. Therefore, the water content can be 4–19% of the oil's mass, such as 5–15% or 5–10%. Emulsification can be carried out at room temperature or room temperature (e.g., 20–25°C). Emulsification methods can include ultrasound, shearing, etc., with ultrasound emulsification being preferred. This paper does not impose specific limitations on emulsification conditions such as emulsification rate and time, as long as a homogeneous emulsified oil without significant stratification or sedimentation is obtained. In some specific embodiments, the intensity of ultrasonic emulsification is 0.5–5.0 W / cm². 3 Preferably, it is 1.0–4.0 W / cm².3 1.5~3.5W / cm 3 Or 2.0~2.7W / cm 3 In an exemplary embodiment, the intensity of ultrasonic emulsification is 1.4–3.6 W / cm. 3 Or 1.8~2.8W / cm 3 The ultrasonic emulsification time is 0.5–5 min, preferably 0.5–1 min or 1–3 min, and the ultrasonic frequency can be 15–40 kHz, preferably 15–20 kHz or 20–30 kHz. Furthermore, commonly used emulsifiers in edible oils cannot be used to obtain emulsified oil; otherwise, after extraction, the emulsifier will be difficult to separate and remove from the emulsified oil.

[0043] In some embodiments, the ultrasonic emulsification frequency is 18–32 kHz, preferably 20–30 kHz, and the intensity is 1.5–3.5 W / cm². 3 Or 2.0~2.7W / cm 3 The ultrasonic emulsification time is 0.8 to 1 minute.

[0044] In the extraction step, whole dried Sichuan peppercorns are added to the emulsified oil and extracted using ultrasound. The extraction temperature is typically 45–55°C. For example, the emulsified oil and dried Sichuan peppercorns can be heated together from room temperature to 45–55°C. The extraction temperature should not be too high or too low, otherwise the extraction efficiency will be affected. Extraction can be carried out in an inert atmosphere, such as nitrogen, helium, argon, or carbon dioxide. The mass of dried Sichuan peppercorns can be 10–20 wt% of the mass of the emulsified oil, preferably 10–12 wt%. Alternatively, the mass ratio of dried Sichuan peppercorns to the oil in the emulsified oil is 1:(5–8), preferably 1:(7–8). The intensity of the ultrasonic extraction is 2.0–3.5 W / cm². 3 For example, 2.0–2.7 W / cm 3 Or 2.7~3.5W / cm 3 The frequency can be 15–30 kHz, preferably 15–20 kHz or 20–30 kHz. Generally, the higher the ultrasonic frequency, the lower the extraction efficiency, so the ultrasonic extraction time can be increased. The ultrasonic extraction time can be selected according to the frequency and intensity of the ultrasound, and can be 5–60 min, for example 5–30 min, 5–20 min, 25–30 min or 15–20 min.

[0045] After extraction, the Sichuan peppercorns are filtered out, and the filtrate is centrifuged to obtain the supernatant oil, which is the Sichuan peppercorn oil discussed in this article. The centrifugation speed can be 3000–7000 rpm, for example, 4000–6000 rpm or 4000–5000 rpm. It should be understood that the supernatant oil obtained after centrifugation does not contain water.

[0046] The complete process for preparing Sichuan pepper oil may optionally include a raw material pretreatment step, such as screening and impurity removal, which typically involves screening out branches, leaves, moldy grains, discolored grains, etc., and removing impurities or dust from the Sichuan pepper.

[0047] Sichuan pepper oil is made primarily from Sichuan peppercorns and vegetable oil.

[0048] This article does not impose any particular restrictions on the source or variety of Sichuan peppercorns. Any Sichuan peppercorns used in this field are acceptable, typically belonging to the Rutaceae family and the Zanthoxylum genus, including but not limited to Qin pepper, Shu pepper, Sichuan pepper, or mountain pepper, such as green Sichuan peppercorns and red Sichuan peppercorns. Dried Sichuan peppercorns are generally preferred, such as dried green Sichuan peppercorns and dried red Sichuan peppercorns, as long as the raw materials meet the requirements of "Grade 1 Dried Sichuan Peppercorns" in GB / T 30391-2013 or "Local Food Safety Standard for Sichuan Peppercorn Oil" in DBS 51 008-2019.

[0049] The vegetable oil in the Sichuan pepper oil can be the same as or different from the oil in the emulsified oil, and can be an oil composition consisting of one or more oils. This invention has no particular limitations; it can be any vegetable oil commonly used in the art. The vegetable oil can be refined vegetable oil, including Grade 1, Grade 2, Grade 3, or Grade 4 oil. Oil types include, but are not limited to, one or more of rice bran oil, refined cottonseed oil, palm oil, rapeseed oil, soybean oil, corn oil, peanut oil, sunflower seed oil, flaxseed oil, sesame oil, olive oil, and evening primrose oil, preferably one or more of rapeseed oil, soybean oil, corn oil, and rice bran oil. This invention does not particularly limit the refined vegetable oil; it can be some commonly used refined vegetable oils in the art. The refining includes at least one step selected from filtration, degumming, dewaxing, deacidification, decolorization, deodorization, degreasing, transesterification, and hydrogenation. Further, the refining may also include the step of treating the vegetable oil with an oxidizing agent, adsorbent, reducing agent, acidic and / or alkaline reagent. In an exemplary embodiment, dried Sichuan pepper is selected and prepared with refined Grade 1 rapeseed oil or refined Grade 1 soybean oil.

[0050] The present invention also provides Sichuan pepper oil prepared by the method described in any embodiment herein, the Sichuan pepper oil having one or more of the following characteristics: the content of linalool in the Sichuan pepper oil is at least 1.00 mg / mL, preferably 1.00 to 2.50 mg / mL; the content of limonene is at least 2.50 mg / mL, preferably 2.50 to 5.00 mg / mL; the content of limonene is at least 6.80 mg / g, preferably 6.80 to 8.00 mg / g; and / or the OSI value of the Sichuan pepper oil at 110°C is at least 10.00 h, preferably 10.00 to 15.00 h.

[0051] Oil composition containing Sichuan pepper oil of the present invention

[0052] In some embodiments, the present invention also provides an oil composition containing Sichuan pepper oil as described in any embodiment herein, such as aromatic essential oils, volatile essential oils, flavoring oils, etc.

[0053] In the oil composition containing the Sichuan pepper oil described herein, other components may be added as needed. While ensuring the full realization of the technical effects of this invention, there are no particular limitations on other components. Specifically, for material safety considerations, other additives in this invention refer to other types of edible oils or nutrients added to improve the nutritional value or appearance of the Sichuan pepper oil. The edible oil may be animal fat.

[0054] In this oil composition, the content of other additives can be adjusted according to actual needs. Generally, the weight of other added oil components is less than 30% of the total weight of the mixed oil, preferably less than 20%, and more preferably less than 10%. Other oils in this oil composition can be vegetable oils and / or animal oils. Vegetable oils can be one or more commonly used in the art, such as rice bran oil, refined cottonseed oil, palm oil, rapeseed oil, soybean oil, corn oil, peanut oil, sunflower oil, flaxseed oil, sesame oil, olive oil, and evening primrose oil, preferably one or more of rapeseed oil, soybean oil, corn oil, and rice bran oil.

[0055] application

[0056] This invention also provides the application of the method for preparing Sichuan pepper oil as described in any embodiment herein in increasing the content of active ingredients in Sichuan pepper oil, improving the aroma and flavor (such as numbing sensation) and / or oxidative stability of Sichuan pepper oil. In this invention, the active ingredients in Sichuan pepper oil include, but are not limited to, one or more of the following: numbing flavor components, volatile oil components, and aroma components. The volatile oil components include olefinic compounds and oxygenated organic hydrocarbons, such as limonene, linalool, linalyl acetate, ocimene, myrcene, and geraniol. Preferably, the volatile oil components include linalool and / or limonene.

[0057] Plant sources of xanthocyanin include the root bark of *Fagara (zanthoxylium) macrophyllum Oliver*, the root bark of *F. xanthoxyloside* Lam., and the pericarp of *F. xanthoxyloside*, all belonging to the Rutaceae family. Therefore, in some embodiments, the present invention also provides a method for improving the extraction rate of xanthocyanin, the method comprising extracting substances containing xanthocyanin using an emulsified oil, wherein the ratio of oil to water in the emulsified oil is as described in any embodiment herein.

[0058] In this article, the taste of Sichuan pepper oil (such as numbing sensation) refers to the sensation caused by the active ingredients in Sichuan pepper stimulating nerve endings in the oral cavity, such as tingling or numbness. Preferably, the active ingredient in the Sichuan pepper is salinomycin.

[0059] In this article, the aroma of Sichuan pepper oil comes from the volatile oil components of Sichuan pepper (such as limonene, linalool, and sabinene), alcohols (leaf alcohol), or aldehydes (benzaldehyde).

[0060] In some embodiments, the active ingredients in the Sichuan pepper oil include one or more of sapinene, limonene, linalool, leaf alcohol, benzaldehyde, linalyl acetate, ocimene, myrcene, geraniol, and zanubrutinamide.

[0061] The present invention has the following beneficial effects:

[0062] This invention provides a method for preparing Sichuan pepper oil. This method can extract the volatile oil and limonene from Sichuan pepper relatively completely without crushing the pepper. The prepared Sichuan pepper oil has a high content of limonene, linalool and limonene, which are representative volatile oil components. It exhibits a rich aroma and strong numbing taste, and has high oxidative stability.

[0063] The present invention will be further described below by way of specific embodiments. It should be understood that these embodiments are merely illustrative and are not intended to limit the scope of the invention. Unless otherwise stated, the methods and reagents used in the embodiments are conventional methods and reagents in the art.

[0064] The following examples and comparative examples use the following methods:

[0065] 1. The determination of oxidative stability (OSI) was carried out in accordance with GB / T 21121-2007. The OSI values ​​of different pepper oils at 110℃ were determined using a Rancimat 743 oil oxidative stability tester.

[0066] 2. The determination of linalool and limonene was performed according to the method of Zhao Zhifeng (Zhao Zhifeng. Study on flavor substances of Sichuan pepper and optimization of Sichuan pepper oil production process. Sichuan University, 2005).

[0067] 3. The determination of pepper amide was based on the local food safety standard for pepper oil, DBS51 / 008-2019.

[0068] 4. Odor Evaluation: Twelve sensory evaluators were randomly selected to smell the peppercorns and score them on the aroma (0-10 points). The scoring criteria were: no obvious peppercorn aroma (<5 points), light aroma (5-7 points), strong aroma (7-9 points), strong aroma, and no off-odor (9-10 points). The final average score of the same peppercorn oil was taken as the final aroma score of that peppercorn oil.

[0069] 5. Taste Evaluation: 12 sensory evaluators were randomly selected to taste the product and score it on a scale of 0-10. The scoring criteria were: no numbing sensation (<5 points), mild numbing sensation (5-7 points), noticeable numbing sensation (7-9 points), and strong numbing sensation (9-10 points). The average score of the scores for the same peppercorn oil was taken as the final taste score of the peppercorn oil.

[0070] Example 1

[0071] Add 5% (by weight) of deionized water to refined Grade 1 rapeseed oil, and perform ultrasonic emulsification at room temperature for 1 minute. The ultrasonic frequency is 20 kHz and the intensity is 2.0 W / cm². 3 After emulsification, whole dried Sichuan peppercorns (1 / 8 the weight of the rapeseed oil) were added and placed together in a sealed ultrasonic reactor. Nitrogen gas was introduced, and the temperature was controlled at 55°C. Ultrasonic extraction was performed for 15 minutes at a frequency of 20 kHz and an intensity of 3.5 W / cm². 3 After extraction, the peppercorn particles were removed by filtration. The filtered liquid was then centrifuged at 4000 rpm, and the supernatant oil was collected to obtain peppercorn oil 1.

[0072] Example 2

[0073] Add 10% (by weight) of deionized water to refined Grade 1 rapeseed oil, and perform ultrasonic emulsification at room temperature for 1 minute. The ultrasonic frequency is 20 kHz and the intensity is 2.0 W / cm². 3 After emulsification, whole dried Sichuan peppercorns (1 / 8 the weight of the rapeseed oil) were added and placed together in a sealed ultrasonic reactor. Nitrogen gas was introduced, and the temperature was controlled at 50°C. Ultrasonic extraction was performed for 15 minutes at a frequency of 20 kHz and an intensity of 2.7 W / cm². 3 After extraction, the peppercorn particles were removed by filtration. The filtered liquid was then centrifuged at 5000 rpm, and the supernatant oil was collected to obtain peppercorn oil 2.

[0074] Example 3

[0075] Add 15% (by weight) of deionized water to refined Grade 1 rapeseed oil, and perform ultrasonic emulsification at room temperature for 1 minute. The ultrasonic frequency is 20 kHz and the intensity is 2 W / cm². 3 After emulsification, whole dried Sichuan peppercorns (1 / 8 the weight of the rapeseed oil) were added and placed together in a sealed ultrasonic reactor. Nitrogen gas was introduced, and the temperature was controlled at 45°C. Ultrasonic extraction was performed for 15 minutes at a frequency of 20 kHz and an intensity of 2.0 W / cm². 3 After extraction, the peppercorn particles were removed by filtration. The filtered liquid was then centrifuged at 6000 rpm, and the supernatant oil was collected to obtain peppercorn oil 3.

[0076] Example 4

[0077] Add 10% (by weight) of deionized water to refined grade 1 soybean oil, and perform ultrasonic emulsification at room temperature for 1 minute. The ultrasonic frequency is 20 kHz and the intensity is 2 W / cm². 3 After emulsification, whole dried peppercorns (1 / 8 the weight of soybean oil) were added and placed together in a sealed ultrasonic reactor. Nitrogen gas was introduced, and the temperature was controlled at 50°C. Ultrasonic extraction was performed for 15 minutes at a frequency of 20 kHz and an intensity of 2.7 W / cm². 3 After extraction, the peppercorn particles were removed by filtration. The filtered liquid was then centrifuged at 5000 rpm, and the supernatant oil was collected to obtain peppercorn oil 4.

[0078] Example 5

[0079] Add 5% (by weight) of deionized water to refined Grade 1 rapeseed oil, and perform ultrasonic emulsification at room temperature for 1 minute. The ultrasonic frequency is 20 kHz and the intensity is 2.5 W / cm². 3 After emulsification, whole dried Sichuan peppercorns (1 / 8 the weight of the rapeseed oil) were added and placed together in a sealed ultrasonic reactor. Nitrogen gas was introduced, and the temperature was controlled at 55°C. Ultrasonic extraction was performed for 15 minutes at a frequency of 20 kHz and an intensity of 3.5 W / cm². 3 After extraction, the peppercorn particles were removed by filtration. The filtered liquid was then centrifuged at 4000 rpm, and the supernatant oil was collected to obtain peppercorn oil 5.

[0080] Example 6

[0081] Add 5% (by weight) of deionized water to refined Grade 1 rapeseed oil, and perform ultrasonic emulsification at room temperature for 2 minutes. The ultrasonic frequency is 30 kHz and the intensity is 1.5 W / cm². 3 After emulsification, whole dried Sichuan peppercorns (1 / 8 the weight of the rapeseed oil) were added and placed together in a sealed ultrasonic reactor. Nitrogen gas was introduced, and the temperature was controlled at 55°C. Ultrasonic extraction was performed for 15 minutes at a frequency of 20 kHz and an intensity of 3.5 W / cm². 3 After extraction, the peppercorn particles were removed by filtration. The filtered liquid was then centrifuged at 4000 rpm, and the supernatant oil was collected to obtain peppercorn oil 6.

[0082] Example 7

[0083] Add 5% (by weight) of deionized water to refined Grade 1 rapeseed oil, and perform ultrasonic emulsification at room temperature for 1 minute. The ultrasonic frequency is 20 kHz and the intensity is 2 W / cm². 3After emulsification, whole dried Sichuan peppercorns (1 / 8 the weight of the rapeseed oil) were added and placed together in a sealed ultrasonic reactor. Nitrogen gas was introduced, and the temperature was controlled at 55°C. Ultrasonic extraction was performed for 30 minutes at a frequency of 30 kHz and an intensity of 2.0 W / cm². 3 After extraction, the peppercorn particles were removed by filtration. The filtered liquid was then centrifuged at 4000 rpm, and the supernatant oil was collected to obtain peppercorn oil 7.

[0084] Example 8

[0085] Add 10% (by weight) of deionized water to refined grade 1 rice bran oil, and perform ultrasonic emulsification at room temperature for 1 minute. The ultrasonic frequency is 20 kHz and the intensity is 2.0 W / cm². 3 After emulsification, whole dried Sichuan peppercorns (1 / 8 the weight of the rice bran oil) were added and placed together in a sealed ultrasonic reactor. Nitrogen gas was introduced, and the temperature was controlled at 50°C. Ultrasonic extraction was performed for 15 minutes at a frequency of 20 kHz and an intensity of 2.7 W / cm². 3 After extraction, the peppercorn particles were removed by filtration. The filtered liquid was then centrifuged at 5000 rpm, and the supernatant oil was collected to obtain peppercorn oil 8.

[0086] Comparative Example 1

[0087] Refined first-grade rapeseed oil was heated to 95℃, and then 1 / 8 of the oil's weight of crushed dried Sichuan peppercorns (20 mesh) was added. The mixture was kept warm and extracted for 1 hour. The resulting oil was filtered to obtain Sichuan peppercorn oil 9.

[0088] Comparative Example 2

[0089] Add 3% deionized water to refined first-grade rapeseed oil and perform ultrasonic emulsification at room temperature for 1 minute. The ultrasonic frequency is 20 kHz and the intensity is 2 W / cm. 3 After emulsification, whole dried Sichuan peppercorns (1 / 8 the weight of the rapeseed oil) were added and placed together in a sealed ultrasonic reactor. Nitrogen gas was introduced, and the temperature was controlled at 55°C. Ultrasonic extraction was performed for 15 minutes at a frequency of 20 kHz and an intensity of 3.5 W / cm². 3 After extraction, the peppercorn particles were removed by filtration. The filtered liquid was then centrifuged at 4000 rpm, and the supernatant was collected to obtain peppercorn oil 10.

[0090] Comparative Example 3

[0091] Whole dried Sichuan peppercorns (1 / 8 the weight of the refined first-grade rapeseed oil) were added to the oil and placed together in a sealed ultrasonic reactor. Nitrogen gas was introduced, and the temperature was controlled at 55℃. Ultrasonic extraction was performed for 15 minutes at a frequency of 20kHz and an intensity of 3.5W / cm². 3After extraction, the peppercorn particles were removed by filtration. The filtered liquid was then centrifuged at 4000 rpm, and the supernatant oil was collected to obtain peppercorn oil 11.

[0092] Comparative Example 4

[0093] Add 20% deionized water to refined first-grade rapeseed oil and ultrasonically emulsify at room temperature for 1 minute at a frequency of 20 kHz and an intensity of 2 W / cm². 3 After emulsification, whole dried Sichuan peppercorns (1 / 8 the weight of the rapeseed oil) were added and placed together in a sealed ultrasonic reactor. Nitrogen gas was introduced, and the temperature was controlled at 55°C. Ultrasonic extraction was performed for 15 minutes at a frequency of 20 kHz and an intensity of 3.5 W / cm². 3 After extraction, the peppercorn particles were removed by filtration. The filtered liquid was then centrifuged at 4000 rpm, and the supernatant oil was collected to obtain peppercorn oil 12.

[0094] Comparative Example 5

[0095] Add 10% deionized water to refined first-grade rapeseed oil and perform ultrasonic emulsification at room temperature for 1 minute. The ultrasonic frequency is 20 kHz and the intensity is 2 W / cm. 3 After emulsification, whole dried peppercorns (1 / 8 the weight of the rapeseed oil) were added and placed together in a sealed ultrasonic reactor. Nitrogen gas was introduced, and the temperature was controlled at 40°C. Ultrasonic extraction was performed for 15 minutes at a frequency of 20 kHz and an intensity of 2.7 W / cm². 3 After extraction, the peppercorn particles were removed by filtration. The filtered liquid was then centrifuged at 5000 rpm, and the supernatant oil was collected to obtain peppercorn oil 13.

[0096] Comparative Example 6

[0097] Add 10% deionized water to refined first-grade rapeseed oil and perform ultrasonic emulsification at room temperature for 1 minute. The ultrasonic frequency is 20 kHz and the intensity is 2 W / cm. 3 After emulsification, whole dried Sichuan peppercorns (1 / 8 the weight of the rapeseed oil) were added and placed together in a sealed ultrasonic reactor. Nitrogen gas was introduced, and the temperature was controlled at 65°C. Ultrasonic extraction was performed for 15 minutes at a frequency of 20 kHz and an intensity of 2.7 W / cm². 3 After extraction, the peppercorn particles were removed by filtration. The filtered liquid was then centrifuged at 5000 rpm, and the supernatant oil was collected to obtain peppercorn oil 14.

[0098] Comparative Example 7

[0099] Add 15% deionized water to refined first-grade rapeseed oil and perform ultrasonic emulsification at room temperature for 1 minute. The ultrasonic frequency is 20 kHz and the intensity is 2 W / cm. 3After emulsification, whole dried Sichuan peppercorns (1 / 8 the weight of the rapeseed oil) were added and placed together in a sealed ultrasonic reactor. Nitrogen gas was introduced, and the temperature was controlled at 45°C. Ultrasonic extraction was performed for 15 minutes at a frequency of 20 kHz and an intensity of 1.5 W / cm². 3 After extraction, the peppercorn particles were removed by filtration. The filtered liquid was then centrifuged at 6000 rpm, and the supernatant oil was collected to obtain peppercorn oil 15.

[0100] Comparative Example 8

[0101] Add 15% deionized water to refined first-grade rapeseed oil and perform ultrasonic emulsification at room temperature for 1 minute. The ultrasonic frequency is 20 kHz and the intensity is 2 W / cm. 3 After emulsification, whole dried Sichuan peppercorns (1 / 8 the weight of the rapeseed oil) were added and placed together in a sealed ultrasonic reactor. Nitrogen gas was introduced, and the temperature was controlled at 45°C. Ultrasonic extraction was performed for 15 minutes at a frequency of 20 kHz and an intensity of 4 W / cm². 3 After extraction, the peppercorn particles were removed by filtration. The filtered liquid was then centrifuged at 6000 rpm, and the supernatant oil was collected to obtain peppercorn oil 16.

[0102] Comparative Example 9

[0103] Whole dried Sichuan peppercorns, pre-soaked in deionized water, were added to refined Grade 1 rapeseed oil. The dry weight of the peppercorns was 1 / 8 of the rapeseed oil's weight, and the water absorption of the peppercorns was 10% of the rapeseed oil's weight. The mixture was placed together in a sealed ultrasonic reactor, nitrogen gas was introduced, the temperature was controlled at 50℃, and ultrasonic extraction was performed for 15 minutes at a frequency of 20 kHz and an intensity of 2.7 W / cm². 3 After extraction, the peppercorn particles were removed by filtration. The filtered liquid was then centrifuged at 5000 rpm, and the supernatant oil was collected to obtain peppercorn oil 17.

[0104] The data on the representative active ingredients and flavor substances of Sichuan pepper oil, including linalool, limonene, and Sichuan pepper amide, as well as the antioxidant capacity of Sichuan pepper oil in the above embodiments and comparative examples are listed in Table 1 below.

[0105] Table 1

[0106]

[0107]

[0108] The aroma and taste scores of the Sichuan pepper oils from the above embodiments and comparative examples are listed in Table 2 below.

[0109] Table 2

[0110]

[0111]

[0112] As shown in the table above, the conventional process (Comparative Example 1) yielded a low extraction rate of Sichuan pepper oil, poor oxidative stability, and unsatisfactory sensory evaluation. Examples 1-7 of this application, without crushing the Sichuan pepper, more completely extracted the volatile oil and thiamethoxam from the pepper. The prepared Sichuan pepper oil had higher contents of thiamethoxam and representative volatile oil components such as linalool and limonene, exhibiting a rich aroma and strong numbing flavor, and high oxidative stability. Furthermore, the increased ultrasonic frequency in Example 7 required a longer extraction time. The extraction temperature in Comparative Example 6 was too high; although the extraction rate was high during ultrasonic extraction, the oxidative stability of the resulting oil decreased.

Claims

1. A method for increasing the content of active ingredients in Sichuan pepper oil, improving the aroma, taste, and / or oxidative stability of Sichuan pepper oil, the method comprising: Oil and water are mixed and emulsified, whole dried peppercorns are extracted with the emulsified oil, the peppercorns are filtered out, and the supernatant is obtained, which is peppercorn oil; wherein, the water in the emulsified oil is 4 to 19% of the oil mass.

2. The method as described in claim 1, characterized in that, The oil in the emulsified oil is a vegetable oil, preferably selected from one or more of rice bran oil, refined cottonseed oil, palm oil, rapeseed oil, soybean oil, corn oil, peanut oil, sunflower seed oil, flaxseed oil, sesame oil, olive oil, and evening primrose oil, and more preferably one or more of rapeseed oil, soybean oil, corn oil, and rice bran oil.

3. The method as described in claim 2, characterized in that, Ultrasonic emulsification is used, wherein the ultrasonic emulsification has one or more of the following characteristics; The intensity of ultrasonic emulsification is 0.5–5.0 W / cm. 3 Preferably, it is 1.0–4.0 W / cm². 3 1.5~3.5W / cm 3 Or 2.0~2.7W / cm 3 ; The ultrasonic emulsification time is 0.5–5 min, preferably 0.5–1 min or 1–3 min; and The ultrasonic frequency is 15–40 kHz, preferably 15–20 kHz or 20–30 kHz.

4. The method as described in claim 1, characterized in that, The extraction is carried out in an inert atmosphere at a temperature of 45–55°C.

5. The method as described in claim 4, characterized in that, The mass of the dried Sichuan peppercorns is 10-20 wt% of the mass of the emulsified oil, preferably 10-12 wt%; or, the mass ratio of the dried Sichuan peppercorns to the oil in the emulsified oil is 1:(5-8), preferably 1:(7-8); Preferably, the extraction is performed using ultrasound; preferably, the intensity of the ultrasonic extraction is 2.0–3.5 W / cm. 3 For example, 2.0–2.7 W / cm 3 Or 2.7~3.5W / cm 3 Preferably, the frequency of the ultrasonic extraction is 15-30 kHz, more preferably 15-20 kHz or 20-30 kHz; preferably, the ultrasonic extraction time is 5-60 min, for example 5-20 min, 25-30 min or 15-20 min.

6. The method according to any one of claims 1-5, characterized in that, The Sichuan peppercorns are Qin pepper, Shu pepper, Sichuan pepper, or mountain pepper; and / or The refining process includes at least one step selected from filtration, degumming, dewaxing, deacidification, decolorization, deodorization, degreasing, transesterification, and hydrogenation.

7. The method as described in claim 1, characterized in that, The method also includes a raw material processing step: screening and / or impurity removal.

8. The Sichuan pepper oil or an oil composition containing the Sichuan pepper oil prepared by the method of any one of claims 1-7; Preferably, the linalool content in the Sichuan pepper oil is at least 1.00 mg / mL, preferably 1.00–2.50 mg / mL; the limonene content is at least 2.50 mg / mL, preferably 2.50–5.00 mg / mL; the limonene content is at least 6.80 mg / g, preferably 6.80–8.00 mg / g; and / or the OSI value of the Sichuan pepper oil at 110°C is at least 10.00 h, preferably 10.00–15.00 h. Preferably, the oil composition further contains a vegetable oil, which may be the same as or different from the oil in the emulsified oil, and is preferably selected from one or more of rice bran oil, refined cottonseed oil, palm oil, rapeseed oil, soybean oil, corn oil, peanut oil, sunflower seed oil, flaxseed oil, sesame oil, olive oil, and evening primrose oil, and more preferably from one or more of rapeseed oil, soybean oil, corn oil, and rice bran oil. Preferably, the vegetable oil is a refined vegetable oil, including grade 1, grade 2, grade 3, or grade 4 oil.

9. The application of the method according to any one of claims 1-7 in the preparation of Sichuan pepper oil.

10. The application as described in claim 9, characterized in that, The active ingredients in the Sichuan pepper oil include one or more of the numbing flavor components and the aroma components of Sichuan pepper oil. Preferably, the active ingredients in the Sichuan pepper oil include one or more of sapinene, limonene, linalool, leaf alcohol, benzaldehyde, linalyl acetate, ocimene, myrcene, geraniol, and zanubrutinamide.

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