Pine needle essence for beverages, method of preparation and pine needle flavored beverage
By capturing the volatile components released before pine needle distillation in a non-oxidizing atmosphere, and combining enzyme treatment and two-stage membrane separation technology, a pine needle flavor suitable for beverages was prepared. This solved the problems of loss of highly volatile components and uneven release of aroma in pine needle beverages, and achieved stable, phased release and persistence of aroma.
Patent Information
- Application Number
- CN202611163933.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2026-08-03
- Publication Date
- 2026-11-06
- Estimated Expiration
- 2046-08-03
AI Technical Summary
Existing pine needle beverage technology suffers from severe loss of highly volatile top aroma components during processing, alters aroma composition, and insufficient water dispersibility. As a result, the aroma release is uneven after the beverage is opened, making it difficult to maintain stability.
Volatile components released from pine needles before distillation are captured in a non-oxidizing atmosphere. After solvent desorption, enzyme treatment and steam distillation are performed. Monoterpenoid and oxygenated terpenoid aroma components are recovered through two-stage membrane separation. These components are then loaded onto food carriers with different release rates to prepare water-dispersible immediate-release and controlled-release base materials. The base material ratio is adjusted to match the dynamic release characteristics of the beverage matrix.
It reduces the loss of highly volatile components of pine needle flavoring in beverages, improves water dispersibility and the phased release characteristics of aroma, enhances the aroma layers and retention after opening, and reduces the impact of raw material batch and beverage matrix differences on aroma.
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Figure CN122664412B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of food flavoring and beverage processing technology, and particularly relates to a pine needle flavoring for beverages, a preparation method thereof, and a pine needle flavored beverage. Background Technology
[0002] Pine needles contain volatile components such as α-pinene, β-pinene, β-myrcene, limonene, borneol acetate, terpinene-4-ol, and α-terpineol. Among these, monoterpenes volatilize relatively quickly, primarily forming the fresh, top aroma of fresh pine needles; oxygenated terpenes volatilize relatively slowly, mainly forming the resinous, woody, and lingering aromas. Due to differences in the boiling point, water solubility, oxidative stability, and partition coefficients of different aroma components in beverage matrices, pine needles are prone to loss of low-boiling-point aroma components, insufficient recovery of oxygenated terpenes, and alterations in aroma composition during washing, crushing, heating extraction, distillation, sterilization, and storage. Adding pine needle essential oil directly to beverages may also result in insufficient water dispersibility, surface oil buildup, an overly strong initial odor, and rapid aroma decay after opening.
[0003] Chinese patent document CN103141893B discloses a pine needle beverage and its preparation method, using pine needles as the main raw material, combined with ingredients such as wolfberry, schisandra, red dates, honey, and white sugar. The preparation process includes soaking pine needles in water, heating to 95°C and maintaining for 45 minutes, followed by filtration, blending, hot filling, and sterilization at 121°C to obtain the pine needle beverage. This technology can directly introduce pine needle components into the beverage, but it mainly uses heating and decoction to extract pine needle substances. Highly volatile monoterpenoid components are prone to escape or oxidation during heating, heat preservation, and sterilization. At the same time, this technology does not separately recover pine needle essential oil, pine needle aromatic water, and the top aroma components released before distillation, nor does it address the control of independent pine needle flavoring for beverages, its water dispersibility, and the aroma release process after opening.
[0004] Chinese patent document CN106047499A discloses a method for extracting volatile oil from red pine needles, a forest air product, and its applications. The method involves obtaining red pine volatile oil through steam distillation and separating low-boiling-point and high-boiling-point volatile components using fractional distillation at different temperatures and vacuum distillation. Experimental results in this document show that low-boiling-point components are preferentially distilled out, while the number of high-boiling-point aromatic components increases with increasing distillation temperature. It also discloses that after the red pine volatile oil is re-released, it mainly retains volatile components such as α-pinene, camphene, limonene, β-pinene, and β-myrcene, while most high-boiling-point components are not released simultaneously. This technology demonstrates that different volatile components of pine needles have different distillation and release characteristics, but it is primarily geared towards forest air products and is not designed for food and beverage applications. Furthermore, it does not address the issues of food-grade recovery of aroma components from pine needle aromatic water, water dispersion of essential oils in acidic or sugary beverages, and the phased release of different aroma components after beverage opening.
[0005] Current pine needle beverage technologies typically focus on the water extraction, decoction, blending, or direct addition of pine needle essential oil to pine needle raw materials. The aroma quality of the resulting products is easily affected by the pine needle variety, harvest time, raw material storage conditions, and heat processing conditions. Static blending based solely on the total content of each aroma component in the flavoring is insufficient to reflect the actual aroma changes over different time periods after the beverage is opened. In the beverage matrix, pH, soluble solids content, emulsification system, and carbonation state all affect the rate at which volatile components migrate from the liquid phase to the headspace. Therefore, a static composition close to that of fresh pine needles does not necessarily mean that the beverage will maintain a similar pine needle aroma in the initial, middle, and later stages of release.
[0006] Therefore, it is necessary to provide a method for preparing pine needle flavoring suitable for beverages, which can reduce the loss of highly volatile top aroma components before distillation, while recovering monoterpenoids and oxygenated terpenoids from pine needle essential oil and pine needle aromatic water, and improving the water dispersibility of each aroma base in the beverage; it is also necessary to adjust the release order and blending ratio of different aroma bases according to the dynamic release characteristics of pine needle aroma in the target beverage matrix, so that the obtained pine needle flavoring can take into account the initial fresh aroma, the continuous main pine resin and the subsequent oxygenated terpenoid aroma after being added to the beverage, thereby improving the aroma layering, aroma retention after opening and batch stability of pine needle flavored beverages. Summary of the Invention
[0007] The technical objective of this invention is to provide a method for preparing pine needle flavoring for beverages, so as to reduce the loss of highly volatile top aroma components during pine needle processing, recover the characteristic aroma components of pine needle essential oil and pine needle aromatic water, improve the water dispersibility of pine needle flavoring in beverages, and make the phased aroma release characteristics of the beverage after opening close to those of fresh pine needles.
[0008] Firstly, in order to achieve the above-mentioned objectives, the present invention adopts the following technical solution:
[0009] A method for preparing pine needle flavoring for beverages, characterized by comprising the following steps:
[0010] S1. Place pine needles in a non-oxidizing atmosphere to capture the volatile components released by the pine needles before steam distillation, and desorb them using a solvent to obtain the top fragrance base.
[0011] S2. The pine needles that have completed the collection of volatile components are subjected to enzyme treatment and steam distillation. The distillation product is then separated into oil and water to obtain pine needle essential oil and pine needle aromatic water.
[0012] S3. The pine needle aromatic water is sequentially passed through a first membrane separation process that preferentially permeates monoterpenoid components and a second membrane separation process that preferentially permeates oxygenated terpenoid components. The permeate from the first membrane separation process is collected as a monoterpenoid concentrate, and the permeate from the second membrane separation process is collected as an oxygenated terpenoid concentrate. The monoterpenoid concentrate is mixed with pine needle essential oil to obtain the main fragrance base, and the oxygenated terpenoid concentrate is used as an oxygenated terpenoid fragrance base.
[0013] S4. Using a food-grade emulsifier, the top aroma base is made into a water-dispersible, fast-release emulsified base. The main aroma base is loaded onto a first food-grade water-dispersible carrier to obtain a first controlled-release base. The oxygen-containing terpene aroma base is encapsulated onto a second food-grade water-dispersible carrier to obtain a second controlled-release base.
[0014] S5. Mix the three base materials according to the mass ratio of water-dispersible immediate-release emulsifying base material, first controlled-release base material and second controlled-release base material of 8-18:52-62:25-35 to obtain pine needle flavoring for beverages.
[0015] As a further improvement, the pine needles are fresh pine needles from Pinus species with a clearly defined source and suitable for preparing natural flavorings for food; the monoterpenoid components include at least two of α-pinene, β-pinene, β-myrcene and limonene, and the oxygenated terpenoid components include at least two of borneol acetate, terpinene-4-ol and α-terpineol.
[0016] As a further improvement, in step S1, the non-oxidizing atmosphere is formed by one or both of nitrogen and carbon dioxide, and the oxygen volume content in the environment where the pine needles are located is not higher than 2% when capturing volatile components; the non-oxidizing gas carrying volatile components is passed through a hydrophobic porous adsorbent material for food contact, desorbed with food-grade ethanol, and the desorbed liquid is concentrated at a temperature not higher than 30°C to obtain the top fragrance base.
[0017] As a further improvement, in step S2, the enzyme treatment includes: cutting pine needles into segments of 5-15 mm in length, adding a food industry compound enzyme solution containing cellulase and pectinase, wherein the amount of the compound enzyme added is 0.20%-0.50% of the pine needle mass, alternating between vacuum treatment and atmospheric pressure treatment at 35-45°C for 2-4 cycles, and continuing enzymatic hydrolysis for 20-45 min; the vacuum degree in each cycle is -0.070 to -0.090 MPa, the vacuum treatment time is 3-6 min, and the atmospheric pressure treatment time is 3-8 min.
[0018] As a further improvement, in step S2, the steam distillation is carried out under reduced pressure, and the temperature of the distillate is 75-85°C. The ratio of the total corrected response value of monoterpene hydrocarbon components to the total corrected response value of oxygenated terpene components in the distillation product in the first 10 minutes is used as the initial reference ratio. Samples are taken at intervals during subsequent distillation. When the current ratio decreases to 30%-60% of the initial reference ratio and remains so for 3-10 minutes, the steam distillation is stopped.
[0019] As a further improvement, in step S3, the first membrane separation process uses a polydimethylsiloxane composite membrane for pervaporation separation, the first membrane separation temperature is 25-30℃, and the absolute pressure on the permeate side is 1.5-3.0 kPa; the retentate from the first membrane separation process is used as the feed for the second membrane separation process, the second membrane separation process uses a polyether block amide composite membrane for pervaporation separation, the second membrane separation temperature is 37-45℃, and the absolute pressure on the permeate side is 1.0-2.5 kPa; the permeates from the first membrane separation process and the second membrane separation process are condensed and collected at a temperature not higher than -15℃.
[0020] As a further improvement, in step S4, the food-grade emulsifier is selected from one or more of gum arabic, sodium octenyl succinate starch, and modified starch; the flavor base, food-grade emulsifier, and water are mixed, and an emulsion is formed by shear emulsification and high-pressure homogenization. The volume average particle size of the emulsion is 0.1 to 2.0 μm. The emulsion is used directly as a water-dispersible instant-release emulsifying base, or the emulsion is spray-dried to obtain a water-dispersible instant-release emulsifying base that redisperses upon contact with water.
[0021] As a further improvement, in step S4, the first food water-dispersible carrier is selected from one or more of porous starch, maltodextrin, gum arabic, and porous cellulose, and the mass ratio of the main flavor base to the first food water-dispersible carrier is 1:2 to 1:6; the second food water-dispersible carrier is selected from one or more of β-cyclodextrin, hydroxypropyl-β-cyclodextrin, and methyl-β-cyclodextrin, and the mass ratio of the oxygenated terpene flavor base to the second food water-dispersible carrier is 1:4 to 1:8; the time for the water-dispersible immediate-release emulsifying base, the first controlled-release base, and the second controlled-release base to reach their maximum release rate after being dispersed in the beverage is sequentially delayed.
[0022] Secondly, the present invention also provides a pine needle flavoring for beverages, comprising a water-dispersible immediate-release emulsifying base, a first controlled-release base, and a second controlled-release base; the water-dispersible immediate-release emulsifying base comprises volatile components released by pine needles in a non-oxidizing atmosphere before steam distillation and a food-grade emulsifier; the first controlled-release base comprises pine needle essential oil, a monoterpene hydrocarbon concentrate separated from pine needle aromatic water, and a first food-grade water-dispersible carrier loading both; the second controlled-release base comprises an oxygenated terpene concentrate separated from pine needle aromatic water and a second food-grade water-dispersible carrier encapsulating the oxygenated terpene concentrate; the mass ratio of the water-dispersible immediate-release emulsifying base, the first controlled-release base, and the second controlled-release base is 8–18:52–62:25–35.
[0023] Thirdly, the present invention also provides a pine needle flavored beverage, comprising a beverage base and the pine needle flavoring for beverages, wherein the pine needle flavoring for beverages has a mass content of 0.01% to 0.20% in the pine needle flavored beverage; the pine needle flavored beverage is a liquid preparation of a milk-containing beverage, a carbonated beverage, a flavored beverage, a plant-based beverage, a tea beverage, a fruit-flavored beverage, or a solid beverage.
[0024] This invention reduces the escape and oxidation of top aroma components such as α-pinene and β-pinene during raw material processing and heating by capturing highly volatile components released before pine needle distillation in a non-oxidizing atmosphere; it controls the steam distillation process based on the response relationship between monoterpenes and oxygenated terpenes to reduce aroma conversion caused by over-distillation; it performs two-stage selective membrane separation on the pine needle aromatic water to obtain monoterpenes and oxygenated terpenes concentrates, improving the overall recovery rate of pine needle aroma components; and it further prepares the top aroma base into a water-dispersible, fast-release emulsion base, and separates the main aroma base and oxygenated terpenes aroma base separately. By loading or encapsulating the three base materials onto food carriers with different release rates, the maximum release rate time of the three base materials in the beverage is shifted sequentially. The blending ratio of the three base materials is determined based on the reference release sequence in the corresponding model beverage matrix of the target beverage, thereby improving the dispersion stability of pine needle flavoring in acidic, sugary, or carbonated beverages, reducing floating oil and aroma bursts, and making the resulting beverage present a fresh top aroma, a continuous main pine aroma, and a lingering oxygenated terpene wood aroma after opening. It also reduces the impact of batch differences in raw materials and beverage matrix on the aroma of the finished product, and improves the aroma layering, aroma retention, and batch stability of pine needle flavored beverages. Attached Figure Description
[0025] Figure 1 This is a process flow diagram of the method for preparing pine needle flavoring for beverages according to the present invention.
[0026] Figure 2 This is a schematic diagram of the structure of the steam distillation apparatus for capturing volatile components before distillation according to the present invention.
[0027] Figure 3This is a schematic diagram of the two-stage selective membrane separation device for pine needle aromatic water according to the present invention.
[0028] Figure 4 This is a normalized release rate curve of the water-dispersible immediate-release emulsifying base, the first controlled-release base, and the second controlled-release base dispersed in a beverage in Example 1 of the present invention.
[0029] Figure 5 This is a comparison chart of the response distribution of characteristic aroma components of pine needles at different release times in the beverage after adding pine needle flavoring to the reference release sequence of the same batch of fresh pine needles in Example 1 of the present invention.
[0030] Figure 6 This is a comparison chart of the dynamic matching distance between Embodiment 1 of the present invention and various comparative examples at different release periods.
[0031] Figure 7 The figures show simulated thermal desorption GC-MS total ion chromatograms of the same batch of fresh pine needles at different release times in the model beverage matrix. Figure 7 (a) represents the data collection period from 0 to 10 minutes; Figure 7 (b) represents the data collection period of 20–40 minutes; Figure 7 (c) represents the collection period of 90–120 min; peaks 1–7 correspond to α-pinene, β-pinene, myrcene, limonene, 4-terpineol, α-terpineol, and bornyl acetate, respectively.
[0032] Explanation of reference numerals in the attached drawings: 1. Non-oxidizing gas source; 2. Pressure reducing valve; 3. Mass flow controller; 4. Oxygen content detector; 5. Sealed processing container; 6. Hydrophobic adsorption column; 7. Steam generator; 8. Distillation vessel; 9. Condenser; 10. Oil-water separator; 11. Pine needle essential oil collection container; 12. Pine needle aromatic water collection container; 13. First feed pump; 14. First heat exchanger; 15. First membrane module; 16. First condenser; 17. First vacuum pump; 18. Second feed pump; 19. Second heat exchanger; 20. Second membrane module; 21. Second condenser; 22. Second vacuum pump; 23. Monoterpene enrichment collection container; 24. Oxygenated terpene enrichment collection container. Detailed Implementation
[0033] The present invention will be further described below with reference to the accompanying drawings and specific embodiments. It should be understood that the listed embodiments are used to illustrate the technical solutions of the present invention and the technical effects they can achieve, and are not intended to limit the scope of protection of the present invention. Unless otherwise specified, all raw materials are raw materials that can be used in food processing. The pine needle raw materials, food-grade emulsifiers, food-grade carriers, food industry enzyme preparations, food-grade ethanol, and adsorption materials and membrane modules that come into contact with the materials should all meet the corresponding food safety requirements.
[0034] I. Terminology
[0035] (a) Pine needles for food use
[0036] The pine needle raw material for food use in this specific embodiment refers to fresh pine needles of the genus Pinus that are of clearly identified origin, free from mold and pests, and whose pesticide residues and heavy metal tests meet the requirements for food raw materials, and which have passed raw material safety review and can be used to prepare natural flavorings for food. Different pine needle varieties only affect the initial composition of characteristic aroma components and the proportion of each aroma base material, and do not change the basic process route of this invention.
[0037] (II) Characteristic aroma components of pine needles
[0038] In this specific embodiment, α-pinene, β-pinene, β-myrcene, limonene, borneol acetate, terpinene-4-ol, and α-terpineol were selected as characteristic aroma components of pine needles. Among them, α-pinene, β-pinene, β-myrcene, and limonene are classified as monoterpenes, while borneol acetate, terpinene-4-ol, and α-terpineol are classified as oxyterpenes.
[0039] (III) Model Beverage Base
[0040] A model beverage matrix refers to a matrix that is identical or substantially identical to the target beverage in terms of pH, soluble solids content, and carbonation state, but without the addition of pine needle flavoring. The model beverage matrix is used to establish a reference release sequence for the same batch of fresh pine needles and to determine the blending ratio of the immediate-release emulsifying base, the first controlled-release base, and the second controlled-release base. For other ingredients in the target beverage, if they significantly affect the liquid-gas distribution of aroma components, the corresponding ingredients of the same type and in the same amount are added to the model beverage matrix.
[0041] (iv) Reference release sequence
[0042] The reference release sequence refers to the sequence of corrected responses of each characteristic aroma component of pine needles measured at different time periods under the same conditions as the target beverage after opening: fresh pine needles from the same batch are placed in a model beverage matrix and the temperature, gas flow rate, and collection time are the same as those after opening the target beverage.
[0043] (v) Three aroma bases
[0044] The top aroma base refers to the volatile aroma components captured from the gas released from pine needles in a non-oxidizing atmosphere before steam distillation; the main aroma base refers to the aroma base formed by mixing pine needle essential oil with monoterpene hydrocarbon concentrates obtained in the first membrane separation process; and the oxygenated terpene aroma base refers to the oxygenated terpene concentrates obtained in the second membrane separation process.
[0045] II. Experimental Materials and Detection Methods
[0046] (a) Main materials and equipment
[0047] The main equipment used in the experiment included a dynamic headspace sampling device, a thermal desorption instrument, a gas chromatograph-mass spectrometer, a vacuum steam distillation device, an oil-water separator, a first membrane module, a second membrane module, a high-pressure homogenizer, a spray dryer, a freeze dryer, a laser particle size analyzer, a pH meter, a refractometer, a carbon dioxide content detector, and a constant temperature storage box.
[0048] The first and second membrane modules used in this embodiment were both purchased from Pervatech BV in the Netherlands, with module model FSTC-049 and an effective membrane area of 0.0089 m². 2 The first membrane module is filled with a flat-sheet PDMS organic preferential permeation composite membrane, and the second membrane module is filled with a flat-sheet PEBA organic preferential permeation composite membrane. The two membrane modules are installed independently and operated in series. The first membrane module uses a polydimethylsiloxane composite membrane with a separation layer thickness of 3–8 μm; the second membrane module uses a polyether block amide composite membrane with a separation layer thickness of 2–6 μm. Before use, the membrane modules are sequentially cleaned with food-grade ethanol and deionized water until no abnormal volatiles are detectable in the cleaning water.
[0049] The emulsifiers used in food processing include gum arabic, sodium octenyl succinate starch, or a mixture thereof; the water-dispersible carriers used in the first food processing include maltodextrin, gum arabic, porous starch, or porous cellulose; and the water-dispersible carriers used in the second food processing include β-cyclodextrin, hydroxypropyl-β-cyclodextrin, or methyl-β-cyclodextrin.
[0050] (ii) Reference release sequence detection method
[0051] Take 10.00g of fresh pine needles from the same batch, cut them into segments 5-10mm in length, add 100mL of model beverage matrix, place in a 250mL dynamic headspace sampling bottle, and equilibrate at 10±1℃ for 5min. For carbonated model beverage matrix, store it sealed before equilibration and maintain the same carbon dioxide content as the target beverage, and simulate opening when sampling begins.
[0052] Volatile components were continuously passed through the headspace of the sampling bottle at a gas flow rate of 100 mL / min, and collected at 0–10 min, 20–40 min, and 90–120 min. Thermal desorption tubes were used to collect the volatile components at different release time points, followed by GC-MS analysis. Figure 7 (As shown). To ensure consistent release conditions for fresh pine needles and pine needle essence, both were tested using the same model beverage matrix, sample volume, temperature, gas flow rate, and sampling time.
[0053] GC-MS was performed using a 30 m × 0.25 mm × 0.25 μm weakly polar capillary column; helium was used as the carrier gas at a flow rate of 1.0 mL / min; the initial column temperature was 40 °C, held for 3 min, then increased to 180 °C at 5 °C / min, and then increased to 240 °C at 10 °C / min, held for 5 min; the electron impact ion source had an electron energy of 70 eV and an ion source temperature of 230 °C, with a scan range of m / z 35–400. Characteristic aroma components of pine needles were identified using retention times of standards, retention indices, and mass spectrometry databases, and corrected using internal standards and relative response factors.
[0054] The corrected response percentage of the i-th characteristic aroma component of pine needles during the t-th release period is calculated according to the following formula:
[0055] ;
[0056] In the formula, The corrected response percentage of the i-th characteristic aroma component of pine needles during the t-th release period; The peak area of the aroma component after correction by internal standard and relative response factor; n is the number of selected characteristic aroma components of pine needles, which is 7 in this embodiment.
[0057] (III) Dynamic release detection of pine needle flavoring in beverages
[0058] Add pine needle flavoring to the model beverage matrix according to the set dosage, stir or shake until homogeneous, and then fill into 250mL beverage bottles, with each bottle containing 200mL of liquid. Equilibrate at 4℃ for 24h. During detection, raise the sample temperature to 10±1℃, start timing upon opening, and perform dynamic headspace sampling according to the same three release time periods as the reference release sequence.
[0059] The dynamic matching distance for the t-th release period is calculated using the following formula:
[0060] ;
[0061] In the formula, The dynamic matching distance for the t-th release period; The corrected response percentage of the i-th characteristic pine needle aroma component in the reference release sequence; This refers to the corrected response percentage of the corresponding components during the same release period after adding pine needle flavoring for beverages. A smaller dynamic matching distance indicates that the aroma composition during the corresponding release period is closer to that of fresh pine needles from the same batch. In this embodiment, a dynamic matching distance of no more than 0.20 for all three release periods is considered to meet the preset matching condition.
[0062] (iv) Release peak detection
[0063] The immediate-release emulsified base, the first controlled-release base, and the second controlled-release base were added to the model beverage matrix according to the same mass of aroma active ingredients. Volatile components were collected every 1 minute from 0 to 10 minutes, and every 2 minutes from 10 to 120 minutes. The total mass of the seven characteristic pine needle aroma components captured per unit time was used as the release amount, and the release rate was calculated based on the release amounts in adjacent time periods. The time corresponding to the maximum release rate was the time when the corresponding base reached its maximum release rate.
[0064] (v) Dispersion stability test
[0065] Add the pine needle flavoring to the target beverage according to the set amount, mix under the same stirring conditions for 2 minutes, and observe whether the flavoring forms visible oil droplets; fill the beverage into transparent glass bottles of the same diameter, and let it stand for 24 hours at 4℃ and 25℃ respectively, and measure the width of the oil ring on the liquid surface and the volume of the sediment at the bottom of the bottle; after gently shaking 10 times, observe whether the sediment can be redispersed.
[0066] (vi) Sensory evaluation
[0067] Twelve evaluators trained in pine needle aroma recognition conducted a blind taste test on the beverage at 10±1℃. Evaluation indicators included initial freshness, continuity of the main pine aroma, lingering aftertaste, off-flavors, and similarity to fresh pine needle aroma, each scored out of 9. Three parallel samples were prepared for each sample, and the average of all evaluation results was taken.
[0068] III. Examples and Comparative Examples
[0069] Example 1
[0070] This embodiment uses fresh pine needles of Pinus tabuliformis that have passed food ingredient review as raw material, and a non-carbonated flavored beverage as the target beverage.
[0071] (a) Model beverage matrix and reference release sequence
[0072] The model beverage matrix consisted of drinking water, white sugar, and citric acid, with a pH of 3.50, a soluble solids content of 8.0°Brix, and no carbon dioxide. Reference release sequences were established using the same batch of fresh pine needles following the aforementioned method; the results are shown in Table 1.
[0073] Table 1. Reference release sequence for Example 1
[0074]
[0075] As shown in Table 1, monoterpenoids were the main release components during the 0-10 min release period; the proportion of oxygenated terpenoids increased during the 20-40 min release period; and the combined response of borneol acetate, terpinene-4-ol, and α-terpineol accounted for 60% during the 90-120 min release period.
[0076] (ii) Collection of top aroma before distillation
[0077] Weigh 5.0 kg of fresh pine needles and place them in a container. Figure 2 In the sealed treatment container shown, the air inside the container was first replaced with nitrogen at a rate of 5 L / min for 10 min. When the oxygen volume content in the outlet gas decreased to 0.8%, the nitrogen flow rate was adjusted to 1.5 L / min, and the container was purged at 20°C for 30 min.
[0078] Nitrogen gas carrying volatile components of pine needles was passed through an adsorption column packed with a styrene-divinylbenzene type hydrophobic macroporous adsorbent material used in food processing. After purging, desorption was performed with food-grade ethanol, followed by concentration under reduced pressure below 25°C to obtain the topping aroma base. The oxygen volume content within the container was maintained between 0.5% and 1.1% during the collection process. The combined corrected response percentage of α-pinene, β-pinene, β-myrcene, and limonene in the topping aroma base was 83.6%.
[0079] (III) Enzyme treatment and steam distillation
[0080] The collected pine needles were cut into segments of 5–15 mm in length. A citrate buffer solution with a pH of 4.8 was added at 1.5 times the weight of the pine needles. A compound enzyme consisting of cellulase and pectinase in a mass ratio of 1:1 was added at 0.30% of the weight of the pine needles.
[0081] Vacuum treatment was performed at 40℃ and -0.080MPa for 5 minutes, followed by atmospheric pressure restoration and a 5-minute maintenance period. This cycle was repeated three times, and then enzymatic hydrolysis was continued at 40℃ for 30 minutes. After the enzyme treatment, the pine needles were transferred to a distillation vessel and subjected to reduced pressure steam distillation at -0.040MPa gauge pressure to maintain the material temperature at 78–84℃.
[0082] The ratio of the total corrected response value of monoterpenoid components to the total corrected response value of oxygenated terpenoid components in the distillation product over the previous 10 minutes was used as the initial reference ratio R0. In this example, R0 was measured to be 4.82. After distilling for 75 minutes, the ratio of the current ratio to the initial reference ratio decreased to 0.47; after continuing distillation for another 5 minutes, the ratio remained between 0.43 and 0.47, so distillation was stopped at 80 minutes. 23.6 g of pine needle essential oil and 3.82 kg of pine needle aromatic water were obtained by oil-water separation.
[0083] (iv) Two-stage selective membrane separation
[0084] The pine needle aromatic water was filtered through a 5μm filter material, according to... Figure 3 The process shown enters the first membrane module. The first membrane module uses a PDMS composite membrane with a membrane area of 0.20 m², a first membrane separation temperature of 28 °C, and an absolute pressure on the permeate side of 2.0 kPa; the permeate is condensed and collected at -20 °C to obtain monoterpene hydrocarbon enrichment.
[0085] The first membrane retentate was heated to 42°C and then entered the PEBA composite membrane module. The absolute pressure on the permeate side was 1.5 kPa. The second membrane permeate was condensed and collected at -25°C to obtain oxygen-containing terpene concentrate. The results of the two-stage membrane separation are shown in Table 2.
[0086] Table 2 Results of two-stage selective membrane separation in Example 1
[0087]
[0088] The monoterpene hydrocarbon concentrate obtained after concentrating the first membrane permeate was mixed with pine needle essential oil to obtain the main fragrance base; the oxygenated terpene concentrate obtained after concentrating the second membrane permeate was used as the oxygenated terpene fragrance base.
[0089] (v) Preparation of three water-dispersible base materials
[0090] Take 10 parts by weight of top fragrance base material, 20 parts by weight of sodium octenyl succinate starch, 10 parts by weight of gum arabic and 70 parts by weight of deionized water, shear at 10000 r / min for 3 min, and then homogenize for two cycles under primary pressure of 40 MPa and secondary pressure of 8 MPa to obtain an emulsion with an average particle size of 0.46 μm; spray dry under inlet air temperature of 90℃ and outlet air temperature of 48℃ to obtain an instant-release emulsion base material that can be rapidly redispersed in water.
[0091] Take 20 parts by weight of the main fragrance base material, 30 parts by weight of gum arabic, 50 parts by weight of maltodextrin and 200 parts by weight of deionized water, shear at 8000 r / min for 5 min, homogenize for two cycles at a first pressure of 30 MPa and a second pressure of 6 MPa, and then spray dry at an inlet air temperature of 115℃ and an outlet air temperature of 58℃ to obtain the first controlled-release base material.
[0092] Oxygenated terpene flavor base material and hydroxypropyl-β-cyclodextrin were mixed at a mass ratio of 1:6, and a 20% (w / w) food-grade ethanol aqueous solution was used as a solvent. The mixture was stirred at 40°C for 2 hours, and after removing the ethanol under reduced pressure, it was freeze-dried to obtain the second controlled-release base material.
[0093] Three base materials were added to the model beverage matrix for peak release detection. The immediate-release emulsified base material, the first controlled-release base material, and the second controlled-release base material reached their maximum release rates at 3 min, 38 min, and 84 min, respectively. The normalized release rate curves for the three materials are shown below. Figure 4 As shown, Figure 4 This indicates that the time for the three base materials to reach their maximum release rate shifts sequentially.
[0094] (vi) Dynamic matching and beverage preparation
[0095] Multiple rounds of blending tests were conducted on the three base materials based on the mass of aroma active substances contained in each base material. It was determined that when the mass ratio of aroma active substances in the immediate-release emulsified base material, the first controlled-release base material, and the second controlled-release base material was 12:58:30, the dynamic matching conditions were met in all three release periods.
[0096] The three base materials were mixed in a predetermined ratio to obtain powdered pine needle flavoring for beverages. This pine needle flavoring was added to the model beverage matrix at 0.05% of the beverage mass, stirred for 2 minutes, filled, and equilibrated at 4°C for 24 hours. Dynamic headspace analysis results are shown in Table 3.
[0097] Table 3 Aroma response distribution of pine needle flavored beverage in Example 1
[0098]
[0099] Based on Tables 1 and 3, the dynamic matching distances for the three release periods are 0.06, 0.04, and 0.04, respectively. Figure 5 The aroma response distribution of the beverage after the addition of pine needle flavoring is shown, with both exhibiting similar trends across the three release time periods.
[0100] Example 2
[0101] This embodiment uses fresh pine needles from red pine trees as raw material and a carbonated beverage as the target beverage. The pH of the model beverage matrix is 3.20, the soluble solids content is 10.0°Brix, and the carbon dioxide content is 3.0 g / L.
[0102] The air in the sealed treatment container was replaced with carbon dioxide. During the collection process, the oxygen volume content was maintained at 0.6%–1.2%, the collection temperature was 18℃, the carbon dioxide flow rate was 1.2 L / min, and the collection time was 35 min. The amount of compound enzyme added was 0.20% of the pine needle mass, and the mass ratio of cellulase to pectinase was 1:0.5. Two alternating cycles of vacuum and atmospheric pressure were performed at 35℃ and -0.075 MPa, followed by enzymatic hydrolysis for 40 min.
[0103] During steam distillation, R0 was measured to be 5.16. Distillation was stopped when the current ratio decreased to 60% of R0 and remained so for 3 minutes. The first membrane separation temperature was 25℃ and the absolute pressure on the permeate side was 2.5 kPa; the second membrane separation temperature was 37℃ and the absolute pressure on the permeate side was 1.8 kPa.
[0104] The immediate-release emulsifying base material is prepared from gum arabic and sodium octenyl succinate starch; the first controlled-release base material is prepared from gum arabic and maltodextrin; and the second controlled-release base material is prepared from β-cyclodextrin. The mass ratio of the three base materials is 15:55:30 based on the mass of the aroma active ingredients, and the amount of pine needle flavoring added is 0.08% of the beverage mass.
[0105] The test results showed that the immediate-release emulsion base, the first controlled-release base, and the second controlled-release base reached their maximum release rates at 4 min, 32 min, and 68 min, respectively; the dynamic matching distances for the three release periods were 0.08, 0.07, and 0.09, respectively.
[0106] Example 3
[0107] This embodiment uses fresh pine needles from Masson pine as raw material and a non-carbonated tea beverage as the target beverage. The model beverage matrix has a pH of 4.20, a soluble solids content of 5.0°Brix, and contains the same amount of tea extract as the target tea beverage.
[0108] Nitrogen gas was used for pre-distillation aroma collection, with an oxygen volume content of 0.4%–0.8% during the collection process. The amount of compound enzyme added was 0.50% of the pine needle mass, and the mass ratio of cellulase to pectinase was 1:2. Four alternating cycles of vacuum and atmospheric pressure were performed at 45℃ and -0.085MPa, followed by enzymatic hydrolysis for 25 min.
[0109] Steam distillation was stopped when the current ratio in the distillate decreased to 30% of R0 and remained so for 10 minutes. The first membrane separation temperature was 30℃, and the second membrane separation temperature was 45℃. The first controlled-release substrate was a carrier composed of porous starch and maltodextrin in a mass ratio of 1:2, and the second controlled-release substrate was methyl-β-cyclodextrin. The mass ratio of the three substrates was 10:60:30 based on the mass of the aroma active ingredients, and the amount of pine needle flavoring added was 0.04% of the beverage mass.
[0110] The test results showed that the three base materials reached their maximum release rates at 5 min, 48 min and 108 min, respectively; the dynamic matching distances for the three release periods were 0.09, 0.08 and 0.11, respectively.
[0111] Example 4
[0112] This embodiment uses fresh pine needles from the Chinese pine as raw material and a low-sugar plant-based beverage as the target beverage. The model beverage matrix has a pH of 3.80, a soluble solids content of 3.0°Brix, and is free of carbon dioxide.
[0113] The oxygen volume content during the pre-distillation trapping process was 1.0%–1.5%; the amount of compound enzyme added was 0.35% of the pine needle mass; the enzyme treatment temperature was 42℃; and three alternating cycles of vacuum and atmospheric pressure were performed; distillation was stopped when the current ratio in the distillation product decreased to 50% of R0 and remained so for 6 minutes.
[0114] The first membrane separation temperature is 27℃, and the second membrane separation temperature is 40℃. The first controlled-release base material is a carrier composed of porous cellulose, gum arabic, and maltodextrin, and the second controlled-release base material is hydroxypropyl-β-cyclodextrin. Based on the mass of aroma active ingredients, the mass ratio of the three base materials is 13:57:30, and the amount of pine needle flavoring added is 0.06% of the beverage mass.
[0115] The test results showed that the three base materials reached their maximum release rates at 3 min, 30 min and 74 min, respectively; the dynamic matching distances for the three release periods were 0.07, 0.09 and 0.10, respectively.
[0116] The main results of Examples 1 to 4 are shown in Table 4.
[0117] Table 4. Main detection results of different embodiments
[0118]
[0119] As shown in Table 4, under different pine needle raw materials, different beverage types, and different process parameters within the scope of the claims, the dynamic matching distance of the three release periods is no greater than 0.20, indicating that the present invention can be applied to different beverage bases.
[0120] Comparative Example 1
[0121] This comparative example was used to evaluate the effect of pre-distillation aroma capture. The same raw materials and processes as in Example 1 were used, but the pre-distillation aroma capture step was omitted, and pine needle oil of the same amount of aroma active substances was used instead of the aroma base. The resulting beverage had dynamic matching distances of 0.31, 0.12, and 0.10 at the three release periods. The total response percentage of the four monoterpenoids during the 0–10 min release period was lower than in Example 1, indicating that pine needle oil cannot completely replace the aroma components captured before distillation.
[0122] Comparative Example 2
[0123] This comparative example was used to evaluate the effect of pine needle aromatic water recovery. The same top aroma capture and steam distillation process as in Example 1 was used, but membrane separation of the pine needle aromatic water was not performed; only pine needle essential oil was used to prepare the main aroma base, and no oxygenated terpene aroma base was included. The resulting beverage had dynamic matching distances of 0.18, 0.24, and 0.46 at the three release time points, respectively. At 90–120 min, the total response proportion of oxygenated terpene components was only 38.5%, significantly lower than the 60.0% in the reference release sequence.
[0124] Comparative Example 3
[0125] This comparative example only performed the first membrane separation, preventing the first membrane retentate from entering the second membrane module. The permeate from the first membrane was mixed with pine needle essential oil to prepare the main fragrance base, without preparing oxygenated terpene fragrance base. The resulting beverage had dynamic matching distances of 0.12, 0.20, and 0.36 at the three release time points, and the total response proportion of oxygenated terpene components was 42.7% from 90 to 120 min.
[0126] Comparative Example 4
[0127] This comparative example was used to evaluate the effect of the carrier produced by the differentiated food. The same three aroma bases as in Example 1 were used, but both the main aroma base and the oxygenated terpene aroma base were spray-dried using the same carrier composed of gum arabic and maltodextrin. The first controlled-release base and the oxygenated terpene controlled-release base reached their maximum release rates at 37 min and 43 min, respectively, with a peak time difference of only 6 min. The dynamic matching distances of the resulting beverages at the three release periods were 0.14, 0.28, and 0.44, respectively.
[0128] Comparative Example 5
[0129] This comparative example uses the same three aroma bases and food carriers as in Example 1, but does not determine the blending ratio based on the reference release sequence of the three release periods. Instead, it is statically blended based on the cumulative response ratio of the seven characteristic aroma components of pine needles within 120 minutes.
[0130] The cumulative composition of the seven characteristic aroma components of pine needles in the obtained beverage was similar to that of the same batch of fresh pine needles. However, the dynamic matching distances at the three release periods were 0.08, 0.31 and 0.50, respectively, indicating that the similarity of the cumulative composition could not replace the dynamic matching at different time periods.
[0131] Comparative Example 6
[0132] This comparative example is used to evaluate the effect of adapting the model beverage matrix. The same red pine raw material and carbonated beverage as in Example 2 were used, but when determining the proportions of the three base materials, deionized water was used instead of the same carbonated model beverage matrix as the target beverage to establish a reference release sequence.
[0133] When the pine needle flavoring, determined based on the test results in deionized water, was added to the carbonated beverage of Example 2, the dynamic matching distances for the three release periods were 0.22, 0.25, and 0.33, respectively, influenced by acidity, sugar content, and carbon dioxide emission, all higher than those of Example 2. This indicates that determining the blending ratio in a model beverage matrix that matches the target beverage is beneficial in reducing the influence of beverage composition on aroma release.
[0134] Comparative Example 7
[0135] This comparative example is used to evaluate the effects of water-dispersible, fast-release emulsifying base material and food carrier. The top aroma base material, pine needle essential oil, monoterpene hydrocarbon concentrate, and oxygenated terpene concentrate obtained in Example 1 were directly mixed in the same proportion of aroma active ingredients without emulsification, carrier loading, or cyclodextrin inclusion, and then directly added to the model beverage matrix at 0.05% of the beverage mass.
[0136] After stirring for 2 minutes, visible oil droplets appeared on the surface of the beverage; after standing at 4℃ for 24 hours, an oil ring with an average width of 2.4 mm formed on the liquid surface. The dynamic matching distances for the three release periods were 0.26, 0.30, and 0.43, respectively. This indicates that directly adding pine needle aroma base to the beverage makes it difficult to achieve both water dispersibility and a phased release effect.
[0137] IV. Comprehensive Evaluation of Technical Effects
[0138] The dynamic matching results of Example 1 and each comparative example are shown in Table 5. Figure 6 The plot is based on the data in Table 5.
[0139] Table 5. Dynamic matching results between Example 1 and each comparative example.
[0140]
[0141] Depend on Figure 6 As shown in Table 5, pre-distillation aroma capture mainly reduces compositional deviation during the 0–10 min release period; two-stage membrane separation of pine needle aromatic water mainly reduces compositional deviation during the 90–120 min release period; and dynamic matching of carriers for differentiated foods and the matrix of the target beverage model can simultaneously reduce compositional deviation during the middle and later release periods.
[0142] The dispersion stability and sensory evaluation of Example 1 and some comparative examples were performed, and the results are shown in Table 6.
[0143] Table 6. Dispersion stability and sensory evaluation results
[0144]
[0145] Table 6 shows that the beverages prepared in Examples 1-4 did not form visible oil rings after standing at 4°C for 24 hours, and a small amount of sediment could be redispersed with slight shaking; Comparative Example 7, which did not use emulsifiers or food-grade carriers, showed obvious surface oil rings. The similarity of the aroma to fresh pine needles and the lingering aroma scores of Examples 1-4 were higher than those of the comparative examples.
[0146] V. Repeatability and Storage Stability Tests
[0147] Three independent batches of food-grade pine needles were used to prepare pine needle flavoring for beverages, following the method in Example 1. The proportions of the three base materials were determined for each batch based on its own reference release sequence. The results are shown in Table 7.
[0148] Table 7. Repeatability results for different raw material batches
[0149]
[0150] The overall recovery rate of aroma components in all three batches was higher than 84%, and the dynamic matching distance between the three release periods was no greater than 0.20. This indicates that establishing a reference release sequence based on the same batch of pine needles and adjusting the blending ratio of the three base materials can reduce the impact of batch differences in pine needle raw materials on the aroma of beverages.
[0151] The beverage prepared in Example 1 was sealed and stored in a light-proof environment with pine needle flavoring at 4°C and 25°C. The total retention rate of seven characteristic pine needle aroma components was measured at 0, 30, 60, and 90 days. The total retention rate after 90 days of storage at 4°C was 91.2%, and the total retention rate after 90 days of storage at 25°C was 86.4%. After the flavoring stored for 90 days was added to the model beverage matrix, the dynamic matching distances at the three release time points were 0.09, 0.08, and 0.10, respectively, still meeting the preset matching conditions.
[0152] In summary, this invention achieves uniform dispersion of pine needle flavoring in different beverage matrices through pre-distillation non-oxidative top aroma capture, aroma-response-controlled steam distillation, two-stage selective membrane separation of pine needle aromatic water, differentiated preparation of three types of food water-dispersible base materials, and time-segmented dynamic matching in the target beverage matrix. This results in the sequential formation of a fresh top aroma, a continuous main pine resin, and a subsequent oxygenated terpene aroma after the beverage is opened. Essentially the same dynamic aroma retention effect can be obtained under different pine needle raw materials and different beverage types.
Claims
1. A method for preparing a pine needle flavor for beverages, characterized by, Includes the following steps: S1. Place pine needles in a non-oxidizing atmosphere to capture the volatile components released by the pine needles before steam distillation, and desorb them using a solvent to obtain the top fragrance base. S2. The pine needles that have completed the collection of volatile components are subjected to enzyme treatment and steam distillation. The distillation product is then separated into oil and water to obtain pine needle essential oil and pine needle aromatic water. S3. The pine needle aromatic water is sequentially passed through a first membrane separation process that preferentially permeates monoterpenoid components and a second membrane separation process that preferentially permeates oxygenated terpenoid components. The permeate from the first membrane separation process is collected as a monoterpenoid concentrate, and the permeate from the second membrane separation process is collected as an oxygenated terpenoid concentrate. The monoterpenoid concentrate is mixed with pine needle essential oil to obtain the main fragrance base, and the oxygenated terpenoid concentrate is used as an oxygenated terpenoid fragrance base. S4. Using a food-grade emulsifier, the top aroma base is made into a water-dispersible, fast-release emulsified base. The main aroma base is loaded onto a first food-grade water-dispersible carrier to obtain a first controlled-release base. The oxygen-containing terpene aroma base is encapsulated onto a second food-grade water-dispersible carrier to obtain a second controlled-release base. S5. Mix the three base materials according to the mass ratio of water-dispersible immediate-release emulsifying base material, first controlled-release base material and second controlled-release base material of 8-18:52-62:25-35 to obtain pine needle flavoring for beverages. In step S1, the non-oxidizing gas carrying volatile components is passed through a hydrophobic porous adsorbent material for food contact, desorbed with food-grade ethanol, and the desorbed liquid is concentrated at a temperature not exceeding 30°C to obtain the top aroma base. In step S2, the enzyme treatment includes: cutting pine needles into segments of 5-15 mm in length, adding a food industry compound enzyme solution containing cellulase and pectinase, wherein the amount of the compound enzyme added is 0.20%-0.50% of the pine needle mass, alternating between vacuum treatment and atmospheric pressure treatment at 35-45°C for 2-4 cycles, and continuing enzymatic hydrolysis for 20-45 min; the vacuum degree in each cycle is -0.070 to -0.090 MPa, the vacuum treatment time is 3-6 min, and the atmospheric pressure treatment time is 3-8 min; In step S3, the first membrane separation process uses a polydimethylsiloxane composite membrane for pervaporation separation, the first membrane separation temperature is 25-30℃, and the absolute pressure on the permeate side is 1.5-3.0 kPa; the retentate from the first membrane separation process is used as the feed for the second membrane separation process, the second membrane separation process uses a polyether block amide composite membrane for pervaporation separation, the second membrane separation temperature is 37-45℃, and the absolute pressure on the permeate side is 1.0-2.5 kPa; In step S4, the food emulsifier is selected from one or more of gum arabic, sodium octenyl succinate starch, and modified starch; In step S4, the first food water dispersible carrier is selected from one or more of porous starch, maltodextrin, gum arabic, and porous cellulose, and the mass ratio of the main flavor base to the first food water dispersible carrier is 1:2 to 1:6; the second food water dispersible carrier is selected from one or more of β-cyclodextrin, hydroxypropyl-β-cyclodextrin, and methyl-β-cyclodextrin, and the mass ratio of the oxygenated terpene flavor base to the second food water dispersible carrier is 1:4 to 1:
8. In step S5, the mixing ratio of the three base materials is determined based on the reference release sequence in the matrix of the target beverage and dynamically matched according to time periods; the time it takes for the water-dispersible immediate-release emulsifying base material, the first controlled-release base material, and the second controlled-release base material to reach their maximum release rate after being dispersed in the beverage. The model beverage matrix refers to a matrix that is the same as or substantially the same as the target beverage in terms of pH, soluble solids content, and carbonation state, but without the addition of pine needle flavoring; the reference release sequence refers to the sequence of corrected responses of each characteristic aroma component of pine needles measured at different time intervals under the same conditions of temperature, gas flow rate, and collection time as the target beverage after opening, when fresh pine needles of the same batch are placed in the model beverage matrix.
2. The method for preparing pine needle flavoring for beverages according to claim 1, characterized in that, The pine needles are fresh pine needles from Pinus species with a clearly identified source and suitable for preparing natural flavorings for food; the monoterpenoid hydrocarbons include at least two of α-pinene, β-pinene, β-myrcene, and limonene, and the oxygenated terpenoids include at least two of borneol acetate, terpinene-4-ol, and α-terpineol.
3. The method for preparing pine needle flavoring for beverages according to claim 1, characterized in that, In step S1, the non-oxidizing atmosphere is formed by one or both of nitrogen and carbon dioxide, and the oxygen volume content in the environment where the pine needles are located does not exceed 2% when capturing volatile components.
4. The method for preparing pine needle flavoring for beverages according to claim 1, characterized in that, In step S2, the steam distillation is carried out under reduced pressure, and the temperature of the distillate is 75-85°C. The ratio of the total corrected response value of monoterpene hydrocarbon components to the total corrected response value of oxygenated terpene components in the distillation product in the first 10 minutes is used as the initial reference ratio. Samples are taken at intervals during subsequent distillation. When the current ratio decreases to 30%-60% of the initial reference ratio and remains so for 3-10 minutes, the steam distillation is stopped.
5. The method for preparing pine needle flavoring for beverages according to claim 1, characterized in that, The permeates from the first and second membrane separation processes are condensed and collected at a temperature not exceeding -15°C.
6. The method for preparing pine needle flavoring for beverages according to claim 1, characterized in that, A flavoring base, a food-grade emulsifier, and water are mixed and then sheared and homogenized under high pressure to form an emulsion. The volume average particle size of the emulsion is 0.1–2.0 μm. The emulsion is used directly as a water-dispersible, fast-release emulsifying base, or the emulsion is spray-dried to obtain a water-dispersible, fast-release emulsifying base that redisperses upon contact with water.
7. A pine needle flavoring for beverages, characterized in that, The pine needle flavoring is prepared by the method according to any one of claims 1-6; it comprises a water-dispersible immediate-release emulsifying base, a first controlled-release base, and a second controlled-release base; the water-dispersible immediate-release emulsifying base comprises volatile components released by pine needles in a non-oxidizing atmosphere before steam distillation and a food-grade emulsifier; the first controlled-release base comprises pine needle essential oil, a monoterpene hydrocarbon concentrate separated from pine needle aromatic water, and a first food-grade water-dispersible carrier loading both; the second controlled-release base comprises an oxygenated terpene concentrate separated from pine needle aromatic water and a second food-grade water-dispersible carrier encapsulating the oxygenated terpene concentrate; the mass ratio of the water-dispersible immediate-release emulsifying base, the first controlled-release base, and the second controlled-release base is 8-18:52-62:25-35.
8. A pine needle flavored beverage, characterized in that, The beverage includes a beverage base and the pine needle flavoring for beverages as described in claim 7, wherein the pine needle flavoring for beverages has a mass content of 0.01% to 0.20% in the pine needle flavored beverage; the pine needle flavored beverage is a liquid preparation of a milk-containing beverage, a carbonated beverage, a flavored beverage, a plant-based beverage, a tea beverage, a fruit-flavored beverage, or a solid beverage.
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