Preparation method of high-fragrance osmanthus concentrated liquid suitable for beverage wine

Abstract

The application discloses a preparation method of a high-fragrance osmanthus concentrated solution suitable for beverage wine, relates to the technical field of osmanthus concentrated solution processing, and comprises the following steps: vacuum drying fresh osmanthus, sequentially performing vacuum low-temperature extraction and composite enzyme hydrolysis water extraction, respectively preparing osmanthus fragrance component extraction liquid and osmanthus taste component extraction liquid, mixing the two kinds of extraction liquid, performing low-temperature aging, centrifugation and filtration to obtain a clear liquid, filtering water out by using a reverse osmosis membrane, detecting fragrance markers of the concentrated solution, determining at least nine characteristic fragrance markers and actual measured contents of the nine characteristic fragrance markers, comparing the actual measured contents with standard target contents of the markers, backfilling fragrance when the concentrated solution does not meet the requirements, and completing preparation of the osmanthus concentrated solution when the comprehensive compliance rate and the single compliance rate of the contents of all the fragrance markers are within the set numerical range. The application solves the problems of high-concentration retention of fragrance substances and consistency of fragrance proportions in preparation of the osmanthus concentrated solution.

Description

Technical Field

[0001] This invention relates to the field of osmanthus concentrate processing technology, and more specifically, to a method for preparing a highly aromatic osmanthus concentrate suitable for alcoholic beverages. Background Technology

[0002] Osmanthus has a strong floral fragrance and high edible and medicinal value. It can also be used as a natural flavoring ingredient in the food and beverage industry. Fresh osmanthus flowers are usually dried with hot air and then extracted. Osmanthus concentrate is prepared by hot evaporation and concentration technology and used to blend perfumes, beverages, and food.

[0003] However, when commercially available osmanthus concentrate is actually used in alcoholic beverages, the traditional extraction process cannot effectively remove these soluble macromolecules because the osmanthus raw material contains a large amount of pectin, protein, and crude fiber. When the conventional osmanthus concentrate is added to alcoholic beverages, especially high-proof alcoholic beverages, the high polarity of ethanol easily leads to the "alcohol precipitation" of pectin and protein, producing a large amount of flocculent precipitate. This is one of the defects of existing osmanthus alcoholic beverages. These flocculent precipitates can easily interfere with the flavor stability of alcoholic beverages and reduce the appearance quality of alcoholic beverage products.

[0004] In addition, when using traditional petal fragrance extraction processes, the key volatile aroma substances in osmanthus (such as β-linalool, β-ionone, γ-decanoic acid lactone, etc.) are highly heat-sensitive and are easily lost or thermally degraded in large quantities during traditional high-temperature distillation or high-temperature concentration extraction processes. This results in a significant decrease in the aroma intensity of the osmanthus concentrate, making it impossible to maintain a high concentration of osmanthus aroma and flavor. Furthermore, prolonged high-temperature extraction can easily lead to excessive dissolution of bitter substances such as flavonoid glycosides and terpene lactones in osmanthus. In a high-alcohol environment, ethanol has an amplifying effect on the perception of bitterness, making the bitterness of the product more pronounced.

[0005] Moreover, due to the influence of different growing environments (sunlight, soil, pests) and different growth conditions (variety, plant health status), the aroma component content of different varieties and different plants of the same variety is prone to significant fluctuations. Traditional processes lack precise quantitative control methods, resulting in poor consistency of aroma quality among different batches of osmanthus concentrate, which cannot meet the requirements for quality stability and flavor stability in the beverage formulation process.

[0006] Existing Chinese patent CN108740166A discloses a method for preparing tea concentrate with aroma refilling, including steps such as supercritical CO2 extraction of tea aroma, deodorized tea leaf water extraction and concentration enzymatic hydrolysis, and aroma refilling. However, the technical solution of this patent is designed for the application of tea concentrate in non-alcoholic beverages, and does not address the unique technical issues of controlling alcohol precipitation, suppressing bitterness, and preserving aroma authenticity of osmanthus raw materials in high-proof liquor applications. Furthermore, its aroma refilling method is based on empirical proportional mixing, lacking precise quantitative control methods. Summary of the Invention

[0007] The purpose of this invention is to provide a method for preparing a high-fragrance osmanthus concentrate suitable for alcoholic beverages, which solves the problems of high concentration retention of aroma substances and consistent aroma ratio in the preparation of osmanthus concentrate.

[0008] The embodiments of the present invention are achieved through the following technical solutions:

[0009] A method for preparing a high-fragrance osmanthus concentrate suitable for alcoholic beverages includes the following steps:

[0010] Step 1: Vacuum dry the fresh osmanthus flowers at a temperature not exceeding 40℃.

[0011] Step 2: The dried osmanthus flowers are subjected to low-temperature extraction and enzymatic hydrolysis in water extraction to extract the aroma components and flavor components of osmanthus flowers, respectively.

[0012] Step 2.1: Extract the aroma components of dried osmanthus flowers using supercritical CO2 fluid extraction to obtain an extract and deodorized osmanthus flower residue. The extraction temperature should not exceed 45℃.

[0013] Step 2.2: Add the deodorized osmanthus residue to the compound enzyme solution and perform a three-stage gradient temperature extraction to obtain the osmanthus flavor component extract.

[0014] In step 2.2, the complex enzyme includes pectinase, cellulase and protease.

[0015] Step 3: Mix the osmanthus aroma component extract and the osmanthus flavor component extract from Step 2, and then perform low-temperature aging, centrifugation, coarse filtration through a ceramic membrane, and fine filtration through an ultrafiltration membrane to obtain a clear liquid.

[0016] Step 4: Use a reverse osmosis membrane to filter out the water from the clarified liquid to obtain osmanthus concentrate.

[0017] Step 5: Detect the aroma markers of osmanthus in the concentrate from Step 4 using the HS-SPME-GC-MS method to identify at least 9 characteristic aroma markers and their measured contents. Compare these contents with the set standard target contents for each marker. For aroma markers whose measured contents do not match the standard contents, perform aroma backfilling. When the overall compliance rate and the compliance rate of each aroma marker are within the set value range, the osmanthus concentrate preparation is complete.

[0018] Step 6: After sterilizing the concentrated solution prepared in Step 5 at high temperature, cold fill it.

[0019] The three-stage gradient heating extraction process is as follows:

[0020] The first temperature setting is 40℃, and the temperature is kept constant for 1 hour.

[0021] The second stage involves setting the temperature to increase from 40℃ to 55℃ at a rate of 1℃ / min, and then maintaining the temperature for 2 hours.

[0022] The third setting gradually increases the temperature from 55℃ to 70℃ at a rate of 1℃ / min, and then holds the temperature at that temperature for half an hour.

[0023] The nine characteristic aroma markers in osmanthus include β-linalool, β-ionone, α-ionone, γ-decanoic acid lactone, cis-linalool oxide, trans-linalool oxide, cis-ocimene, 4-hexenyl acetate, and dihydro-β-ionone.

[0024] In step 5, at least 10 batches of fresh osmanthus samples are taken, and osmanthus concentrate is prepared according to the methods described in steps 1 to 4. The content of 9 characteristic aroma markers in osmanthus is detected by HS-SPME-GC-MS method for each batch of osmanthus concentrate. The arithmetic mean of the content determination results of at least 10 batches is used as the standard target content of the 9 characteristic aroma markers in osmanthus.

[0025] The aroma refilling steps are as follows:

[0026] S5.1 Calculate the weight of the aroma markers that need to be added to the osmanthus concentrate obtained in step 4, and then convert it into the mass of the aroma supplement liquid.

[0027] S5.2 Stir the osmanthus concentrate at low speed and room temperature in a sealed environment.

[0028] S5.3. Inject the aroma replenishing solution into the osmanthus concentrate at a rate of 0.5 mL / min.

[0029] S5.4 After the aroma replenishment solution is injected, continue stirring for 15 minutes, and then let it stand for 2 hours to equilibrate.

[0030] S5.5. The osmanthus concentrate after backfilling is retested using the HS-SPME-GC-MS method. The overall compliance rate and the compliance rate of individual markers are recalculated to see if they are both within the set range. If both the overall compliance rate and the compliance rate of individual markers are within the set range, the aroma backfilling is considered complete. If one or more markers are not within the set range, the aroma backfilling step is repeated.

[0031] In step S5.5, the numerical range for the overall compliance rate and the compliance rate of a single marker is set to 0.98-1.02.

[0032] In step 1, the drying time for fresh osmanthus flowers ranges from 4 to 6 hours. The moisture content of the osmanthus raw material is checked every hour. When the moisture content of the fresh osmanthus flowers is not higher than 8%, the vacuum drying is completed.

[0033] In step 3:

[0034] The low-temperature aging process involves placing the mixture in a cold settling tank and letting it stand at 2°C for 18 hours.

[0035] The centrifugation process involves taking the supernatant formed by settling and centrifuging it in a disc centrifuge.

[0036] The ceramic membrane coarse filtration process involves passing the centrifuged supernatant through a ceramic membrane with a pore size of 0.1 μm for coarse filtration.

[0037] The ultrafiltration membrane fine filtration process involves passing the supernatant after coarse filtration through an ultrafiltration membrane with a molecular weight cutoff of 20 kDa to obtain a clarified liquid.

[0038] The ratio of pectinase, cellulase and protease added is 5:3:2.

[0039] The technical solutions of the embodiments of the present invention have at least the following advantages and beneficial effects:

[0040] 1. The present invention provides a method for preparing a high-aroma osmanthus concentrate suitable for alcoholic beverages. This method separates and extracts aroma components from flavor components, utilizing low-temperature extraction to reduce the loss of osmanthus aroma caused by traditional high-temperature pyrolysis, thus maintaining a high aroma concentration. For flavor components, a complex enzymatic hydrolysis combined with multi-stage heating and low-temperature extraction is employed. This process enzymatically hydrolyzes turbidity-causing macromolecules such as pectin, fiber, and protein, simultaneously extracting flavor-active substances. This reduces the residue of precipitates and bitter substances in the osmanthus concentrate, further enhancing the aroma and flavor of the osmanthus concentrate when used in alcoholic beverage formulations, and maintaining the clarity after formulation.

[0041] 2. The present invention provides a method for preparing high-aroma osmanthus concentrate suitable for alcoholic beverages. Through aroma backfilling technology, using the standard target content of nine characteristic aroma markers as a reference, the method precisely backfills the aroma replenishment liquid by meeting the requirements of comprehensive compliance rate and single-component compliance rate. This ensures that the content and proportion of the nine key aroma components in each batch of product remain within the same required range, reducing the aroma variation coefficient between different batches, thereby forming a stable aroma and flavor, facilitating subsequent blending and application in alcoholic beverages. Detailed Implementation

[0042] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. The detailed description of the embodiments of the present invention is not intended to limit the scope of the claimed invention, but merely to illustrate selected embodiments of the invention. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0043] Example 1

[0044] Ingredient ratio: 10kg of fresh osmanthus flowers.

[0045] In this embodiment, the preparation method of a high-fragrance osmanthus concentrate is as follows:

[0046] Step 1: Select freshly picked osmanthus flowers as raw material. After removing stems, leaves, residue, and damaged flowers, spread the fresh osmanthus flowers evenly on the surface of a vacuum drying tray, with a thickness not exceeding 2cm (to reduce the thickness, as excessive thickness will affect the drying time). Then, place the vacuum drying tray into a vacuum drying oven (model DZF-6090), and adjust the heating temperature to 35℃ (not exceeding 40℃) for vacuum drying for 4-6 hours, until the petals of the fresh osmanthus flowers begin to curl slightly. During this process, check the moisture content of the osmanthus raw material every hour. When the moisture content is not higher than 8% (detected by a halogen moisture analyzer, model MB25), turn off the vacuum and heating, and introduce nitrogen to break the vacuum. Remove the dried and dehydrated osmanthus raw material, cool it to room temperature, and then seal and store it for later use.

[0047] It is worth noting that the purpose of vacuum heating and drying is that, in a vacuum environment, the boiling point of water is lowered, and the water inside the vacuoles in the osmanthus petal cells can quickly vaporize and expand at a lower temperature, creating micropores in the cell walls to achieve physical cell wall disruption and improve the mass transfer efficiency of subsequent extraction. The vacuum environment can also prevent oxidative browning of osmanthus during the drying process, maintaining the golden color and complete aroma and flavor of the osmanthus petals.

[0048] It is worth noting that the reason for not heating the temperature above 40℃ is that the volatilization temperature critical point of most of the volatile aromatic components in osmanthus (such as β-linalool, β-ionone, etc.) is about 40-45℃. If the drying temperature exceeds 40℃, these aromatic substances will easily volatilize and be lost quickly. Therefore, controlling the drying temperature below 40℃ can effectively preserve the osmanthus aromatic substances in the dried osmanthus.

[0049] Step 2: The dried osmanthus flowers were subjected to vacuum low-temperature extraction and enzymatic hydrolysis in water extraction to obtain osmanthus aroma component extract and osmanthus flavor component extract, respectively.

[0050] Step 2.1: Weigh 3 kg of dried osmanthus flowers from Step 1 and put them into the extraction tank of the low-temperature extraction device for low-temperature extraction.

[0051] The extraction process involves maintaining the extraction temperature in the extraction tank at 35°C using a constant-temperature water bath. CO2 is introduced into the tank, and CO2, in its supercritical state, exhibits both gas-liquid properties, high diffusivity, and low viscosity, allowing it to fully contact the osmanthus flowers and dissolve and extract the aromatic components. The CO2 and aromatic components are then refluxed back into the extraction tank through condensation (below 0°C) (gas-liquid separation). After continuous extraction for at least 3 hours, a pale yellow, transparent, oily liquid is collected in the extraction tank, which is the osmanthus aromatic component extract. This extract is then collected and sealed for low-temperature storage.

[0052] Two collection bottles are set up when collecting the floral aroma component extract in the extraction tank: a main collection bottle and a secondary collection bottle. The main collection bottle collects 12.3g of osmanthus aroma component extract, which is used to mix with the flavor component extract in the subsequent step 3. Finally, the secondary collection bottle collects about 2-3g of the remaining osmanthus aroma component extract, which is used as the aroma replenishment liquid in the aroma backfilling step in the subsequent step 5.

[0053] Among them, 2.85 kg of osmanthus residue after deodorization remained in the extraction tank.

[0054] It is worth noting that the low-temperature extraction device is an existing device (model TQ-300L) that uses supercritical low-temperature extraction technology (such as supercritical CO2 fluid extraction). It uses fluid in a supercritical state as a solvent to extract components with different solubilities from osmanthus. Moreover, the low temperature can reduce the oxidation and dissipation of heat-sensitive substances in osmanthus, so that they can still retain their effective function and be extracted.

[0055] Step 2.2: Load 2.85 kg of osmanthus residue obtained in Step 2.1 into an enzymatic hydrolysis reactor (model FMG-50L). Add 22.8 L of purified water at a material-to-liquid ratio of 1:8 (the material-to-liquid ratio in traditional enzymatic hydrolysis is generally in the range of 1:6-1:9; in this embodiment, 1:8 is selected). Turn on the stirrer and stir at low speed (60 rpm). Prepare a compound enzyme solution and add it to the enzymatic hydrolysis reactor. Adjust the pH to 5.0 with food-grade citric acid to create a suitable environment for enzymatic hydrolysis. Then, perform a three-stage gradient temperature extraction.

[0056] The preparation method for the complex enzyme solution is as follows:

[0057] Weigh out 15g of food-grade pectinase, 9g of cellulase, and 6g of protease, and dissolve them in 100mL of purified water at room temperature to prepare a compound enzyme solution.

[0058] The reason for using 15g of food-grade pectinase, 9g of cellulase, and 6g of protease in different proportions is that the main components of osmanthus cell walls include pectin (approximately 8-12%), cellulose (approximately 12-18%), and a small amount of protein (approximately 6-10%). Among them, the amount of pectinase added is the highest (accounting for 50%) because pectin is the main turbid substance in osmanthus extract that causes "alcohol precipitation" and is also the main macromolecule that encapsulates and adsorbs flavor substances. Fully degrading pectin is crucial for subsequent clarification and the release of flavor substances. The amount of cellulase added is the second highest (accounting for 30%), which aims to break down the fibrous skeleton of osmanthus cell walls, release intracellular contents, and improve the extraction rate of total soluble solids. The amount of protease added is relatively low (accounting for 20%) because the protein content in osmanthus raw materials is relatively low, and excessive protein hydrolysis may produce bitter peptides, affecting the taste of the product.

[0059] Eight experimental groups were set up, with 2.85 kg of osmanthus residue in each group. The enzymes added to each group were dissolved in 100 mL of purified water at room temperature. The comparison table of each enzyme at different g values ​​is shown below:

[0060] Table 1: Comparison of enzymatic hydrolysis results of different enzyme preparations

[0061]

[0062] As shown in the table above, when the amount of pectinase added exceeds 15g, the increase in the pectin degradation rate in the osmanthus residue mixture is very small with the increase of pectinase dosage; when the amount of cellulase added exceeds 9g, the increase in the cellulose degradation rate in the osmanthus residue mixture slows down with the increase of cellulase dosage; when the amount of protease added exceeds 6g, the increase in the protein degradation rate in the osmanthus residue mixture is very small with the increase of protease dosage. Considering that enzyme preparations all have a certain taste, and taking into account both cost-effectiveness and flavor cleanliness, the degradation rate of the three enzymes is optimal when the ratio reaches 5:3:2, which is the best ratio.

[0063] Please refer to Table 2 for the enzymatic hydrolysis process of water extraction with three-stage gradient temperature increase:

[0064] The first stage of low-temperature activation enzymatic hydrolysis involves setting the external water bath temperature of the enzymatic hydrolysis reaction vessel to 40°C and maintaining this temperature for 1 hour.

[0065] The reason for setting the first stage temperature to 40℃ is that 40℃ is the optimal reaction temperature for pectinase. At this temperature, pectinase is preferentially activated, rapidly degrades pectin substances, reduces the viscosity of the extract, and allows the flavor substances encapsulated by pectin to be initially released. 40℃ is also a temperature range where the volatility of osmanthus aroma components is relatively low, which can reduce the continued loss of a small amount of aroma substances that may remain in the deodorization residue.

[0066] The second stage involves medium-temperature high-efficiency enzymatic hydrolysis. The temperature of the water bath outside the enzymatic hydrolysis reactor is gradually increased to 55°C at a rate of 1°C / min, and then kept at a constant temperature for 2 hours.

[0067] The reason for setting the second stage temperature to 55℃ is that 55℃ is the optimal reaction temperature for cellulase and protease. At this temperature, cellulase is activated and can effectively degrade the cellulose skeleton in the cell wall of osmanthus, promoting the full release of intracellular flavor substances. Protease is activated and degrades residual protein, releasing amino acids with a sweet taste (such as glutamic acid and aspartic acid). This is the main enzymatic hydrolysis process, so a 2-hour incubation time is required to ensure that cellulose and protein are fully hydrolyzed, increasing the soluble solids content.

[0068] The third stage of high-temperature enzyme inactivation involves gradually increasing the temperature of the water bath outside the enzymatic reaction vessel to 70°C at a rate of 1°C / min, and then maintaining the temperature at this rate for half an hour.

[0069] The reason for setting the third stage temperature at 70℃ is that pectinase, cellulase, and protease begin to rapidly inactivate and become inactive. Maintaining this temperature for 30 minutes ensures complete inactivation of all three enzymes, preventing excessive enzyme activity that could lead to flavor degradation (such as the production of bitter peptides from excessive protein hydrolysis) and reducing the risk of darkening of color or the development of a cooked taste due to prolonged high temperatures. Simultaneously, the 70℃ extraction temperature helps increase the solubility of some high-boiling-point flavor compounds (such as flavonoids and polyphenols), enhancing the richness and sweetness of the extract.

[0070] After enzymatic hydrolysis, the enzymatic hydrolysis reaction vessel contained a turbid liquid with osmanthus residue. After filtration through a stainless steel screen, 21.5L of filtrate was obtained, which was the extract of osmanthus flavor components. This filtrate was collected and stored in a sealed container at low temperature.

[0071] Table 2: Three-stage gradient temperature enzymatic hydrolysis and water extraction

[0072]

[0073] In order to obtain a clear extract and reduce the impact of suspended particles in the extract on the color and aroma of the osmanthus concentrate, the extract needs to be clarified.

[0074] Step 3: Add 12.3g of osmanthus fragrance component extract to 21.5L of osmanthus flavor component extract, stir thoroughly for 15min to ensure uniform mixing, then place in a cold settling tank and let stand at 2℃ for 18 hours for low-temperature aging. Then, collect 20L of the supernatant formed during the settling process and centrifuge it in a disc centrifuge (model DHC270) to obtain 19.2L of supernatant. Then, pass the centrifuged supernatant sequentially through a ceramic membrane (Al2O3-ZrO2 composite ceramic membrane) with a pore size of 0.1μm, a hollow fiber ultrafiltration membrane (material is polyethersulfone PES, molecular weight cutoff is 20kDa) for coarse filtration and fine filtration to obtain 17.8L of clear liquid. The changes in solution at different process stages during the preparation of the clear liquid from the mixed solution are shown in Table 3.

[0075] Table 3: Preparation of Clarified Liquid

[0076]

[0077] After the extract is initially clarified, the clarified liquid still contains a lot of water, which has a certain dilution effect on the aroma concentration of osmanthus. The aroma compounds in the clarified liquid are soluble substances, and it is difficult to directly remove water and concentrate them by traditional methods of settling, centrifugation and filtration.

[0078] Step 4: Pump 17.8L of clarified liquid into the reverse osmosis membrane for continuous osmosis concentration. This concentrates the soluble substances (such as sugars, vitamins, minerals, and aroma compounds) remaining in the clarified liquid, allowing only water molecules in the clarified liquid to pass through. This concentrates the osmanthus-infused clarified liquid containing aroma compounds, while preserving the aroma components in the liquid from loss during the concentration process.

[0079] It is worth noting that components that can produce turbidity (such as fibrous substances, large protein molecules, and osmanthus micro-fragments) are removed in steps 2.2 and 3 above. Therefore, the soluble substances in the concentrated clarified liquid in the reverse osmosis membrane are mainly volatile aroma compounds, small molecule sugars, amino acids, phenylethanol compounds, flavonoids, and pigment compounds.

[0080] Please refer to Table 4. After 17.8L of clarified liquid is concentrated through reverse osmosis membrane, 1.6L of concentrated liquid is obtained. At this time, the soluble solids content in the blocked concentrated liquid reaches the maximum value of 22°Brix (if solids precipitate during concentration, they are filtered out simultaneously).

[0081] Table 4: Reverse Osmosis Concentration of Clarified Liquid

[0082]

[0083] Among them, the aroma components of osmanthus mainly include β-linalool, β-ionone, α-ionone, γ-decanoic acid lactone, cis-linalool oxide, trans-linalool oxide, cis-ocimene, 4-hexenyl acetate, dihydro-β-ionone and other aroma compounds. When osmanthus concentrate is formulated into beverages, the unique aroma atmosphere of osmanthus concentrate can be generated through the above aroma compounds.

[0084] Specifically, β-linalool has a lily of the valley fragrance, a fresh aroma with slight woody and citrus notes. β-linalool has the highest content in the total aroma components of osmanthus concentrate, contributing to the volume and fullness of the overall osmanthus aroma and serving as the builder of the osmanthus aroma framework.

[0085] Specifically, β-ionone has a strong characteristic osmanthus floral fragrance with a complex aroma of violet, raspberry and cypress. It has strong diffusion power, can form a sweet and rich fragrance, and has a very low odor threshold (about 0.007 μg / L in water). Even a small amount can be detected by the sense of smell.

[0086] Specifically, α-ionone has a soft and sweet violet fragrance, which is milder and more fruity than β-ionone, with a faint aroma of cedarwood and raspberry. It works synergistically with β-ionone to create the fragrance characteristics of osmanthus, which has both a strong floral impact and a sweet and soft fruity and woody aroma.

[0087] Specifically, γ-decanoic acid lactone has a strong and sweet peach and coconut milk aroma, with a creamy and fruity character. Although the content of γ-decanoic acid lactone is relatively low (about 1.26% in Osmanthus fragrans), its odor threshold is also very low (about 0.011 μg / L in water), which can contribute to the sweetness and mellowness of Osmanthus concentrate, making Osmanthus concentrate more flavorful in beverages.

[0088] Specifically, cis-linalool oxide has a fresh floral scent with subtle woody and earthy notes, which can enhance the clarity of the osmanthus fragrance.

[0089] Specifically, trans-linalool oxide has a soft, sweet floral scent with a slight camphor-like coolness, which can enhance the freshness and softness of the fragrance.

[0090] Specifically, cis-ocimene has a fresh grassy and herbal scent, accompanied by a faint citrus and tropical fruit aroma. The scent is light and can bring out the natural plant feeling of osmanthus fragrance, reducing the artificial synthetic feel.

[0091] Specifically, 4-hexenyl acetate has a fresh, fruity, and sweet aroma, similar to pear and banana, with a hint of green leaves. It can combine the floral and fruity aromas of osmanthus to form a floral-fruity complex fragrance, increasing the richness and complexity of the osmanthus aroma.

[0092] Specifically, dihydro-β-ionone has a mellow and sweet woody and fruity aroma. It is a slow-release aroma substance. The sweet base aroma of dihydro-β-ionone can be slowly released in alcoholic beverages, providing a lasting aftertaste.

[0093] Furthermore, in order to determine the standard content of each aroma compound in osmanthus, at least 10 batches of fresh osmanthus samples (each batch ≥500g, and all batches were picked at the same time and place to reduce variability) were taken. Osmanthus concentrate was prepared according to the methods described in steps 1 to 4 of the above embodiments. Each batch of product was detected by HS-SPME-GC-MS. By searching the NIST spectral library and comparing the retention index, the key compounds in the osmanthus aroma (the above 9 aroma compounds were taken in this embodiment) were identified. The arithmetic mean of the determination results of 10 batches was used as the standard target content of each marker.

[0094] The characteristic aroma markers and their standard target contents in the osmanthus concentrate prepared according to the method of this invention have been verified through actual process testing, as shown in the table below:

[0095] Table 5: Standard target content of characteristic aroma markers in Osmanthus flower concentrate

[0096]

[0097]

[0098] It is worth noting that the above nine markers cover the main aroma components of Osmanthus fragrans. Among them, AM-01 to AM-08 are common components of Osmanthus fragrans, Osmanthus fragrans var. aurantiacus, and Osmanthus fragrans var. cinnamon. AM-09 (dihydro-β-ionone) is a characteristic component of Osmanthus fragrans and has a relatively high content (relative content 5.42%), which makes an important contribution to the formation of the sweet and rich aroma of Osmanthus fragrans. Therefore, in this embodiment, the above nine aroma compounds are selected as aroma markers for Osmanthus fragrans concentrate. In the Osmanthus fragrans batch implemented in this embodiment, the above standard target content is used as the backfill reference benchmark for aroma deviation compensation.

[0099] It is worth noting that in the actual formulation process of alcoholic beverages using osmanthus concentrate for flavoring, the standard target content of osmanthus concentrate can be set at multiple levels according to the aroma concentration requirements of different alcoholic beverages:

[0100] Grade 1 (rich aroma level) is applicable to strong aroma type baijiu and sauce aroma type baijiu. The standard target content is more than 1.2 times the average value of the measured results of 10 batches in the above examples.

[0101] Level 2 (Aroma Standard Level) is applicable to light-aroma baijiu and low-alcohol blended liquor, with the average value of the measured results of 10 batches in the above examples as the standard target content.

[0102] Level 3 (light aroma) is suitable for ordinary fruit wines and rice wines, with the standard target content being less than 0.8 times the average of the measured results of 10 batches in the above examples.

[0103] Step 5: Take 2g of the concentrated solution from Step 4 and detect the aroma markers of osmanthus using the HS-SPME-GC-MS method. Identify at least 9 characteristic aroma markers and their measured contents, and compare them with the set standard target contents of each marker. For aroma markers whose measured contents do not match the standard contents, perform aroma backfilling.

[0104] This embodiment uses the preparation of a secondary osmanthus concentrate (aroma standard grade) as a requirement, and the detection results of aroma markers in osmanthus are as follows:

[0105] Table 6: Compliance Test of Osmanthus Fragrance Markers

[0106]

[0107] It is worth noting that the measured values ​​of each marker are the contents of the nine characteristic aroma markers determined in the steps of this embodiment.

[0108] Calculation of overall compliance rate R:

[0109] R = (94.6% + 94.1% + 93.5% + 93.9% + 94.3% + 93.6% + 93.5% + 93.8% +93.9%) ÷ 9 = 93.9%

[0110] Therefore, R = 93.9% < 98%, and the compliance rate of each marker is less than 98%, indicating that the content of each aroma marker in the batch of osmanthus concentrate in this embodiment does not meet the standard, and each aroma marker does not meet the target content of the secondary standard for aroma concentration of osmanthus concentrate in the preparation of light-aroma baijiu and low-alcohol blended wine.

[0111] The reason for the above-mentioned substandard results is that the quality of osmanthus aroma varies from batch to batch during the actual concentration process, and the proportions of various aroma markers within the same batch of osmanthus are also inconsistent. If different batches of osmanthus concentrate are directly bottled and shipped for subsequent formulation of alcoholic beverages, the aroma and flavor of the alcoholic beverages formulated from different batches of osmanthus concentrate will also differ (the content of various aroma markers is inconsistent), resulting in inconsistent quality of the formulated alcoholic beverages and making it impossible to maintain a stable and uniform osmanthus aroma.

[0112] To address the aforementioned issues, in this embodiment, the content of each batch of osmanthus aroma markers is measured and compared with the set standard target content of each marker. Aroma markers whose measured content does not match the standard content are individually backfilled to ensure that the content ratio of each aroma marker in each batch of osmanthus concentrate remains consistent.

[0113] In this embodiment, if the compliance rate of each aroma marker component is within the range of 0.98-1.02, the aroma of the current batch of osmanthus concentrate is determined to be compliant. If the compliance rate is not within the range of 0.98-1.02, the aroma of the current batch of osmanthus concentrate needs to be refilled.

[0114] The density of the osmanthus concentrate after reverse osmosis concentration in step 4 was measured using the hydrometer method (or specific gravity method) for measuring liquid food, with reference to the current national standard GB 5009.2 "National Food Safety Standard - Determination of Relative Density of Food". The relative density was measured to be 1.05 g / mL at 20℃. Therefore, the mass of 1.6 L of osmanthus concentrate is: 1.6 L × 1.05 g / mL = 1680 g.

[0115] Table 7: Amount of Aroma Markers Added to Osmanthus Concentrate

[0116]

[0117] The aroma refilling steps are as follows:

[0118] S5.1 Calculate the missing mass N of each marker, and calculate the weight M of the aroma supplement liquid that needs to be added, based on the total amount of osmanthus concentrate and the content of each marker in the osmanthus concentrate.

[0119] in,

[0120] Z is set as the content of each marker in the osmanthus concentrate.

[0121] Table 7 shows the weight M of the aroma replenishment solution required to replenish 1.6L of osmanthus concentrate. However, this aroma replenishment solution is the standard osmanthus concentrate obtained through steps 1-4 in Table 5. In actual aroma backfilling preparation, it is not possible to obtain the standard osmanthus concentrate from a single batch (each batch has differences). Therefore, in actual aroma backfilling preparation, it is necessary to use the osmanthus aroma component extract collected in the secondary collection bottle in step 2 to prepare the aroma replenishment solution to be added.

[0122] In this embodiment, as can be seen from the above steps, 12.3g of the osmanthus fragrance component extract in the main collection bottle is used to prepare 1.6L of osmanthus concentrate (i.e., 1680g). Thus, the final dilution factor of the osmanthus fragrance component extract in the original step 2 is 1680g / 12.3g, which is approximately 136.6 times. Therefore, in step 5, to prepare the fragrance supplement liquid that needs to be added using the osmanthus fragrance component extract in the secondary collection bottle of step 2, the osmanthus fragrance component extract in the secondary collection bottle of step 2 needs to be diluted 136.6 times with pure water to obtain the weight of fragrance supplement liquid that needs to be added as shown in Table 7.

[0123] It is worth noting that, because the 1.6L osmanthus concentrate was mixed with the osmanthus aroma component extract and the flavor component extract in steps 3 and 4, the concentration of each aroma marker component in the original osmanthus aroma component extract was reduced. Furthermore, it underwent low-temperature aging, centrifugation, coarse filtration through a ceramic membrane, fine filtration through an ultrafiltration membrane, and reverse osmosis concentration. This resulted in the loss of some volatile aroma markers, such as evaporation or adsorption by the membrane surface. Therefore, the measured content of each aroma marker in the 1.6L osmanthus concentrate obtained in step 4 (Table 6) will be lower than the aroma component content after direct dilution of the osmanthus aroma component extract. In contrast, the aroma replenishment solution used for aroma refilling is obtained by directly diluting the osmanthus aroma component extract in the secondary collection bottle with pure water, without any loss of aroma components. Therefore, the content of each aroma component in the aroma replenishment solution is higher than the measured content of each aroma component in the osmanthus concentrate. Injecting the aroma replenishment solution into the 1.6L osmanthus concentrate can increase the content of each aroma marker and bring it to the standard target content.

[0124] Table 8: Required Amount of Osmanthus Fragrance Component Extract in Sub-collection Bottle

[0125]

[0126] As shown in Tables 7 and 8, when refilling the osmanthus concentrate with fragrance, the osmanthus fragrance component extract in the secondary collection bottle can be extracted in the range of 0.67g-0.80g, and then diluted with pure water to a weight range of 91.4g-109.5g to obtain the fragrance replenishment solution to be added.

[0127] During the actual aroma backfilling, the average amount of osmanthus aroma component extract added before dilution in Table 8, i.e., 0.75g, is taken to obtain the average weight of aroma supplement liquid to be added for each aroma marker, which is 102.4g.

[0128] It is worth noting that in some feasible embodiments, the spare osmanthus fragrance component extract may be insufficient to make up for all the missing amounts. In this case, food-grade propylene glycol (purity ≥99.5%) can be used as a solvent to dissolve the monomeric fragrance raw materials of each marker that need to be supplemented, and supplemented in the form of osmanthus fragrance.

[0129] S5.2. Pour 1.6L of concentrate into a mixing tank, maintain the temperature at room temperature, then introduce nitrogen into the tank to seal it, and start stirring at low speed.

[0130] S5.3. The aroma replenishment solution prepared in S5.1 is loaded into a micro-injection pump and injected into the stirred tank at a rate of 0.5 mL / min for 20 min. The injection outlet is rotated and set at the stirring shaft of the stirred tank.

[0131] S5.4 After the aroma replenishment solution is injected, continue stirring for 15 minutes, and then let it stand for 2 hours to equilibrate.

[0132] S5.5. The concentrated liquid after backfilling is retested by HS-SPME-GC-MS method. The overall compliance rate R and the compliance rate of individual markers are recalculated to see if they are both within the range of 0.98-1.02 set in this embodiment. If they are both within the set range, the aroma backfilling is completed. If one or more markers are not within the set range, the aroma backfilling continues.

[0133] Table 9: Compliance Rate of Each Marker After Aroma Refilling

[0134]

[0135] As shown in Table 9, the overall compliance rate is:

[0136] R=(100.6% + 100.4% + 100.0% + 100.0% + 100.6% + 100.0% + 100.0% +100.0% + 100.3%)÷9= 100.2%

[0137] At this point, R = 100.2% is within the range of 98%-102%, and the compliance rate of all markers is within the range of 98%-102%, indicating that the aroma refill meets the standards.

[0138] It is worth noting that the osmanthus concentrate in step 4 is obtained by mixing the osmanthus aroma component extract and the flavor component extract extracted in step 2. Therefore, in addition to containing the osmanthus aroma markers in the osmanthus aroma component extract, it should also contain the residual osmanthus aroma markers in the flavor component extract, thus affecting the actual dilution ratio of the osmanthus aroma component extract. However, after the aroma replenishment liquid obtained in step 5.1 is backfilled into the concentrate in step 4, as shown in Table 9, the components of each aroma marker in the osmanthus concentrate after aroma backfilling are all in a qualified state. Therefore, it can be concluded that the content of each osmanthus aroma marker in the osmanthus flavor component extract is very small and will not affect the calculation of the dilution ratio of the osmanthus aroma component extract after subsequent concentration. Therefore, in this embodiment, it is not necessary to consider the influence of the osmanthus flavor component extract on the dilution ratio of the osmanthus aroma component extract in the secondary collection bottle during aroma backfilling.

[0139] Step 6: After the osmanthus concentrate with the aroma backfill meets the standard, heat it to 88°C using a plate heater, keep it at that temperature for 20 seconds, cool it to 30°C, and then fill it into bottles. This will produce a high-aroma osmanthus concentrate product with a uniform aroma and flavor, which can be used to prepare beverages.

[0140] It is worth noting that in this embodiment, the types and origins of the osmanthus raw materials and enzyme preparations are shown in Table 10:

[0141]

[0142] Example 2

[0143] Following the methods in steps 1-6 of Example 1 above, a batch of secondary osmanthus concentrate (aroma standard grade) with satisfactory aroma backfilling was prepared as the aroma blending base liquid for beverage wine.

[0144] It is worth noting that in the preparation of traditional alcoholic beverages (baijiu base liquor), the general safe ratio of aroma concentrate added to the alcoholic beverage is 0.05%-0.25%. Therefore, the aroma blending base liquor added per liter of baijiu base liquor should be in the range of 0.5mL-2.5mL. In this embodiment, the amount of secondary osmanthus concentrate added is set to 1.5mL / L.

[0145] Raw material ratio: 500L of light-aroma baijiu (52% vol); 0.75L of secondary osmanthus concentrate.

[0146] In this embodiment, the steps for preparing the beverage wine using high-quality osmanthus flower concentrate are as follows:

[0147] In a stainless steel blending tank (equipped with a stirrer and metering pump) with an effective volume of at least 600L, first pump in 500L of light-aroma baijiu base liquor, turn on the stirrer at 60rpm, and pump 0.75L of osmanthus concentrate into the blending tank at a rate of 0.1L / min through the metering pump. After the pumping is complete, continue stirring for 30 minutes to ensure that the osmanthus concentrate and base liquor are fully mixed. After stirring is stopped, let it stand for 12 hours to allow the aroma molecules to fully combine with the liquor, and the finished light-aroma baijiu with standard osmanthus aroma is obtained.

[0148] The above are merely preferred embodiments of the present invention and are not intended to limit the present invention. Various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A method for preparing a high-fragrance osmanthus concentrate suitable for alcoholic beverages, characterized in that, Includes the following steps: Step 1: Vacuum dry the fresh osmanthus flowers at a temperature not exceeding 40℃. Step 2: The dried osmanthus flowers are subjected to low-temperature extraction and enzymatic hydrolysis with water extraction to extract the aroma components and flavor components of osmanthus flowers, respectively. Step 2.1: Extract the aroma components of dried osmanthus flowers using supercritical CO2 fluid extraction to obtain an extract and deodorized osmanthus flower residue. The extraction temperature should not exceed 45℃. Step 2.2: Add the deodorized osmanthus residue to the compound enzyme solution and perform a three-stage gradient temperature extraction to obtain an extract of osmanthus flavor components; In step 2.2, the complex enzyme includes pectinase, cellulase, and protease; Step 3: Mix the osmanthus aroma component extract and the osmanthus flavor component extract from Step 2, and then perform low-temperature aging, centrifugation, coarse filtration through a ceramic membrane, and fine filtration through an ultrafiltration membrane to obtain a clear liquid. Step 4: Use a reverse osmosis membrane to filter out the water from the clarified liquid to obtain osmanthus concentrate; Step 5: Detect the aroma markers of osmanthus in the concentrate from Step 4 using the HS-SPME-GC-MS method to identify at least 9 characteristic aroma markers and their measured contents. Compare these contents with the set standard target contents for each marker. For aroma markers whose measured contents do not match the standard contents, perform aroma backfilling. When the overall compliance rate and the compliance rate of each aroma marker are within the set value range, the osmanthus concentrate preparation is complete. Step 6: After sterilizing the concentrated solution prepared in Step 5 at high temperature, cold fill the solution.

2. The method for preparing a high-fragrance osmanthus concentrate suitable for alcoholic beverages according to claim 1, characterized in that, The three-stage gradient temperature extraction process is as follows: The first stage temperature is set at 40℃, and the temperature is kept constant for 1 hour. The second stage sets the temperature to be increased from 40℃ to 55℃ at a heating rate of 1℃ / min, and then kept at a constant temperature for 2 hours. The third setting gradually increases the temperature from 55℃ to 70℃ at a rate of 1℃ / min, and then holds the temperature at that temperature for half an hour.

3. The method for preparing a high-fragrance osmanthus concentrate suitable for alcoholic beverages according to claim 1, characterized in that, The nine characteristic aroma markers in osmanthus include β-linalool, β-ionone, α-ionone, γ-decanoic acid lactone, cis-linalool oxide, trans-linalool oxide, cis-ocimene, 4-hexenyl acetate, and dihydro-β-ionone.

4. The method for preparing a high-fragrance osmanthus concentrate suitable for alcoholic beverages according to claim 1, characterized in that, In step 5, at least 10 batches of fresh osmanthus samples are taken, and osmanthus concentrate is prepared according to the methods described in steps 1 to 4. The content of 9 characteristic aroma markers in osmanthus is detected by HS-SPME-GC-MS method for each batch of osmanthus concentrate. The arithmetic mean of the content determination results of at least 10 batches is used as the standard target content of the 9 characteristic aroma markers in osmanthus.

5. The method for preparing a high-fragrance osmanthus concentrate suitable for alcoholic beverages according to claim 1, characterized in that, The aroma refilling steps are as follows: S5.1 Calculate the weight of the aroma markers that need to be added to the osmanthus concentrate obtained in step 4, and then convert it into the mass of the aroma supplement liquid. S5.2 Stir the osmanthus concentrate at low speed in a sealed environment at room temperature; S5.

3. Inject the aroma replenishing solution into the osmanthus concentrate at a rate of 0.5 mL / min; S5.4 After the aroma replenishment solution is injected, continue stirring for 15 minutes, and then let it stand for 2 hours to equilibrate. S5.

5. The osmanthus concentrate after backfilling is retested using the HS-SPME-GC-MS method. The overall compliance rate and the compliance rate of individual markers are recalculated to see if they are both within the set range. If both the overall compliance rate and the compliance rate of individual markers are within the set range, the aroma backfilling is considered complete. If one or more markers are not within the set range, the aroma backfilling step is repeated. In step S5.5, the numerical range for the overall compliance rate and the compliance rate of a single marker is set to 0.98-1.

02.

6. The method for preparing a high-fragrance osmanthus concentrate suitable for alcoholic beverages according to claim 1, characterized in that, In step 1, the drying time for fresh osmanthus flowers ranges from 4 to 6 hours. The moisture content of the osmanthus raw material is checked every hour. When the moisture content of the fresh osmanthus flowers is not higher than 8%, the vacuum drying is completed.

7. The method for preparing a high-aroma osmanthus concentrate suitable for alcoholic beverages according to claim 1, characterized in that, In step 3: The low-temperature aging process involves placing the mixture in a cold settling tank and letting it stand at 2°C for 18 hours. The centrifugation process involves aspirating the supernatant formed during settling and centrifuging it in a disc centrifuge. The ceramic membrane coarse filtration process involves passing the centrifuged supernatant through a ceramic membrane with a pore size of 0.1 μm for coarse filtration. The ultrafiltration membrane fine filtration process involves passing the supernatant after coarse filtration through an ultrafiltration membrane with a molecular weight cutoff of 20 kDa to obtain a clarified liquid.

8. The method for preparing a high-fragrance osmanthus concentrate suitable for alcoholic beverages according to claim 1, characterized in that, The ratio of pectinase, cellulase and protease added is 5:3:2.

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