An antioxidant spice composition, a method of making the same, and use in red oil products

Abstract

The application discloses an antioxidative spicy composition and a preparation method and application thereof in red oil products, and relates to the field of food processing. The preparation method comprises the following steps: putting oil-soluble raw materials into compound edible vegetable oil, extracting under a medium-temperature condition, filtering, and taking the obtained oil; putting water-soluble raw materials into an ethanol aqueous solution, refluxing and extracting, and obtaining extractum after post-treatment; heating the oil and the extractum, high-speed shearing and dispersing, and uniformly refining after cooling, so as to obtain the antioxidative spicy composition; and the antioxidative spicy composition is added into the red oil when the temperature of the red oil is cooled to 60-80 DEG C after being prepared, and the adding amount is 0.5-3% of the total mass of the red oil. The total phenol content of the obtained composition reaches 68.4 mg GAE / g, the particle size D90 of the dispersed phase in the composition is less than 2 microns, the composition is not stratified and precipitated after being stored at room temperature for 6 months in the red oil, the peroxide value reaches 0.25 g / 100 g, and the induction period is more than 24 days.

Description

Technical Field

[0001] This invention relates to the field of food processing technology, specifically to an antioxidant spice composition and its preparation method, and its application in chili oil products. Background Technology

[0002] Chili oil is an indispensable condiment in Chinese cuisine, especially Sichuan cuisine, known for its bright red color and rich, spicy aroma. However, chili oil contains a large amount of unsaturated fatty acids, which are highly susceptible to oxidation and rancidity during storage and sales due to exposure to light, temperature, and oxygen in the air. This results in an unpleasant rancid taste, which not only degrades the flavor of the chili oil but also reduces its nutritional value and may even produce harmful substances, severely shortening the product's shelf life.

[0003] To slow down oil oxidation, synthetic antioxidants, such as TBHQ (tert-butylhydroquinone) and BHT (butylated hydroxytoluene), are often added industrially. However, with increasing consumer concern for food safety and health, the safety of synthetic antioxidants has become highly controversial, and their use is strictly limited. Therefore, developing efficient and natural antioxidants has become a hot research topic in the industry.

[0004] Spices are rich in natural antioxidants such as phenols and flavonoids. Existing technologies have reported the direct addition of spices to chili oil to enhance flavor and antioxidant properties. For example, a mixture of spices such as fennel, pepper, and white cardamom, along with water-soluble phospholipids and sodium D-isoascorbate, is added to cooled chili oil. However, this method still relies on some synthetic or chemically modified additives, and the effective antioxidant components in spices are easily destroyed during high-temperature extraction, resulting in incomplete release and insufficient antioxidant efficacy. Furthermore, some studies have used spice essential oils in blends, which show significant antioxidant effects, but the extraction cost of essential oils is high, and the strong aroma can easily mask or alter the original flavor of the chili oil, limiting its application. Summary of the Invention

[0005] The purpose of this invention is to provide an antioxidant spice composition and its preparation method, as well as its application in chili oil products. Through specific spice screening, compounding, and gradient extraction processes, the synergistic release of oil-soluble and water-soluble antioxidant components in the spices is achieved, significantly improving the antioxidant stability of chili oil products without relying on artificially synthesized antioxidants.

[0006] To solve the above-mentioned technical problems, the present invention adopts the following technical solution:

[0007] A method for preparing an antioxidant spice composition includes the following steps:

[0008] S100. Add oil-soluble raw materials to compound edible vegetable oil, extract under medium temperature conditions, filter and take the obtained oil.

[0009] S200. The water-soluble raw material is added to an ethanol-water solution, refluxed for extraction, and then post-processed to obtain a paste-like extract.

[0010] S300. After heating the above-mentioned oil and extract, the mixture is dispersed by high-speed shearing, cooled, and then uniformly refined to obtain the target composition.

[0011] The mass ratio of the oil to the extract is 10:0.5~2; the compounded edible vegetable oil is made by compounding high oleic acid vegetable oil and medium chain triglycerides (MCT oil) in a mass ratio of 1.5~4:1.

[0012] This invention addresses the core issue of how to achieve synergistic effects of antioxidants with different properties, and constructs a systematic solution from the extraction source to the final form.

[0013] At the extraction source, this invention first breaks through the limitations of single-vegetable oil extraction. Conventional extraction media have fixed polarity and limited solubility range, while the core of step S100 lies in the formulation of a compound edible vegetable oil—combining high-oleic acid vegetable oil with medium-chain triglycerides in a specific ratio to construct an extraction environment with a continuous polarity gradient. When oil-soluble spices are added, active ingredients of different polarities spontaneously partition according to the principle of "like dissolves like." Fat-soluble terpenes and cinnamaldehyde tend to dissolve in the high-oleic acid oil phase, while medium-polarity phenolic acids are effectively extracted by medium-chain triglycerides. Thus, a single extraction can obtain a richer spectrum of antioxidant substances than a single oil, laying the material foundation for the subsequent synergistic effect.

[0014] In terms of component completion, the S200 step achieves precise targeted enrichment through alcohol-water extraction. Spices contain highly polar antioxidants such as tea polyphenols and rosmarinic acid, which have extremely low solubility in pure oil. The S200 step uses an ethanol-water system to directionally extract these highly polar substances and enrich them in the form of an extract. Combined with the S100 step, it enriches both fat-soluble and water-soluble components separately, ensuring the integrity of the antioxidant spectrum in the final composition and effectively avoiding the loss of active ingredients that inevitably occurs with single extraction methods. Total phenol content is an important indicator for evaluating the activity of natural antioxidants. This invention, through the combination of plant oils and a zoned extraction process, achieves a total phenol content of 68.4 mg GAE / g in the composition, a 31.3% increase compared to single oil extraction, laying a material foundation for excellent antioxidant performance.

[0015] This invention not only focuses on increasing the total phenol content, but also endows the composition with a unique microstructure (particle size D90≤2μm) through the S300 process, enabling phenolic substances to be stably dispersed in the oil phase and enriched in the key interface regions of the oxidation reaction. The synergistic effect of total phenol content and particle size control jointly achieves excellent antioxidant effects with an induction period of over 24 days. The S300 step of this invention adopts a purely physical process of thermal induction-shear dispersion-flash cooling, achieving stable dispersion without the addition of any emulsifiers. First, the oil phase is heated to a higher temperature, while the aqueous phase extract is preheated and softened; then, the aqueous phase is injected into the oil phase in a high-speed shear field. The high-temperature environment reduces the viscosity of the system, causing the aqueous phase to be instantly broken into micron-sized or even submicron-sized droplets under shear force; subsequently, flash cooling freezes the broken droplets, thus stably suspending them in the oil phase as solid particles, forming a kinetically stable physical suspension system.

[0016] In this invention, steps S100 and S200 together determine the material composition and component spectrum of the composition, providing the material prerequisite for its antioxidant efficacy. Step S300 endows the composition with a unique microstructure, not only solving the application problem of water-oil incompatibility but also giving rise to sustained-release function and interfacial antioxidant properties. If the products obtained in the first two steps are simply mixed, they may be unusable due to phase separation or have a short-lived antioxidant effect due to rapid consumption of active ingredients. This invention utilizes this progressive design from component spectrum construction to spatial structure shaping, enabling the final composition to achieve synergistic effects and obtain long-lasting and stable natural antioxidant properties.

[0017] Furthermore, by weight,

[0018] The oil-soluble ingredients include: 15-25 parts star anise, 10-20 parts cinnamon, 8-15 parts cardamom, 10-18 parts amomum villosum, 20-30 parts fennel seeds, and 5-10 parts bay leaves;

[0019] Water-soluble ingredients include: 8-12 parts cloves, 15-25 parts licorice, 10-20 parts rosemary, 10-15 parts perilla, and 5-10 parts green tea.

[0020] The raw material formulation of this invention is not a random combination, but a scientific formulation based on the types and contents of antioxidant active ingredients in each spice. Star anise, cinnamon, and fennel are rich in volatile terpenes and phenols, providing the main body of fat-soluble antioxidants; cardamom, amomum, and bay leaves contribute moderately polar phenolic acid components; while eugenol, rosmarinic acid, and tea polyphenols in cloves, rosemary, and green tea are representative of strong polar antioxidants; licorice and perilla have both sweetening and auxiliary antioxidant functions. This formulation achieves a balance between fat-soluble and water-soluble antioxidants in the final composition, ensuring both the free radical scavenging capacity within the oil phase and strengthening the antioxidant barrier in the interfacial region, laying the material foundation for the subsequent synergistic effect.

[0021] Furthermore, this invention constructs an extraction medium with a polarity gradient by combining high-oleic acid vegetable oil and medium-chain triglycerides in step S100. This medium can not only efficiently extract antioxidants of different polarities, but also simultaneously enrich various volatile flavor precursors in spices. Non-polar terpenes are mainly enriched in the high-oleic oil phase, while medium-polar aldehydes and ketones are effectively captured by medium-chain triglycerides. The clove, licorice, and other components extracted by alcohol-water in step S200 not only contribute polar antioxidants such as rosmarinic acid and tea polyphenols, but also contain substances such as eugenol and glycyrrhizin, which bring a unique aftertaste and fragrance to the chili oil. The S300 process stably disperses the above two types of components in the oil phase in the form of submicron particles, so that the flavor substances can be continuously and evenly released during the storage and use of chili oil, avoiding the uneven flavor release caused by the addition of traditional spice powders or the aroma loss caused by direct high-temperature extraction.

[0022] Further, in step S100, the oil-soluble raw material is washed, dried, crushed to 20-40 mesh, added to edible vegetable oil, and extracted at a constant temperature of 60-80℃ for 2-4 hours. After filtration, the obtained oil is taken. The mass ratio of the oil-soluble raw material to the edible vegetable oil is 1:2-4.

[0023] Furthermore, the high-oleic acid vegetable oil is selected from one or two of high-oleic acid sunflower seed oil and olive oil.

[0024] Both high-oleic sunflower seed oil and olive oil are rich in oleic acid (monounsaturated fatty acid content >75%), exhibiting excellent oxidative stability. When combined with medium-chain triglycerides, their non-polar characteristics are further emphasized, which is beneficial for the accumulation of fat-soluble terpenes. Furthermore, both oils have a mild flavor that does not mask the flavor of spices, making them suitable for red oil products.

[0025] Further, in step S200, the water-soluble raw material is washed, dried, crushed to 20-40 mesh, added to an ethanol aqueous solution, and extracted by reflux at 50-70°C for 1-3 hours. After filtration, the filtrate is concentrated under reduced pressure to recover the ethanol and obtain a paste-like extract.

[0026] Furthermore, the mass ratio of the ethanol aqueous solution to the water-soluble raw material is 6~10:1; the volume fraction of ethanol in the ethanol aqueous solution is 40~75%.

[0027] The 40-75% ethanol-water system has the best extraction selectivity for polyphenols and flavonoids in spices, and can make the antioxidant activity (DPPH scavenging rate) of component B reach its peak.

[0028] Further, in step S300, the extract is softened at 40-50°C; the oil is heated to 70-80°C, the extract is added to the oil, sheared at 3000-4000 rpm for 20-30 minutes, rapidly cooled to below 25°C at a rate of about 10-15°C / min, and homogenized under high pressure to obtain the target composition.

[0029] A cooling rate of 10~15℃ / min is just right to maintain the uniformity of the system while ensuring the particle size (D90<2μm), allowing the composition to maintain physical stability for more than 6 months under emulsifier-free conditions. If the cooling is too slow, the broken droplets have enough time to collide and merge, leading to increased particle size or even stratification; if the cooling is too fast, thermal stress may cause instability in the system.

[0030] Furthermore, high-pressure homogenization includes the following: pressure of 25~35MPa, and number of cycles of 1~3.

[0031] After the high-pressure homogenization step, the particle size D90 of the dispersed phase in the composition can be stably controlled below 2 μm. The kinetic stability is achieved by Brownian motion, and the narrow particle size distribution ensures batch-to-batch reproducibility.

[0032] An antioxidant spice composition prepared by the preparation method described above, wherein the dispersed phase particle size D90 ≤ 2 μm is provided in the composition.

[0033] The antioxidant spice composition is used in the preparation of red oil products. The antioxidant spice composition is added after the red oil is cooked and cooled to 60-80°C. The amount added is 0.5-3% of the total mass of the red oil.

[0034] Compared with the prior art, the beneficial effects of the present invention are:

[0035] In this invention, steps S100 and S200 work synergistically to ensure a more complete spectrum of antioxidants in the final composition, increasing the total phenol content by 25-35% compared to extraction from a single oil. Step S300 involves the complete absence of any emulsifiers, resulting in a dispersed phase particle size D90 < 2 μm in the obtained composition, which shows no stratification or precipitation after storage at room temperature for more than 6 months. Furthermore, the composition prepared using this method exhibits an induction period exceeding 24 days to achieve a peroxide value of 0.25 g / 100 g, significantly superior to single components or simple mixtures. Simultaneously, the entire preparation process of this invention does not use antioxidants, emulsifiers, or stabilizers, and the composition is 100% derived from natural spices and edible vegetable oils. Detailed Implementation

[0036] The present invention will now be further described.

[0037] Example 1

[0038] The oil-soluble ingredients include: 20g star anise, 15g cinnamon, 10g cardamom, 12g amomum villosum, 25g fennel seeds, and 8g bay leaves.

[0039] The water-soluble ingredients include: 10g cloves, 20g licorice, 15g rosemary, 12g perilla, and 8g green tea.

[0040] A method for preparing an antioxidant spice composition includes the following steps:

[0041] S100. After washing and drying the oil-soluble raw material, crush it to 30 mesh, put it into edible vegetable oil, and extract it at a constant temperature of 70°C for 3 hours. After filtration, take the obtained oil. The mass ratio of the oil-soluble raw material to the edible vegetable oil is 1:3.

[0042] The compounded edible vegetable oil is made by blending high-oleic sunflower seed oil and medium-chain triglycerides in a mass ratio of 2.3:1.

[0043] S200. After washing and drying the water-soluble raw material, crush it to 30 mesh, add it to an ethanol-water solution, and reflux extract it at 60°C for 2 hours. Filter the solution, concentrate the filtrate under reduced pressure to recover the ethanol, and obtain a paste-like extract. The mass ratio of the ethanol-water solution to the water-soluble raw material is 8:1; the volume fraction of ethanol in the ethanol-water solution is 55%.

[0044] S300: Soften the paste-like extract at 45°C; heat the oil to 75°C, add the paste-like extract to the oil, shear at 3500 rpm for 25 minutes, rapidly cool to 20°C at a rate of approximately 12°C / min, homogenize under high pressure at 30 MPa, and cycle twice to obtain an antioxidant spice composition.

[0045] The mass ratio of the oil to the extract is 10:1.2.

[0046] Example 2

[0047] The oil-soluble ingredients include: 15g star anise, 10g cinnamon, 8g cardamom, 10g amomum villosum, 20g fennel seeds, and 5g bay leaves;

[0048] The water-soluble ingredients include: 8g cloves, 15g licorice, 10g rosemary, 10g perilla, and 5g green tea.

[0049] A method for preparing an antioxidant spice composition includes the following steps:

[0050] S100. After washing and drying the oil-soluble raw material, crush it to 20 mesh, put it into edible vegetable oil, and extract it at a constant temperature of 60°C for 2 hours. After filtration, take the obtained oil. The mass ratio of the oil-soluble raw material to the edible vegetable oil is 1:2.

[0051] The compounded edible vegetable oil is made by blending high-oleic sunflower seed oil and medium-chain triglycerides in a mass ratio of 1.5:1.

[0052] S200. After washing and drying the water-soluble raw material, crush it to 25 mesh, add it to an ethanol-water solution, and reflux extract it at 50°C for 1 hour. Filter the solution, concentrate the filtrate under reduced pressure to recover the ethanol, and obtain a paste-like extract. The mass ratio of the ethanol-water solution to the water-soluble raw material is 6:1; the volume fraction of ethanol in the ethanol-water solution is 40%.

[0053] S300: Soften the paste-like extract at 40°C; heat the oil to 70°C, add the paste-like extract to the oil, shear at 3000 rpm for 20 minutes, rapidly cool to 22°C at a rate of about 10°C / min, homogenize under high pressure at 25 MPa, and cycle once to obtain an antioxidant spice composition.

[0054] The mass ratio of the oil to the extract is 10:0.5.

[0055] Example 3

[0056] The oil-soluble ingredients include: 25g star anise, 20g cinnamon, 15g cardamom, 18g amomum villosum, 30g fennel seeds, and 10g bay leaves;

[0057] The water-soluble ingredients include: 12g cloves, 25g licorice, 20g rosemary, 15g perilla, and 10g green tea.

[0058] A method for preparing an antioxidant spice composition includes the following steps:

[0059] S100. After washing and drying the oil-soluble raw material, crush it to 40 mesh, put it into edible vegetable oil, and extract it at a constant temperature of 80°C for 4 hours. After filtration, take the obtained oil. The mass ratio of the oil-soluble raw material to the edible vegetable oil is 1:4.

[0060] The compounded edible vegetable oil is made by blending high-oleic sunflower seed oil and medium-chain triglycerides in a mass ratio of 4:1.

[0061] S200. After washing and drying the water-soluble raw material, crush it to 40 mesh, add it to an ethanol-water solution, and reflux extract it at 70°C for 3 hours. Filter the solution, concentrate the filtrate under reduced pressure to recover the ethanol, and obtain a paste-like extract. The mass ratio of the ethanol-water solution to the water-soluble raw material is 10:1; the volume fraction of ethanol in the ethanol-water solution is 75%.

[0062] S300: Soften the paste-like extract at 50°C; heat the oil to 80°C, add the paste-like extract to the oil, shear at 4000 rpm for 30 minutes, rapidly cool to 18°C ​​at a rate of about 15°C / min, homogenize under high pressure at 35 MPa, and cycle 3 times to obtain an antioxidant spice composition.

[0063] The mass ratio of the oil to the extract is 10:2.

[0064] Example 4

[0065] The compounded edible vegetable oil is composed of olive oil and medium-chain triglycerides in a mass ratio of 2.3:1. The remaining parameters and steps are the same as in Example 1.

[0066] Example 5

[0067] The compounded edible vegetable oil is composed of high-oleic sunflower seed oil, olive oil, and medium-chain triglycerides in a mass ratio of 1:1.3:1. The remaining parameters and steps are the same as in Example 1.

[0068] Comparative Example 1

[0069] In S100, a single high-oleic sunflower seed oil is used instead of the compound vegetable oil, and the other parameters and steps are the same as in Example 1.

[0070] Comparative Example 2

[0071] The oil-soluble raw material and the water-soluble raw material were combined (total weight same as in Example 1), washed, dried and crushed to 40 mesh, and added to 8 times the mass of 60% ethanol aqueous solution. The mixture was refluxed at 60°C for 2 hours, filtered, and the filtrate was concentrated under reduced pressure to recover the ethanol, thus obtaining a mixed extract.

[0072] Comparative Example 3

[0073] In S300, rapid cooling is eliminated, and cooling is performed at 1°C / min to 20°C. The remaining parameters are the same as in Example 1.

[0074] Comparative Example 4

[0075] After shear dispersion is completed in S300, high-pressure homogenization is not performed, and the remaining parameters are the same as in Example 1.

[0076] Comparative Example 5

[0077] Instead of using a thermally induced shear dispersion process, S300 adds 1% polyglycerol ricinoleate by mass of the total system and mixes it simply by stirring.

[0078] The properties of the antioxidant spice compositions prepared by the methods in Examples 1-5 and Comparative Examples 1-5 are shown in Table 1.

[0079] DPPH scavenging rate reflects the composition's ability to scavenge DPPH free radicals; a higher value indicates stronger antioxidant activity. DPPH scavenging rate determination method: Take an appropriate amount of the antioxidant spice composition, dilute it to a suitable concentration with anhydrous ethanol, add 0.1 mM DPPH ethanol solution, react in the dark for 30 minutes, measure the absorbance at 517 nm, and calculate the scavenging rate.

[0080] FRAP value reflects the composition's ability to deliver Fe 3+ Reduced to Fe 2+ The ability to reduce total reducing power (FRAP) is an important indicator for evaluating total reducing power. The FRAP value determination method involves mixing the composition with FRAP working solution (containing TPTZ, FeCl3, and acetate buffer), reacting at 37°C for 10 minutes, and measuring the absorbance at 593 nm. A standard curve is plotted using FeSO4 standard solution, and the results are expressed as μmol Fe... 2+ / g represents.

[0081] Table 1. Performance of the antioxidant spice compositions prepared by the methods of Examples 1-5 and Comparative Examples 1-5

[0082]

[0083] Note: "-" indicates that it cannot be measured (stratification).

[0084] The total phenol content was determined by the Folin-Ciocalteu method, expressed as gallic acid equivalent.

[0085] The particle size D90 is the cumulative 90% particle size of the dispersed phase particles.

[0086] As shown in Table 1, in Examples 1-3, the extraction oil used was high-oleic sunflower seed oil:MCT at a mass ratio of 1.5-4:1, with a total phenol content of 52.7-72.3 mg GAE / g and a dispersed phase D90 < 2 μm in the composition. Within the compounding ratio range of this invention, the total phenol content can be effectively controlled by adjusting the compounding ratio of high-oleic sunflower seed oil to medium-chain triglycerides; when the ratio approaches 2.3:1, the extraction system shows better matching with different polarity phenolic substances in spices, and the total phenol content is at a higher level.

[0087] Example 4 used olive oil:MCT = 2.3:1 as the extraction oil, with a total phenol content of 68.1 mg GAE / g, slightly lower than the 68.4 mg GAE / g in Example 1. This indicates that although different high-oleic acid vegetable oils can all synergistically construct polar gradient extraction media with medium-chain triglycerides, high-oleic acid sunflower seed oil has a slightly better extraction efficiency for spice phenolic substances in the system of this invention than olive oil.

[0088] Example 5 used a ternary blend of high-oleic sunflower seed oil, olive oil, and MCT (1:1.3:1) as the extraction oil, achieving a total phenol content of 69.6 mg GAE / g, a further improvement over Example 1. This indicates that blending multiple oils can further optimize the polarity distribution of the extraction medium, resulting in more complete dissolution of phenolic substances of different polarities.

[0089] The DPPH scavenging rates of Examples 1, 3, and 5 all exceeded 83%, and the FRAP values ​​all exceeded 850 μmol Fe. 2+ / g, proving that the compound vegetable oil and the partitioned extraction process effectively enriched highly active antioxidant components.

[0090] Comparative Example 1 used a single high-oleic sunflower seed oil instead of the compound vegetable oil for extraction, with all other process parameters identical to Example 1. The resulting composition had a total phenolic content of 52.1 mg GAE / g, a 23.8% decrease compared to Example 1 (68.4 mg GAE / g). The DPPH scavenging rate and FRAP value were correspondingly lower, confirming the synergistic effect of the compound vegetable oil in the extraction process—the polar gradient extraction medium constructed from the combination of high-oleic vegetable oil and medium-chain triglycerides can more comprehensively extract phenolic substances of different polarities from spices.

[0091] Comparative Example 2 employed undivided extraction, mixing all oil-soluble and water-soluble raw materials before alcohol extraction. The resulting extract had a total phenol content of only 46.3 mg GAE / g, a decrease of 32.3% compared to Example 1. This is because the polar gradient extraction advantage of high-oleic acid vegetable oil and MCT could not be utilized during mixed extraction, and the selectivity of the alcohol-water system for extracting components of different polarities was weakened, leading to the loss of active ingredients.

[0092] Comparative Example 3 used natural cooling instead of flash cooling. Although the total phenol content was basically the same as in Example 1, at 67.8 mg GAE / g, the particle size D90 was greater than 10 μm. This is because after high-speed shearing and fragmentation, the fine droplets are in a high surface energy state. If the cooling rate is too slow (about 1 °C / min), the droplets have enough time to collide and merge, leading to a gradual increase in particle size. However, the flash cooling of 10~15 °C / min used in this invention can quickly fix the morphology of the fragmented droplets, preventing them from agglomerating and fixing them in the oil phase as tiny particles. The results of Comparative Example 3 verify the key role of flash cooling in maintaining the dispersed phase size and ensuring the stability of the system.

[0093] Comparative Example 4 did not undergo high-pressure homogenization after shear dispersion and flash cooling, and the resulting composition had a particle size D90 of 5~8μm. This indicates that high-pressure homogenization is a necessary step to obtain submicron particle sizes.

[0094] Although the total phenol content of Comparative Examples 3 and 4 was comparable to that of Example 1 (67-68 mg GAE / g), the antioxidant index was lower due to the large particle size (>10 μm or 5-8 μm), proving that the microstructure has an important influence on the activity.

[0095] After adding emulsifier, the particle size of Comparative Example 5 met the standard, and the antioxidant index was close to that of Example 1, but slightly lower, indicating that the emulsifier may slightly interfere with the interfacial antioxidant activity.

[0096] The antioxidant spice compositions prepared by the methods of Examples 1-5 and Comparative Examples 1-5 were added to freshly prepared chili oil at 70°C at an amount of 2% of the total mass of the chili oil, forming Examples 1-1, 2-1, 3-1, 4-1, 5-1 and Comparative Examples 1-1, 2-1, 3-1, 4-1, 5-1. Simultaneously, the chili oil prepared by the method of Example 1 was added to freshly prepared chili oil at 60°C at an amount of 0.5% of the total mass of the chili oil, forming Examples 1-2. The chili oil prepared by the method of Example 1 was added to freshly prepared chili oil at 80°C at an amount of 3% of the total mass of the chili oil, forming Examples 1-3.

[0097] The preparation methods for chili oil include the following:

[0098] Take 100g of chili powder (coarse to fine powder in a 1:1 ratio) and place it in a stainless steel container. Heat 500g of rapeseed oil to 160℃, add 20g of sliced ​​onion, 15g of ginger slices, and 20g of scallion segments, and fry over low heat until golden brown. Remove the onion and scallion segments. Raise the oil temperature to 180℃, then turn off the heat and let it cool naturally to 150℃. Pour 1 / 3 of the hot oil into the chili powder and stir quickly. When the oil temperature drops to 120℃, add another 1 / 3 of the hot oil and stir. When the oil temperature drops to 90℃, add the remaining hot oil and stir well. Let it stand for 24 hours, then filter to remove the chili residue. You will then have freshly prepared chili oil.

[0099] The properties of the red oil with the above-mentioned antioxidant spice composition were determined, and the results are shown in Table 2.

[0100] Table 2 Performance of Red Oil with Added Antioxidant Spices

[0101]

[0102] Note: The induction period was determined using the accelerated oxidation method at 60℃, and the time it takes for the peroxide value to reach 0.25 g / 100g was taken as the time.

[0103] As shown in Table 2, all samples from Examples 1-1 to 5-1, 1-2, and 1-3 did not exhibit stratification or precipitation after centrifugation at 4000 rpm for 30 minutes, and remained stable after 180 days of storage at room temperature, highly consistent with the centrifugation results. This indicates that the antioxidant spice composition prepared in this invention possesses excellent physical stability in the red oil system and can meet the shelf-life requirements for practical applications.

[0104] Although the total phenol content of Comparative Example 1-1 was significantly lower than that of Example 1, its induction period could still reach 18-20 days, and the particle size D90 was less than 2 μm, with no stratification after centrifugation. This indicates that although the total amount of antioxidants decreased due to insufficient extraction efficiency of single vegetable oil extraction, it did not affect the stable dispersion structure formed by the S300 process.

[0105] In ratio 2-1, because no partitioned extraction was used, the extract contained both highly polar and non-polar components. When red oil was added directly, the highly polar substances rapidly aggregated and precipitated due to their poor affinity with the oil phase, preventing the system from forming a stable dispersion. After centrifugation, obvious stratification occurred, and the induction period was only 12-14 days. This clearly demonstrates that only by enriching different polar components separately using S100 and S200 can a suitable material basis be provided for subsequent physical dispersion. Partitioned extraction is a prerequisite for the entire technical solution.

[0106] Comparative Example 3-1 used natural cooling instead of flash cooling after shear dispersion, resulting in a particle size increase to over 10 μm. Significant precipitation occurred after centrifugation, and the induction period was shortened to 16-18 days. This is because the fine droplets formed by high-speed shear are in a high surface energy state. If the cooling rate is too slow (approximately 1 °C / min), the droplets have sufficient time to collide and merge. However, the flash cooling of 10-15 °C / min used in this invention rapidly "freezes" the fragmented droplet morphology, fixing them in the oil phase as tiny particles before they can aggregate. This verifies the crucial role of flash cooling in maintaining the dispersed phase size and ensuring system stability. Furthermore, data from Examples 1-1 and 3-1 show that when the total phenol content is similar, particle size becomes the key factor determining the induction period.

[0107] Comparative Example 4-1, without high-pressure homogenization after shear dispersion and flash cooling, resulted in a composition with a particle size D90 of 5-8 μm. Slight precipitation occurred after centrifugation, with an induction period of 18-20 days. Although shear dispersion broke the extract to the micron level, particles of 5-8 μm still could not completely resist gravitational sedimentation and would slowly precipitate during long-term storage. This invention further refines the particle size to below 2 μm through high-pressure homogenization at 25-35 MPa, ensuring that the Brownian motion of the particles is sufficient to resist sedimentation and achieve kinetic stability. Comparative Example 4 demonstrates that high-pressure homogenization is a necessary step to move a dispersion system from short-term stability to long-term stability.

[0108] Comparative Example 5-1 achieved stability using a traditional emulsification method with the addition of polyglycerol ricinoleate (1%). Although the particle size met the standard (<2μm) and no stratification occurred after centrifugation, the induction period was 22-24 days, slightly shorter than the 24 days or more in Example 1, and non-natural ingredients were introduced into the ingredient list. This is because the added emulsifier and the antioxidant components compete for adsorption at the oil-water interface, potentially occupying some interfacial sites and affecting the enrichment and interfacial activity of polar antioxidants (such as tea polyphenols and rosmarinic acid), thus slightly weakening the antioxidant efficiency. In contrast, the dispersion system constructed by the present invention through a purely physical pathway requires no emulsifier, and the interface is entirely occupied by the antioxidant components themselves, ensuring both the natural properties of the ingredient list and maximizing antioxidant efficacy.

[0109] The above results show that the antioxidant spice composition of the present invention can effectively exert its antioxidant effect and has good physical stability within the addition range of 0.5-3% and addition temperature range of 60-80℃.

Claims

1. A method for preparing an antioxidant spice composition, characterized in that, Includes the following steps: S100. Add oil-soluble raw materials to compound edible vegetable oil, extract under medium temperature conditions, filter and take the obtained oil. S200. The water-soluble raw material is added to an ethanol-water solution, refluxed for extraction, and then post-processed to obtain a paste-like extract. S300. After heating the above-mentioned oil and extract, the mixture is dispersed by high-speed shearing, cooled, and then uniformly refined to obtain the target composition. The mass ratio of the oil to the extract is 10:0.5~2; the compounded edible vegetable oil is made by compounding high oleic acid vegetable oil and medium chain triglycerides in a mass ratio of 1.5~4:

1.

2. The preparation method according to claim 1, characterized in that, By weight, The oil-soluble ingredients include: 15-25 parts star anise, 10-20 parts cinnamon, 8-15 parts cardamom, 10-18 parts amomum villosum, 20-30 parts fennel seeds, and 5-10 parts bay leaves; Water-soluble ingredients include: 8-12 parts cloves, 15-25 parts licorice, 10-20 parts rosemary, 10-15 parts perilla, and 5-10 parts green tea.

3. The preparation method according to claim 1, characterized in that, In step S100, the oil-soluble raw material is washed, dried, crushed to 20-40 mesh, and then added to edible vegetable oil. It is then extracted at a constant temperature of 60-80℃ for 2-4 hours, filtered, and the resulting oil is collected. The mass ratio of the oil-soluble raw material to the edible vegetable oil is 1:2-4.

4. The preparation method according to claim 3, characterized in that, The high-oleic acid vegetable oil is selected from one or both of high-oleic acid sunflower seed oil and olive oil.

5. The preparation method according to claim 1, characterized in that, In step S200, the water-soluble raw material is washed, dried, crushed to 25-40 mesh, added to an ethanol aqueous solution, and extracted by reflux at 50-70℃ for 1-3 hours. After filtration, the filtrate is concentrated under reduced pressure to recover the ethanol and obtain an extract in the form of a paste.

6. The preparation method according to claim 5, characterized in that, The mass ratio of the ethanol aqueous solution to the water-soluble raw material is 6~10:1; the volume fraction of ethanol in the ethanol aqueous solution is 40~75%.

7. The preparation method according to claim 1, characterized in that, In step S300, the extract is softened at 40-50°C; the oil is heated to 70-80°C, the extract is added to the oil, sheared at 3000-4000 rpm for 20-30 minutes, rapidly cooled to below 25°C at a rate of about 10-15°C / min, and homogenized under high pressure to obtain the target composition.

8. The preparation method according to claim 7, characterized in that, High-pressure homogenization includes the following: pressure of 25~35MPa, number of cycles of 1~3.

9. An antioxidant spice composition prepared by the method according to any one of claims 1 to 8, characterized in that, The dispersed phase particle size D90 in the composition is < 2 μm.

10. The application of the antioxidant spice composition as described in claim 9 in the preparation of red oil products, characterized in that, The antioxidant spice composition is added after the chili oil is cooked and cooled to 60-80°C, and the amount added is 0.5-3% of the total mass of the chili oil.

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