Spicy oil, preparation method and application

Abstract

The invention belongs to the technical field of food processing, and particularly discloses spicy oil and a preparation method and application thereof.The spicy oil is extracted from fried spicy hotpot condiment through the supercritical carbon dioxide extraction technology, and the supercritical carbon dioxide extraction technology is as follows: the extraction time is 30-50 min, the CO2 flow is 20-40 kg / h, the extraction temperature is 60-70 DEG C, and the extraction pressure is 1.5-3.0 Mpa. Compared with a traditional braising extraction technology, the preparation method has the advantages that the extraction time is obviously shortened, the utilization rate of grease is increased, the capsaicin content of the prepared spicy oil is 80-110 mg / g, the zanthoxylamide content is 60-90 mg / g, the flavor of the spicy oil is richer, and the effective components of the whole flavor are increased by 5.03 times. Seasoning oil conforming to national safety standards can be obtained after the flavor of the spicy oil is further optimized through blending, and the spicy oil can be used for industrial conversion of the spicy oil.

Description

Technical Field

[0001] The invention belongs to the technical field of food processing, and particularly relates to spicy oil, a preparation method and application thereof. Background Art

[0002] Hot pot refers to a cooking method that uses a pot as a utensil, a heat source to burn the pot, and water or soup to boil to cook food. It can be eaten while cooking, or the pot itself has a heat preservation effect, so the food is still steaming hot when eating. Due to the particularity of cooking methods and eating, a large amount of grease, that is, hot pot oil, will be left after each hot pot. Due to the incorporation of more seasoning ingredients, hot pot oil has a special fragrance, which is also considered to be the key to people's love for hot pot. So far, hot pot has spread rapidly across the country with its great inclusiveness and easy improvement. It is most famous for its spicy and fragrant flavors in Sichuan and Chongqing. At the same time, how to effectively extract and apply spicy oil has become a hot spot in the food flavor industry.

[0003] The more popular spicy oils on the market are all made through hot pot frying and stewing and fermentation. Although the spicy flavor can be extracted, its extraction efficiency is low, the stewing and fermentation cycle is long, and it cannot completely restore the original spicy flavor of the hot pot. This has always been a difficult problem in the industry.

[0004] Based on this, the present invention is proposed. Summary of the invention

[0005] Based on the above reasons, one of the purposes of the present invention is to provide a spicy oil and a preparation method thereof. By supercritical carbon dioxide extraction technology, capsaicin and prickly ash amide in hot pot base are fully extracted, and the extraction time of the spicy oil is shortened to obtain spicy and numbing spicy oil; the second purpose of the present invention is to use the prepared spicy oil for making seasonings, and the seasoning oil obtained after flavoring meets the national food safety standards.

[0006] The invention firstly discloses a spicy oil, wherein the capsaicin content of the spicy oil is 80-110 mg / g and the pepperamide content of the spicy oil is 60-90 mg / g.

[0007] The invention also discloses a method for preparing spicy oil, which comprises the following steps: extracting spicy oil from the fried spicy hot pot base by using supercritical carbon dioxide extraction technology.

[0008] Furthermore, the supercritical carbon dioxide extraction technology is as follows: extraction time is 30-50 min, CO2 flow rate is 20-40 kg / h, extraction temperature is 60-70° C., and extraction pressure is 1.5-3.0 MPa.

[0009] Preferably, the supercritical carbon dioxide extraction technology is: extraction time is 45 minutes, CO2 flow rate is 30 kg / h, extraction temperature is 60°C, and extraction pressure is 2.5 MPa.

[0010] Furthermore, when the supercritical carbon dioxide extraction technology is used for extraction, the loading volume is less than 70% of the volume of the extraction kettle, and glass beads are loaded.

[0011] Furthermore, the spicy hot pot base needs to be mixed evenly and then crushed before the extraction.

[0012] The present invention also provides spicy oil prepared according to the preparation method, wherein the content of capsaicin in the spicy oil is 80-110 mg / g, and the content of prickly ash amide is 60-90 mg / g.

[0013] The invention also provides application of the spicy oil in seasonings.

[0014] The invention also provides a seasoning comprising the spicy oil.

[0015] Compared with the prior art, the present invention has the following beneficial effects: The present invention adopts supercritical carbon dioxide extraction technology to extract the spicy oil in the hot pot base. Compared with the traditional stewing and leaching technology, the extraction time is significantly shortened, the utilization rate of oil is improved, and it is safe and non-toxic. The prepared spicy oil has a capsaicin content of 80-110 mg / g and a prickly ash amide content of 60-90 mg / g. The overall flavor effective ingredients are increased by 5.03 times, the flavor is richer, and the sensory quality is better. At the same time, due to the shortening of the extraction time, the characteristic flavor of the hot pot is well preserved. After the spicy oil is flavored and the flavor is further optimized, a seasoning oil that meets national safety standards can be obtained, which can be used for the industrial conversion of spicy oil. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 is the standard curve of capsaicin content; Figure 2 is the standard curve of hydroxy-α-sanshool content; Figure 3 The effect of extraction time on capsaicin content; Figure 4 The effect of CO2 flow rate on capsaicin content; Figure 5 The effect of extraction temperature on capsaicin content; Figure 6 The effect of extraction pressure on capsaicin content; Figure 7 The effect of extraction time on the content of prickly ash amide; Figure 8The effect of CO2 flow rate on the content of prickly ash amide; Fig. 9 is the effect of extraction temperature on the content of prickly ash amide; Fig.10 is the effect of extraction pressure on the content of prickly ash amide; Fig.11 The figure is a comparison chart of the sensory profiles of the two spicy oils of Example 1 and Comparative Example 1. DETAILED DESCRIPTION

[0017] In order to make the purpose, technical scheme and advantages of the present invention clearer, the present invention is further described in detail below in conjunction with specific embodiments.It should be understood that these descriptions are exemplary only, and are not intended to limit the scope of the present invention.In addition, in the following description, the description of known structures and technologies is omitted to avoid unnecessary confusion of the concept of the present invention.Unspecified conditions in the embodiments are carried out according to the conditions of normal conditions or manufacturer recommendations.Reagents used or instruments that do not specify manufacturers are conventional products that can be purchased and obtained commercially.

[0018] The first embodiment of the present invention provides a spicy oil, wherein the capsaicin content of the spicy oil is 80-110 mg / g and the pepperamide content of the spicy oil is 60-90 mg / g.

[0019] The second embodiment of the present invention provides a method for preparing spicy oil, comprising the following steps: extracting spicy oil from the fried spicy hot pot base using supercritical carbon dioxide extraction technology.

[0020] It should be noted that the spicy hot pot base of the present invention is a common spicy flavor composite seasoning in the market, including but not limited to the following raw materials: dried chili, prickly ash, star anise, cumin, tsaoko, bay leaf, kaempferia, cinnamon, nutmeg, cloves, onion, ginger, garlic, sugar, bean paste, animal fat, vegetable fat, etc., and also includes pretreatment steps such as selection, cleaning, and soaking before frying, and is fried by conventional methods. The raw materials of the hot pot base are adjusted according to different formulas, and no limitation is made here.

[0021] In some specific embodiments, the supercritical carbon dioxide extraction technology is: extraction time is 30-50min, CO2 flow rate is 20-40kg / h, extraction temperature is 60-70℃, extraction pressure is 1.5-3.0Mpa; the preferred embodiment is that the extraction time is 45min, CO2 flow rate is 30kg / h, extraction temperature is 60℃, and extraction pressure is 2.5Mpa. The applicant has optimized the supercritical carbon dioxide extraction process many times and obtained the preferred extraction process parameters. Under this condition, the content of capsaicin and prickly ash amide in the spicy oil extracted is high. This application shortens the long-term stewing and fermentation time in the prior art to within 1 hour, reduces the dissipation of flavor, retains more characteristic flavors, and makes the extracted spicy oil have a prominent flavor of special hot pot and better sensory quality.

[0022] In some specific embodiments, when the supercritical carbon dioxide extraction technology is used for extraction, the loading volume is less than 70% of the volume of the extraction kettle, and glass beads are loaded; the spicy hot pot base needs to be mixed evenly and then crushed before extraction. The extraction raw material of the present invention is a solid-liquid mixture and contains more oil. In the extraction kettle, the solid material is easy to accumulate in the lower layer and has a small contact area with the extraction medium. The movement of the glass beads during the extraction process helps mixing and stirring, further promotes the mass transfer process, and makes the extraction more uniform. The addition of glass beads provides a larger contact area between the extractant and the substance to be separated, thereby improving the extraction efficiency and effect, limiting the loading volume, and facilitating the mass transfer movement of the glass beads. After the material is crushed, it is beneficial for the carbon dioxide fluid to fully contact with the material during the extraction process, thereby improving the extraction efficiency of the solid material.

[0023] The present invention also provides spicy oil prepared according to the preparation method, and application of the spicy oil in seasonings. The spicy oil has a capsaicin content of 80-110 mg / g and a prickly ash amide content of 60-90 mg / g.

[0024] The present invention also provides a seasoning, comprising the spicy oil. The spicy oil of the present invention can be simply flavored and flavored to obtain seasoning oil, which meets the national safety standards after testing, and can also be processed with other spices and seasonings in appropriate amounts to obtain seasoning, which can be used for industrial conversion of spicy oil.

[0025] The following will disclose specific embodiments for implementing the present application, as well as corresponding comparative examples to demonstrate the relevant technical effects of the present application.

[0026] Example 1 Preparation of spicy oil Pretreatment: 1 kg of spicy hot pot base (Sichuan Xingxinsheng Biotechnology Co., Ltd.) was unpacked, mixed evenly, and crushed, loaded into the extraction kettle (the loading volume was less than 70% of the extraction kettle volume), and then loaded with 5 glass beads, using carbon dioxide as the supercritical fluid; Extraction process: first carry out the heating process: start the power supply, connect the cooling water, start the refrigerant switch, turn on the heating switches of the extraction kettle and the separation kettle, and set the temperature of the extraction kettle to 60°C; then carry out the pressure increase process: when the temperature of the refrigerator drops to 4°C and the temperature of the extraction kettle reaches the set temperature and stabilizes for 10 minutes, open the CO2 gas cylinder and the original air inlet valve, first discharge the air in the extraction and separation system, when the extraction pressure is consistent with the tank pressure, start the CO2 pump, gradually increase the pressure of the extraction kettle to 2.5Mpa, adjust the CO2 flow rate to 30kg / h, and set the extraction time to 45min; when the extraction time is reached, collect the spicy oil from the separation kettle.

[0027] The test revealed that the capsaicin content of the spicy oil in this embodiment was 106.24 mg / g, and the pepperamide content was 88.23 mg / g.

[0028] Example 2 Pretreatment: 1 kg of spicy hot pot base (Sichuan Xingxinsheng Biotechnology Co., Ltd.) was unpacked, mixed evenly, and crushed, loaded into the extraction kettle (the loading volume was less than 70% of the extraction kettle volume), and then loaded with 5 glass beads, using carbon dioxide as the supercritical fluid; Extraction process: first carry out the heating process: start the power supply, connect the cooling water, start the refrigerant switch, turn on the heating switches of the extraction kettle and the separation kettle, and set the temperature of the extraction kettle to 70°C; then carry out the pressure increase process: when the temperature of the refrigerator drops to 4°C and the temperature of the extraction kettle reaches the set temperature and stabilizes for 10 minutes, open the CO2 gas cylinder and the original air inlet valve, first discharge the air in the extraction and separation system, when the extraction pressure is consistent with the tank pressure, start the CO2 pump, gradually increase the pressure of the extraction kettle to 3.0Mpa, adjust the CO2 flow rate to 40kg / h, and set the extraction time to 30min; when the extraction time is reached, collect the spicy oil from the separation kettle.

[0029] The test revealed that the spicy oil of this embodiment contained 89.54 mg / g capsaicin and 75.36 mg / g prickly ash amide.

[0030] Example 3 Pretreatment: 1 kg of spicy hot pot base (Sichuan Xingxinsheng Biotechnology Co., Ltd.) was unpacked, mixed evenly, and crushed, loaded into the extraction kettle (the loading volume was less than 70% of the extraction kettle volume), and then loaded with 5 glass beads, using carbon dioxide as the supercritical fluid; Extraction process: first carry out the heating process: start the power supply, connect the cooling water, start the refrigerant switch, turn on the heating switches of the extraction kettle and the separation kettle, and set the temperature of the extraction kettle to 60°C; then carry out the pressure increase process: when the temperature of the refrigerator drops to 4°C and the temperature of the extraction kettle reaches the set temperature and stabilizes for 10 minutes, open the CO2 gas cylinder and the original air inlet valve, first discharge the air in the extraction and separation system, when the extraction pressure is consistent with the tank pressure, start the CO2 pump, gradually increase the pressure of the extraction kettle to 1.5Mpa, adjust the CO2 flow rate to 40kg / h, and set the extraction time to 50min; when the extraction time is reached, collect the spicy oil from the separation kettle.

[0031] The test revealed that the spicy oil of this embodiment contained 85.77 mg / g capsaicin and 68.33 mg / g prickly ash amide.

[0032] Example 4 Pretreatment: 1 kg of spicy hot pot base (Sichuan Xingxinsheng Biotechnology Co., Ltd.) was unpacked, mixed evenly, and crushed, loaded into the extraction kettle (the loading volume was less than 70% of the extraction kettle volume), and then loaded with 5 glass beads, using carbon dioxide as the supercritical fluid; Extraction process: first carry out the heating process: start the power supply, connect the cooling water, start the refrigerant switch, turn on the heating switches of the extraction kettle and the separation kettle, and set the temperature of the extraction kettle to 70°C; then carry out the pressure increase process: when the temperature of the refrigerator drops to 4°C and the temperature of the extraction kettle reaches the set temperature and stabilizes for 10 minutes, open the CO2 cylinder and the original air inlet valve, first discharge the air in the extraction and separation system, when the extraction pressure is consistent with the tank pressure, start the CO2 pump, gradually increase the pressure of the extraction kettle to 2.5Mpa, adjust the CO2 flow rate to 20kg / h, and set the extraction time to 50min; when the extraction time is reached, collect the spicy oil from the separation kettle.

[0033] The test revealed that the capsaicin content of the spicy oil in this embodiment was 84.67 mg / g, and the pepperamide content was 65.79 mg / g.

[0034] Example 5 Pretreatment: 1 kg of spicy hot pot base (Sichuan Xingxinsheng Biotechnology Co., Ltd.) was unpacked, mixed evenly, and crushed, loaded into the extraction kettle (the loading volume was less than 70% of the extraction kettle volume), and then loaded with 5 glass beads, using carbon dioxide as the supercritical fluid; Extraction process: first carry out the heating process: start the power supply, connect the cooling water, start the refrigerant switch, turn on the heating switches of the extraction kettle and the separation kettle, and set the temperature of the extraction kettle to 60°C; then carry out the pressure increase process: when the temperature of the refrigerator drops to 4°C and the temperature of the extraction kettle reaches the set temperature and stabilizes for 10 minutes, open the CO2 cylinder and the original air inlet valve, first discharge the air in the extraction and separation system, when the extraction pressure is consistent with the tank pressure, start the CO2 pump, gradually increase the pressure of the extraction kettle to 2.5Mpa, adjust the CO2 flow rate to 20kg / h, and set the extraction time to 40min; when the extraction time is reached, collect the spicy oil from the separation kettle.

[0035] The test revealed that the capsaicin content of the spicy oil in this embodiment was 86.68 mg / g, and the pepperamide content was 63.15 mg / g.

[0036] Example 6 Preparation of Flavoring Oil The spicy oil obtained in Example 1 is further flavored to obtain seasoning oil.

[0037] Comparative Example 1 The same hot pot base as in Example 1 was used as the raw material, and a common extraction method was adopted. After stewing and fermenting for 72 hours, the mixture was filtered through a 100-mesh sieve, and then allowed to stand for 2 hours to obtain the upper clarified liquid, thereby extracting the spicy oil.

[0038] Test Example 1 Extraction process optimization test The present invention adopts orthogonal experimental design to optimize the CO2 fluid supercritical extraction process of spicy oil, and the prepared spicy oil is analyzed for capsaicin and prickly ash amide content by HPLC high performance liquid chromatography: (1) Determination of capsaicin 1) Preparation of capsaicin standard solution Weigh 1g of capsaicin standard (purity ≥99%, Shanghai Yuanye Biotechnology Co., Ltd.), dissolve it in methanol to a 100mL volumetric flask to obtain a 10mg / mL capsaicin mother solution. Prepare capsaicin standard solutions with concentrations of 0mg / mL, 0.2mg / mL, 0.4mg / mL, 0.8mg / mL, 1.2mg / mL, 1.6mg / mL, and 2.0mg / mL from the mother solution, filter through a 0.45µm filter membrane, and perform chromatographic analysis. Obtain the linear regression equation by calculation.

[0039] 2) HPLC conditions: Refer to GB / T 2126-2007 "Determination of capsaicinoids and expression of pungency in peppers and pepper products" for chromatographic analysis and calculation of content and pungency; Chromatographic column: Zorbax SB-C18 4.6mm×250mm 5µm; mobile phase: methanol+water (65+35); injection volume: 10µL; flow rate: 1mL / min; UV detection wavelength: 280mm; column oven temperature: 30℃.

[0040] 3) Calculation of total amount of capsaicinoids

[0041] Where: Wa is the capsaicin content in the sample, in grams per kilogram (g / kg); C1 is the capsaicin content found on the standard curve, in milligrams per milliliter (µg / mL); V is the sample volume, in milliliters (mL); m is the sample mass, in grams (g). The calculation result is expressed to three decimal places.

[0042] Where: Wb is the content of dihydrocapsaicin in the sample, in grams per kilogram (g / kg); C2 is the content of dihydrocapsaicin found on the standard curve, in milligrams per milliliter (µg / mL); V is the volume of the sample, in milliliters (mL); m is the mass of the sample, in grams (g). The calculation result is expressed to three decimal places.

[0043] Where: W is the total amount of capsaicinoids in the sample, in grams per kilogram (g / kg); 0.9 is the coefficient for converting capsaicin and dihydrocapsaicin to the total amount of capsaicinoids.

[0044] 4) Development of capsaicin standard curve The above method can be used to obtain a standard curve for determining the content of capsaicin by high performance liquid chromatography, such as Figure 1 As shown, its linear regression equation is y=1145416.637x+89.608, R2=0.996.

[0045] (2) Determination of prickly ash amide 1) Preparation of standard solution of thunbergamide The main components of pepper amides are hydroxy-α-sanshool, hydroxy-β-sanshool, hydroxy-γ-sanshool and hydroxy-ε-sanshool. In this experiment, hydroxy-α-sanshool was used as an indicator to determine the total amount of pepper amides.

[0046] Weigh 1g of hydroxy-α-sanshool standard (Tianjin Zhiyuan Chemical Reagent Co., Ltd.), dissolve it in methanol and dilute it to 100mL volumetric flask to obtain 10mg / mL hydroxy-α-sanshool mother solution. Prepare hydroxy-α-sanshool standard solutions with concentrations of 0mg / mL, 0.2mg / mL, 0.4mg / mL, 0.8mg / mL, 1.2mg / mL, 1.6mg / mL, and 2.0mg / mL from the mother solution respectively. Obtain the linear regression equation by calculation.

[0047] 2) HPLC conditions: Refer to GB / T 1291-2020 "High Performance Liquid Chromatography for the Determination of the Total Content of Zanthoxylum bungeanum and Zanthoxylum bungeanum Processed Products" for chromatographic analysis and calculation of each content; Chromatographic column: C18 reverse phase column, 4.6mm×150mm, 5µm; mobile phase: acetonitrile: 1% glacial acetic acid aqueous solution (40:60); injection volume: 20µL; flow rate: 1.5mL / min; UV detection wavelength: 270mm; column oven temperature: 40℃.

[0048] 3) Calculation of the total amount of pepper amides

[0049] Where: X is the total content of sanshool in the sample, in milligrams per gram (mg / g); C is the content of hydroxy-α-sanshool found on the standard curve, in milligrams per milliliter (µg / mL); V is the volume of the sample, in milliliters (mL); K is the sample dilution multiple; m is the sample mass, in grams (g). The calculation result is expressed to three decimal places.

[0050] 4) Drawing of the standard curve of hydroxy-α-sanshool The above method can be used to obtain a standard curve for determining the content of hydroxy-α-sanshool by high performance liquid chromatography, such as Figure 2 As shown, the linear regression equation of prickly ash amide is y=782928.37719x+6482.75439, R2=0.998.

[0051] (3) Single-factor experimental design 1) A single factor experiment was used to screen and analyze the supercritical extraction process conditions that affect capsaicin in spicy oil. According to reference materials, the extraction time for hot pot base was selected as 0min, 20min, 25min, 30min, 35min, 40min, 45min, and 50min, the extraction temperature was 40℃, 50℃, 60℃, 70℃, and 80℃, the CO2 flow rate was 10kg / h, 15kg / h, 20kg / h, 25kg / h, 30kg / h, 35kg / h, and 40kg / h, and the pressure was 1.5Mpa, 2.0Mpa, 2.5Mpa, 3.0Mpa, and 3.5Mpa. Single factor experiments were carried out with capsaicin content and prickly ash amide content as indicators.

[0052] Effects of extraction time, CO2 flow rate, extraction temperature, and extraction pressure on the capsaicin content of spicy oil, see Figure 3-Figure 6 ;Depend on Figure 3 It can be seen that the supercritical CO2 extraction of spicy oil increases with the increase of extraction time, allowing CO2 to fully contact and extract the material, increasing the extraction ratio. However, when the extraction time is too long, supercritical CO2 will increase its extraction resistance and reduce the extraction of effective ingredients. The optimal extraction time is 40 minutes. Figure 4 It can be seen that increasing the CO2 flow rate will increase the extraction rate and increase the contact area between the hot pot base and the supercritical CO2. However, if the supercritical CO2 is increased excessively, the contact area between the hot pot base and the hot pot base will reach the maximum and will no longer increase. In fact, the extraction rate will be reduced due to the excessive flow rate and insufficient extraction time. The optimal supercritical CO2 flow rate for extraction is 30kg / h. Figure 5 It can be seen that increasing the extraction temperature will increase the dissolution rate of phenolic substances in CO2, but excessive heating will make the sample discharge temperature higher, and its effective extraction components will volatilize, thereby reducing the extraction rate. The optimal extraction temperature is 60℃. Figure 6 It can be seen that with the increase of pressure, the fluid effect of supercritical CO2 will be better, thereby increasing the extraction amount, but excessive pressure increase will affect the supercritical state of CO2, thereby affecting the extraction efficiency. The optimal extraction pressure is 3Mpa.

[0053] 2) A single factor experiment was used to screen and analyze the supercritical extraction process conditions that affect the spicy oil prickly ash amide. According to reference materials, the extraction time for hot pot base was selected as 0min, 20min, 25min, 30min, 35min, 40min, 45min, 50min, the extraction temperature was 40℃, 45℃, 50℃, 55℃, 60℃, 65℃, 70℃, the CO2 flow rate was 10kg / h, 15kg / h, 20kg / h, 25kg / h, 30kg / h, 35kg / h, 40kg / h, and the pressure was 1.5Mpa, 2.0Mpa, 2.5Mpa, 3.0Mpa, and 3.5Mpa. Single factor experiments were carried out with prickly ash amide content as an indicator.

[0054] Effects of extraction time, CO2 flow rate, extraction temperature and extraction pressure on the content of prickly ash oil are shown in Figure 7-Figure 10 ;Depend on Figure 7 It can be seen that as the extraction time increases, CO2 fully contacts and extracts the material, increasing the extraction ratio. However, when the extraction time is too long, supercritical CO2 will increase its extraction resistance and reduce the extraction of effective ingredients. When the extraction time is 40 minutes, the content of prickly ash amide is the largest. Figure 8 It can be seen that increasing the CO2 flow rate will increase the extraction rate and increase the contact area between the hot pot base and the supercritical CO2. However, if the supercritical CO2 is increased excessively, the contact area between the hot pot base and the hot pot base will reach the maximum and will no longer increase. In fact, the extraction rate will be reduced due to the excessive flow rate and insufficient extraction time. The optimal supercritical CO2 flow rate for extraction is 35kg / h. Fig. 9 It can be seen that increasing the temperature during extraction will increase the dissolution rate of phenolic substances in CO2, but excessive heating will make the sample discharge temperature higher, and its effective extraction components will volatilize, thereby reducing the extraction rate. The optimal extraction temperature is 65℃. Fig.10 It can be seen that with the increase of pressure, the fluid effect of supercritical CO2 will be better, thereby increasing the extraction amount, but excessive pressure increase will affect the supercritical state of CO2, thereby affecting the extraction efficiency. It can be seen from the figure that the optimal extraction pressure is 2.5Mpa.

[0055] (4) Orthogonal experimental design Based on the single factor experiment, an orthogonal experiment was conducted to determine the optimal extraction process conditions for capsaicin and prickly ash amide in spicy oil, and an orthogonal table with 4 factors and 3 levels was designed, as shown in Table 1 below: Table 1 Experimental table of orthogonal factors for supercritical CO2 extraction .

[0056] 1) Results of orthogonal experiments on supercritical CO2 extraction of capsaicin The results of the orthogonal experiment of supercritical CO2 extraction of capsaicin are shown in Table 2 below: .

[0057] According to the analysis in Table 2, the order of influencing factors of supercritical CO2 extraction of spicy oil is: A>B>C>D, that is, the order of influence of the four factors on the extraction is: extraction time>CO2 flow>extraction temperature>extraction pressure. The optimal process parameters of supercritical CO2 extraction of spicy oil are A3B2C2D2, that is, the extraction time is 50min, the CO2 flow is 30kg / h, the extraction temperature is 60℃, and the extraction pressure is 2.5Mpa. Under this condition, the capsaicin content of spicy oil is 107.31±2.24mg / g.

[0058] 2) Results of orthogonal experiments on supercritical CO2 extraction of prickly ash amide The results of the orthogonal experiment of supercritical CO2 extraction of prickly ash amide are shown in Table 3 below: Table 3 Results of orthogonal experiment of supercritical CO2 extraction of prickly ash amide .

[0059] According to the analysis in Table 3, the order of influencing factors of supercritical CO2 extraction of spicy oil is: C>A>B>D, that is, the order of influence of the four factors on the extraction is: extraction temperature>extraction time>CO2 flow>extraction pressure. The optimal process parameters of supercritical CO2 extraction of spicy oil are A2B2C2D2, that is, the extraction time is 40min, the CO2 flow is 30kg / h, the extraction temperature is 60℃, and the extraction pressure is 2.5Mpa. Under this condition, the content of prickly ash amide in spicy oil is 87.65±1.04mg / g.

[0060] Combining the results of single factor experiment and orthogonal experiment on the extraction of capsaicin and thiamethoxam in spicy oil by supercritical CO2, and analyzing their contents, the optimal conditions for the extraction of spicy oil by supercritical CO2 extraction technology were obtained: extraction time of 45min, CO2 flow rate of 30kg / h, extraction temperature of 60℃, and extraction pressure of 2.5Mpa. Under these conditions, the hot pot oil was extracted, and the content of capsaicin in the spicy oil was 105.28±2.06mg / g, and the content of thiamethoxam was 87.59±1.54mg / g.

[0061] Test Example 2 Determination of spicy oil yield The spicy oil obtained in Example 1 and Comparative Example 1 was subjected to sample yield determination, and the yield calculation formula was: yield (%) = (finished product mass / raw material mass) × 100%. The test results are recorded in Table 4: Table 4 Sample extraction yield .

[0062] It can be seen from Table 4 that after frying, the oil-to-material ratio in the hot pot base is 7:3. According to the yield, it can be calculated that the oil utilization rate in Example 1 (supercritical CO2 extraction) is 90.29%, and the oil utilization rate in Comparative Example 1 (ordinary leaching method) is 80.39%; compared with the traditional stewing and filtering extraction method, the yield of supercritical CO2 extraction technology is increased by nearly 7%, and the oil utilization rate is increased by nearly 10%, indicating that supercritical CO2 extraction technology has achieved a deeper and more effective extraction under the traditional extraction method.

[0063] Test Example 3 Determination of active ingredients The spicy oil obtained in Example 1 and Comparative Example 1 was tested for effective components of the samples, and the main components of the supercritical CO2 extraction method and the main components of the common leaching extraction method were compared and analyzed using a gas chromatography-mass spectrometry analyzer (GC-MS); Gas chromatography conditions: chromatographic column: Rtx-5, helium flow rate: 1.0 mL / min, injection volume: 1 μL; injection port temperature: 230 °C; program temperature: starting temperature: 60 °C, increase to 160 °C at 5 °C / min, then increase to 230 °C at 10 °C / min, and maintain for 9 min; Mass spectrometry conditions: interface temperature 250°C, EI ion source, electron energy 70 eV, ion source temperature 250°C; scanning range: 40-350 m / e; solvent delay time 4.5 min; The test results are recorded in Table 5: Table 5 Active ingredients of samples .

[0064] The results of Table 5 above can be obtained by converting the results of gas chromatography-mass spectrometry analysis, among which the effective ingredient contents of capsanthin, capsaicin, prickly ash amide and fermented black bean oil in Example 1 (supercritical CO2 extraction method) are 6.55, 5.65, 4.14 and 2.97 times that of Comparative Example 1 (conventional extraction method), respectively, and the overall flavor effective ingredients are 5.03 times, with good component state performance, indicating that supercritical CO2 extraction technology has greatly improved the flavor extraction of spicy oil compared with traditional methods.

[0065] Experimental Example 4 Sensory Evaluation Invite 30 food professionals to conduct sensory evaluation on the extracted spicy oil. The evaluation items include four items with a total score of 100 points. The sensory evaluation table is as follows Table 6: Table 6 Sensory evaluation table of spicy oil .

[0066] The spicy oil obtained in Example 1 and Comparative Example 1 was subjected to sensory evaluation, and the results are as follows: Fig.11 As shown by Fig.11It can be seen that the overall flavor evaluation of the spicy oil extracted by supercritical CO2 (Example 1) is higher, and it is more accepted by the public than the ordinary extraction (Comparative Example 1) in terms of aroma, state, color, taste and characteristics.

[0067] Experimental Example 5: Physical and Chemical Index Test of Seasoning Oil The seasoning oil obtained in Example 6 was tested for physical and chemical indicators. The test methods and results are shown in Table 7 below: Table 7 Physical and chemical index detection of seasoning oil .

[0068] As shown in Table 7, all indicators of the samples meet the national food standards, indicating that the spicy oil extracted by supercritical CO2 extraction technology can meet the national food safety standards after blending.

[0069] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any form. Any simple modification or equivalent change made to the above embodiment based on the technical essence of the present invention shall fall within the protection scope of the present invention.

Claims

1. A spicy oil, characterized in that: The spicy oil has a capsaicin content of 80-110 mg / g and a pepperamide content of 60-90 mg / g.

2. A method for preparing spicy oil, characterized in that: The method comprises the following steps: using supercritical carbon dioxide extraction technology to extract spicy oil from the fried spicy hot pot base.

3. The method for preparing spicy oil according to claim 2, characterized in that: The supercritical carbon dioxide extraction technology is as follows: extraction time is 30-50 minutes, CO2 flow rate is 20-40 kg / h, extraction temperature is 60-70° C., and extraction pressure is 1.5-3.0 MPa.

4. The method for preparing spicy oil according to claim 2, characterized in that: The supercritical carbon dioxide extraction technology is as follows: extraction time is 45 minutes, CO2 flow rate is 30 kg / h, extraction temperature is 60° C., and extraction pressure is 2.5 MPa.

5. The method for preparing spicy oil according to claim 2, characterized in that: When the supercritical carbon dioxide extraction technology is used for extraction, the loading volume is less than 70% of the volume of the extraction kettle, and glass beads are loaded.

6. The method for preparing spicy oil according to claim 2, characterized in that: Before the extraction, the spicy hot pot base needs to be mixed evenly and then crushed.

7. A spicy oil prepared according to any one of the preparation methods of claims 2-6, wherein the spicy oil has a capsaicin content of 80-110 mg / g and a pepperamide content of 60-90 mg / g.

8. Use of the spicy oil according to any one of claims 1 or 7 in seasonings.

9. A seasoning, characterized in that Contains the spicy oil described in any one of claims 1 or 7.

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