Supercritical co2 extraction method of wuyi rock tea aroma components and application of the extract

Abstract

The application discloses a supercritical CO2 extraction method of Wuyi rock tea aroma components and application of the extract. The process is aimed at light baking Wuyi rock tea, adopts supercritical CO2 extraction technology, takes anhydrous ethanol as a carrier, and efficiently enriches ester, alcohol and ketone aroma components in tea through optimization of extraction temperature, time, pressure and flow rate and other parameters. The application further discloses application of the obtained extract as a flavoring agent in preparation of perfume. Addition of the supercritical extract of Wuyi rock tea with a specific concentration to fresh perfume can significantly improve the floral, sweet and fresh properties of the perfume and improve the overall aroma quality. The process is green and environment-friendly, the obtained extract has pure aroma, and the application provides a new way for high-value utilization of Wuyi rock tea and development of natural spices.

Description

Technical Field

[0001] This invention belongs to the field of natural product extraction and daily chemical products technology, specifically involving a supercritical CO2 extraction process for aroma components of lightly roasted Wuyi rock tea, and the application of the extract in perfume enhancement. Background Technology

[0002] Wuyi Rock Tea, a prized variety of Chinese oolong tea, is highly sought after for its unique "rocky essence and floral aroma." The light roasting process, which maximizes the preservation of the high-boiling-point, long-lasting floral and fruity aroma components in the tea leaves, has become a mainstream trend in the market in recent years. However, how to apply this unique tea aroma to the daily chemical industry, especially as a natural fragrance in perfume preparation, has always been a challenge for those skilled in the art.

[0003] Currently, the extraction of aroma components from tea mainly relies on traditional steam distillation and organic solvent extraction. While steam distillation is a mature process, the high-temperature, long-duration treatment can easily cause oxidation, hydrolysis, or isomerization of heat-sensitive aromatic substances in tea (such as certain alcohols and esters), resulting in a distorted aroma that fails to capture the original fresh and elegant characteristics of lightly roasted Wuyi rock tea. Organic solvent extraction, on the other hand, often results in solvent residue and extracts containing numerous impurities, requiring complex subsequent purification steps, making it difficult to meet the stringent requirements of high-end perfumes for the purity and safety of raw materials.

[0004] Supercritical CO2 fluid extraction, as a green separation technology, has shown great potential in the extraction of natural products due to its advantages such as low critical temperature (31.06℃), good chemical inertness, and non-toxicity and residue-free operation. Although there are reports of supercritical technology being applied to the decaffeine removal and polyphenol extraction of tea, in the extraction of aroma from Wuyi rock tea, existing technologies usually directly apply the extraction parameters of Pu'er tea or green tea, ignoring the unique dense leaf structure and complex aroma component distribution of lightly roasted Wuyi rock tea.

[0005] Current technologies lack specific optimized supercritical CO2 extraction processes for the extraction of aroma components from lightly roasted Wuyi rock tea, resulting in low extraction efficiency and low yields of characteristic aroma components. Furthermore, existing technologies fail to recognize the unique role of Wuyi rock tea supercritical extracts in perfume enhancement, particularly their synergistic effect on enhancing floral and sweet aroma properties. Therefore, developing a supercritical CO2 extraction method specifically for the aroma components of lightly roasted Wuyi rock tea and innovatively applying it to the perfume enhancement field has significant market value and practical implications. Summary of the Invention

[0006] This invention aims to overcome the shortcomings of existing technologies by providing a supercritical CO2 extraction method for the aroma components of Wuyi rock tea. By optimizing extraction parameters, it achieves efficient enrichment and retention of floral and fruity aroma components in Wuyi rock tea. Another objective of this invention is to provide the application of the Wuyi rock tea supercritical extract prepared by the above method in perfume enhancement, solving the problems of existing perfumes having a single fragrance profile and lacking natural tea flavor. By adding this extract, the complexity and pleasantness of the perfume are significantly enhanced.

[0007] To achieve the above objectives, the present invention adopts the following technical solution:

[0008] In one embodiment, the present invention provides a supercritical CO2 extraction method for the aroma components of Wuyi rock tea, comprising the following steps: (1) Raw material pretreatment: lightly roasted Wuyi rock tea is pulverized and passed through a 20-mesh sieve; (2) Loading and system balancing: tea powder is loaded into the extraction vessel, and the temperature of separation vessel I is set to 45-50℃ and the pressure to 6-8 MPa, and the temperature of separation vessel II is set to 25-35℃ and the pressure to 4-6 MPa, and the system is allowed to stabilize; (3) Supercritical extraction: CO2 is used as the extractant, anhydrous ethanol is used as the entrainer, the extraction temperature is 45-55℃, the extraction pressure is 10-20 MPa, the extraction time is 40-60 min, the CO2 flow rate is 10-22 L / h, and the entrainer dosage is 140-160 mL / 150 g of raw tea powder; (4) Separation and concentration: after extraction, the oil phase extract is separated and collected, and the Wuyi rock tea aroma extract is obtained by vacuum concentration.

[0009] In another embodiment, the lightly roasted Wuyi rock tea of ​​the present invention is an oolong tea processed by a light roasting technique, and the variety is selected from at least one of Rougui, Qidan, Beidou, 105 Huang Guanyin or Shuixian.

[0010] In another embodiment, the entrainer of the present invention is anhydrous ethanol.

[0011] In another embodiment, the optimal extraction parameters of the present invention are: extraction temperature 50°C, extraction pressure 20 MPa, extraction time 58 min, CO2 flow rate 20 L / h, and entrainer anhydrous ethanol volume 150 mL.

[0012] In another embodiment, the aroma extract prepared by the present invention contains one or more of ionone, 3,5-octadien-2-one, damascene, linalool, geraniol, tea ketone, and indole.

[0013] In one embodiment, the present invention provides the application of the Wuyi rock tea aroma extract prepared by the method in perfume enhancement.

[0014] In another embodiment, the present invention adds Wuyi rock tea aroma extract as a natural fragrance enhancer to the perfume base, and obtains a fragrance-enhanced perfume after mixing, sonication, and light-proof standing equilibrium.

[0015] In another embodiment, the present invention uses the total mass of perfume as a basis and the amount of Wuyi rock tea aroma extract added is 0.05% to 2.00%.

[0016] In another embodiment, the optimal addition amount of the Wuyi rock tea aroma extract of the present invention is 0.40%.

[0017] In one embodiment, the present invention provides a method for enhancing the fragrance of a perfume, comprising taking the aroma extract of Wuyi rock tea prepared by the method of the present invention, adding it to a perfume base, and after mixing, sonicating, and equilibrating by standing in the dark, a perfume with the characteristic aroma of Wuyi rock tea is obtained.

[0018] Compared with the prior art, the present invention has the following significant advantages:

[0019] (1) This invention features high extraction efficiency and precise, controllable process parameters. This invention systematically optimized the supercritical CO2 extraction process for lightly roasted Wuyi rock tea through single-factor experiments combined with response surface methodology. The optimal process parameters were determined to be: extraction temperature 50℃, extraction pressure 20 MPa, CO2 flow rate 20 L / h, extraction time 58 min, and entrainer (anhydrous ethanol) dosage 150 mL. Under these optimized conditions, the extraction rate was stable and efficient, with the extraction rate of cinnamon reaching 1.04±0.02%. This process solves the problems of low extraction efficiency and high energy consumption caused by blindly setting parameters in traditional methods, and has good reproducibility and industrial application potential.

[0020] (2) This invention has a high aroma retention rate and effectively enriches characteristic aroma components. This invention uses low-temperature supercritical CO2 extraction technology, which effectively avoids the damage of heat-sensitive aroma components caused by high temperatures. Experimental data show that the aroma recovery rate of lightly roasted Wuyi rock tea by this process is between 40.83% and 54.01%.

[0021] (3) This invention has a significant fragrance-enhancing effect on perfumes, improving sensory quality. This invention is the first to apply supercritical extraction of Wuyi rock tea to the field of perfume enhancement, and has achieved excellent sensory enhancement effects. It can significantly enhance the floral, sweet, and fresh aroma properties of perfumes, improve the overall aroma quality, and does not mask the original base notes of the perfume. It also changes the distribution of volatile components in perfumes, introducing key aroma-active compounds with high rOAV values, such as ionone and linalool.

[0022] (4) This invention is green and environmentally friendly, and the product is highly safe. This invention uses CO2 as the extraction medium and anhydrous ethanol as the entrainer. CO2 is non-toxic, odorless, non-flammable, and recyclable, while ethanol is a food-grade solvent, avoiding the risk of solvent residue in traditional organic solvent extraction methods. The resulting extract is pure and natural, meeting the stringent requirements of modern cosmetics and daily chemical products for the safety and greenness of raw materials, and has extremely high commercial development value. Attached Figure Description

[0023] Figure 1 The effect of extraction temperature on the extraction rate of Wuyi rock tea.

[0024] Figure 2 The effect of extraction pressure on the extraction rate of Wuyi rock tea.

[0025] Figure 3 The effect of extraction time on the extraction rate of Wuyi rock tea.

[0026] Figure 4 The effect of CO2 flow rate on the extraction rate of Wuyi rock tea.

[0027] Figure 5 The effect of entrainer dosage on the extraction rate of Wuyi rock tea.

[0028] Figure 6 A, B, and C represent the response surfaces of the interaction between extraction temperature, extraction time, and entrainer dosage on the extraction rate of Wuyi rock tea, respectively; D, E, and F represent the contour lines of the interaction between extraction temperature, extraction time, and entrainer dosage on the extraction rate of Wuyi rock tea, respectively.

[0029] Figure 7 This is a radar image of an electronic nose.

[0030] Figure 8 Analysis of volatile compounds in extracts of five varieties of Wuyi rock tea. A shows the quantity and proportion of different types of volatile compounds in the extracts; B shows the total relative content of volatile compounds in different extracts; C shows the relative content of different types of volatile compounds in the extracts; D shows the Venn diagram of volatile compounds in the extracts.

[0031] Figure 9 Screening of differentially volatile compounds in extracts of five varieties of Wuyi rock tea. A is the principal component analysis score plot; B is the partial least squares discriminant analysis (PLS-DA) model score plot; C is the results of 200 permutation tests; D is the heatmap of 64 differentially volatile compounds (P<0.05 and VIP>1).

[0032] Figure 10 Heatmaps of key aroma components from different Wuyi rock tea extracts.

[0033] Figure 11 This is a flavor profile of key aroma active substances in Wuyi rock tea extracts.

[0034] Figure 12 Key aroma active components that interact with olfactory receptors (ORs): A is the interaction between coumarin and OR1A1; B is the interaction between E-nerolidol and OR1A1; C is the interaction between coumarin and OR1D2; D is the interaction between caryophyllin and OR1D2; E is the interaction between jasmine lactone and OR1A1; F is the interaction between β-cyclic citral and OR1A1; G is the interaction between jasmone and OR1A1; H is the interaction between β-cyclic citral and OR1D2.

[0035] Figure 13 Quantitative descriptive analysis of the flavor enhancement potential of extracts.

[0036] Figure 14 Flavor enhancement potential analysis for RG-E: A represents the number of volatile compounds in 0.04% RG-E and CK; B represents the relative content of volatile compounds; C represents the relative proportion of volatile compounds; D represents principal component analysis; E represents OPLS-DA analysis; F represents the substitution test; G represents the heatmap of differentially volatile substances; H represents the flavor wheel of key aroma components with rOAV > 1. Detailed Implementation

[0037] The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments. These embodiments are for illustrative purposes only and are not intended to limit the scope of the invention. Unless otherwise specified, the experimental methods used in the following embodiments are conventional methods; the materials and reagents used are commercially available unless otherwise specified; and the experimental conditions are conventional conditions in the art.

[0038] Example 1: Supercritical CO2 extraction of tea aroma components and determination of optimal extraction parameters

[0039] (1) Table 1 lists the materials and reagents required for this embodiment, and Table 2 lists the experimental instruments and equipment:

[0040] Table 1 Experimental Materials and Reagents

[0041] ,

[0042] Table 2 Experimental Instruments and Equipment

[0043] ,

[0044] (2) Raw material pretreatment: Lightly roasted Wuyi rock tea cinnamon was used as the experimental material, and extraction was performed using a HA220-50-06 type supercritical CO2 extraction device. Before the experiment, the tea leaves were pulverized and passed through a 20-mesh sieve. 150g of the sieved tea powder was weighed and placed into a 1 L extraction vessel for extraction using extraction vessel II. When starting the equipment, the main power supply, extraction vessel II, separation vessel I, and the temperature control switches of separation vessel II were turned on in sequence, and the CO2 cylinder was opened. After the temperature reached the set value, the valves were opened in sequence, and the pressure was adjusted to the target parameters. The temperature and pressure of separation vessel I and separation vessel II were kept constant: separation vessel I was 48 ℃ and 8 MPa; separation vessel II was 30 ℃ and 6 MPa. After the CO2 flow rate stabilized, the entrainer pump was started, and anhydrous ethanol was used as the entrainer for extraction. After extraction, the Wuyi rock tea extract was collected from separation vessel b1 and separation vessel b2, respectively. After being concentrated by rotary evaporation, the extract was weighed, and the yield was calculated according to the following formula:

[0045] ;

[0046] In the formula: y, yield, %; m1, mass of Wuyi rock tea extract, g; m2, mass of Wuyi rock tea sample, g.

[0047] To evaluate the influence of key process parameters on the extraction rate of Wuyi rock tea, a single-factor experiment combined with analysis of variance was used. Based on preliminary experiments and literature reports, the extraction rate was used as the response index. Entrainers are an important auxiliary means to improve the extraction efficiency of supercritical CO2 fluid, and their volatility is usually between that of the target component and the supercritical fluid. The mechanism of entrainers is, on the one hand, to regulate their solubility characteristics by changing the density of CO2 fluid; on the other hand, it depends on the interaction between molecules to enhance the affinity and selectivity of the fluid for specific target components

[149] . Therefore, the choice of entrainer dosage also has a significant impact on the extraction rate. Under fixed conditions: extraction pressure 15 MPa, extraction temperature 50 ℃, extraction time 1 h, entrainer dosage 200 mL, CO2 flow rate 10 L / h, the effects of changes in extraction temperature, extraction time, extraction pressure, CO2 flow rate and entrainer dosage on the supercritical extraction rate were systematically studied. The specific test range is shown in Table 3:

[0048] Table 3 Single-factor experimental design

[0049] ,

[0050] Response surface methodology commonly employs two experimental design methods: Box-Behnken Design (BBD) and Central Composite Design (CCD). Box-Behnken Design (BBD) is suitable for process optimization involving 2 to 5 factors, offering advantages such as fewer experiments, optimal process parameters obtainable within the maximum range set in the experiment, and a safe and controllable experimental process. Therefore, based on the suitable levels of each factor obtained from single-factor experiments, this experiment used a BBD design to create a process for optimizing the supercritical CO2 extraction of Wuyi Rock Tea Rougui, with extraction temperature, extraction time, and entrainer dosage as independent variables and the extraction rate of Wuyi Rock Tea Rougui as the response value. Ten verification experiments were then conducted using Rougui, Qidan, Beidou, 105 Huang Guanyin, and Shui Xian under the optimal process conditions.

[0051] The data was organized using Excel 2021, the response surface data was analyzed using Design-Expert 13, and the graphs were drawn using GraphPad Prism.

[0052] (3) Results: Based on the CO2 critical temperature of 31.06℃, five levels of 35, 40, 45, 50, and 55℃ were set to investigate the effect of extraction temperature on the extraction rate of Wuyi rock tea. Figure 1 As shown, the extraction rate initially increases and then decreases with increasing temperature. It rises continuously within the range of 35℃ to 50℃, reaching a peak at 50℃; above 50℃, the extraction rate declines. This trend reflects the bidirectional regulatory effect of temperature on supercritical extraction efficiency. On the one hand, increased temperature promotes the thermal motion of CO2 molecules, enhancing their diffusion coefficient and mass transfer rate within the tea leaves, increasing the probability of contact with target components, and simultaneously increasing the vapor pressure of extractable components, which facilitates the migration of solutes from the matrix to the fluid phase, thereby improving extraction efficiency. On the other hand, excessively high temperatures lead to a significant decrease in CO2 density, weakening its ability to dissolve solutes; simultaneously, excessive heat input may induce the degradation or structural transformation of heat-sensitive aroma components in tea leaves, affecting not only the extraction rate but also potentially damaging the sensory quality of the extract. Considering these factors, 50℃ was selected as the optimal extraction temperature for this experiment, ensuring a high extraction rate while avoiding the loss of active ingredients due to excessively high temperatures.

[0053] This invention investigated the effects of five pressure levels (10, 15, 20, 25, and 30 MPa) on the extraction rate of Wuyi rock tea. The results are as follows: Figure 2As shown, the extraction rate initially increases and then decreases with increasing pressure. Within the 10–20 MPa range, the extraction rate is positively correlated with pressure, continuously increasing with rising pressure, reaching a peak at 20 MPa. This is because in the initial stage of pressure increase (10–20 MPa), the CO2 fluid density increases significantly with increasing pressure, enhancing the solubility effect and increasing the solubility of effective components in tea leaves in CO2, thus promoting extraction efficiency. When the extraction pressure exceeds 20 MPa, the extraction rate decreases significantly. This is because excessively high pressure reduces the compressibility of the CO2 fluid, causing the density increase to plateau, limiting the potential for further improvement in solubility, and making it difficult to further increase solute dissolution efficiency. Furthermore, excessively high pressure causes tea powder particles to be compressed and shrink, increasing bulk density, leading to a reduction in the effective contact area between the tea powder and the CO2 fluid, increasing mass transfer resistance, and thus hindering the extraction process. Therefore, considering multiple factors such as extraction efficiency and production safety, 20 MPa was determined as the optimal extraction pressure for this experiment, used for subsequent process optimization and sample preparation.

[0054] This invention also investigated the variation of Wuyi rock tea extraction rate under different extraction times, and the results are as follows: Figure 3 As shown in the experimental results, the extraction rate initially increases and then decreases with increasing extraction time, reaching a peak at 60 min. In the initial stage of extraction, the extraction rate is low and increases with time. This is because supercritical extraction is a dynamic mass transfer process. In the initial stage, the material has not yet fully contacted the CO2 fluid. However, as the contact time increases, the CO2 fluid continuously penetrates into the tea leaves, and the solute's dissolution in the fluid gradually reaches equilibrium, thus increasing the mass transfer efficiency and leading to a continuous increase in the extraction rate. After 60 min, the extraction rate begins to decrease. Based on the above analysis, 60 min is determined to be the optimal extraction time for this experiment, under which a high extraction rate can be obtained.

[0055] This invention investigated the effect of different CO2 flow rates on the extraction rate of Wuyi rock tea, and the results are as follows: Figure 4 As shown, the extraction rate initially increases and then decreases with increasing CO2 flow rate. When the CO2 flow rate increases from 10 L / h to 20 L / h, the extraction rate continues to rise, reaching a peak at 20 L / h; however, once the CO2 flow rate exceeds 20 L / h, the extraction rate gradually decreases. In the initial stage of increasing CO2 flow rate, the increase in extraction rate is mainly due to improved mass transfer efficiency. As the flow rate increases, the velocity of the fluid through the material layer accelerates, enhancing the stirring contact between the fluid and the tea particles, thereby improving mass transfer efficiency and promoting an increase in extraction rate. Once the flow rate exceeds 20 L / h, the extraction rate begins to decline. Therefore, based on the above analysis, 20 L / h is selected as the optimal CO2 flow rate.

[0056] This invention investigated the effect of different entrainer dosages on the extraction rate of Wuyi rock tea, and the results are as follows: Figure 5 As shown, the extraction rate initially increases and then decreases with increasing entrainer dosage, reaching its maximum at a dosage of 150 mL. When the entrainer dosage is below 150 mL, the extraction rate increases sharply with increasing entrainer dosage. This is because the addition of an appropriate amount of entrainer can effectively enhance the polarity of the supercritical CO2 fluid, improving its solubility for the target components. Simultaneously, the entrainer molecules can competitively bind with the target components in the tea matrix, disrupting the adsorption forces between them and the raw material matrix, thereby promoting the migration of the solute from the solid phase to the fluid phase and significantly improving the extraction efficiency. When the entrainer dosage exceeds 150 mL, the extraction rate decreases. This may be because excessive entrainer forms a continuous liquid film on the surface of the tea particles, creating a physical barrier on the material surface, significantly increasing the mass transfer resistance of the target components diffusing from the solid phase to the supercritical fluid, hindering sufficient contact between CO2 and the target. Furthermore, the addition of excessive entrainer leads to a liquid extraction environment, which is not conducive to further extraction. Therefore, 150 mL is selected as the optimal entrainer dosage.

[0057] Single-factor experiments showed that the effects of extraction temperature, extraction time, and entrainer dosage on the extraction rate all exhibited a trend of first increasing and then decreasing. The extraction rates at 50℃ (e.g., ...) were... Figure 1 As shown), 60 min (as shown) Figure 3 (as shown) and the amount of entrainer used is 150 mL (e.g.) Figure 5 The optimal values ​​were reached at (as shown in the figure). All three factors exhibited typical unimodal response characteristics, and the differences between each optimal level and its neighboring levels were statistically significant. In contrast, the effects of extraction pressure in the range of 15–20 MPa and CO2 flow rate in the range of 10–20 L / h on the extraction rate were not significant, but the extraction rate was optimal at 20 MPa and 20 L / h, respectively (as shown in the figure). Figure 2 , Figure 4(As shown). Therefore, to simplify the experimental scale and focus on the more significant factors, extraction temperature, extraction time, and entrainer dosage were selected as the three factors for response surface optimization. Pressure and CO2 flow rate were fixed at the optimal level and were not used as response surface optimization factors. A Box-Behnken design (BBD) was adopted, with extraction temperature, extraction time, and entrainer dosage as independent variables and the extraction rate of Wuyi rock tea cinnamon as the response value, to optimize the process conditions. After obtaining the optimal process conditions, 10 verification experiments were conducted on five varieties—cinnamon, Qidan, Beidou, 105 Huang Guanyin, and Shuixian—under the optimal conditions. The experimental design and results are shown in Table 4. Multiple regression analysis was performed on the experimental results (Table 4), and regression fitting was carried out on each factor to obtain the regression equation: Y=1.04-0.0189A-0.0215B+0.0313C+0.0449AB+0.0239AC+0.0490BC-0.2505A 2 -0.1435B 2 -0.1989C 2 Where Y is the supercritical extraction rate of Wuyi rock tea, A is the extraction temperature, B is the extraction time, and C is the amount of entrainer. The model variance analysis is shown in Table 5.

[0058] Table 4 Results of supercritical extraction response surface methodology for Wuyi rock tea

[0059] ,

[0060] As shown in Table 5, the F-value of the regression model is 71.22, the P-value is <0.0001, and the coefficient of determination R is [missing value]. 2 =0.9828, R adj =0.9753, indicating that the established quadratic equation has high significance, and the model can effectively characterize the relationship between various process parameters and extraction yield. The coefficient of variation (CV) is 4.07% < 5%, indicating good repeatability of the experimental model. The lack-of-fit term value is 0.1282 (P > 0.05), which is not significant, indicating small experimental error. This shows that the equation has good accuracy and reliability and can be used for theoretical prediction of supercritical extraction experiments of Wuyi rock tea. According to the F and P values, the influence of the three factors on the extraction rate of Wuyi rock tea is in the following order: entrainer addition amount (C) > extraction time (B) > extraction temperature (A).

[0061] Table 5. Analysis of Variance for Response Surface Regression Model

[0062] ,

[0063] To determine the interaction of extraction temperature, extraction time, and entrainer dosage on the extraction rate of Wuyi rock tea, response surfaces and contour plots (such as...) were drawn based on the equations. Figure 6(As shown). The 3D response surface plot and contour plot can visually reflect the significance of the interaction of various factors on the extraction rate of Wuyi rock tea. The greater the curvature and the steeper the slope of the 3D response surface plot, the more significant the interaction of the two factors has on the extraction rate. Figure 6 As shown in Figures A and D, the 3D response surface curves have a steep slope, dense contour lines, and an elliptical shape, indicating a significant interaction between extraction temperature (A) and extraction time (B). Figure 6 B and E represent the interaction between extraction time (B) and entrainer dosage (C). Their 3D response surface curves are steep, with dense contour lines and an approximately elliptical shape, indicating a significant interaction between B and C. Figure 6 In the equations C and F, the interaction between extraction temperature (A) and entrainer dosage (C) is shown. Their 3D response surface curves are relatively smooth with sparse contour lines and a near-circular shape, indicating that the interaction between AC and C is not significant. Analysis of variance (ANOVA) results show that the mean squares of the three interaction terms AB, AC, and BC are 0.0081, 0.0023, and 0.0096, respectively, with corresponding F-values ​​of 8.51, 2.40, and 10.12. Among these, BC has the largest mean square and the highest F-value (P < 0.05), indicating that the interaction between extraction time and entrainer dosage has the most significant contribution to the variation in extraction rate. AB has the next largest mean square and F-value, but P < 0.05, also showing a significant interaction effect. AC has the smallest mean square and F-value, and P > 0.05, indicating that the interaction between extraction temperature and entrainer dosage is not significant. Looking at the coefficients of the multiple regression equation, the coefficients of terms AB, BC, and AC are all positive, indicating a positive synergistic effect among the factors. When temperature and time, and time and entrainer, increase or decrease simultaneously, the combined effect of both on the extraction rate is greater than the algebraic sum of their individual effects. Among them, term BC has the largest mean square, F-value, and highest regression coefficient, further confirming that the synergistic effect between extraction time and entrainer dosage is the strongest; term AB is the second strongest. Although the regression coefficient of term AC is positive, its mean square is small, its F-value is low, and P > 0.05, therefore there is no reliable interaction between extraction temperature and entrainer dosage.

[0064] This invention, through Design-Expert 13 software analysis, determined the optimal extraction temperature to be 49.784 ℃, the optimal extraction time to be 57.886 min, and the optimal entrainer dosage to be 152.071 mL, achieving a maximum extraction rate of 1.0380%. Considering the limitations of practical operation, the process conditions were adjusted to an extraction temperature of 50 ℃, an extraction time of 58 min, and an entrainer dosage of 150 mL. Under these parameters, the average extraction rate of Wuyi Rock Tea using supercritical extraction was 1.04±0.02%, close to the optimal value predicted by the software model, indicating that the model has good predictive ability and can be used in practical operations. Based on the optimized parameters, supercritical CO2 fluid extraction was performed on Wuyi Rock Tea varieties Qidan, Beidou, 105 Huang Guanyin, and Shuixian, with extraction yields of 1.111±0.31%, 0.85±0.10%, 0.75±0.13%, and 1.011±0.19%, respectively.

[0065] Through single-factor experiments combined with response surface methodology optimization, this invention determined the optimal process conditions for supercritical CO2 fluid extraction of Wuyi rock tea. The optimal extraction parameters were: extraction temperature 50℃, extraction time 58 min, extraction pressure 20 MPa, CO2 flow rate 20 L / h, and entrainer volume 150 mL. Under these optimized conditions, the extraction rates of five Wuyi rock tea varieties were: Rougui 1.04±0.02%, Qidan 1.11±0.31%, Beidou 0.85±0.10%, 105 Huang Guanyin 0.75±0.13%, and Shui Xian 1.01±0.19%. The standard deviations of ten parallel experiments for each variety were all within acceptable ranges, indicating that the experimental method has good stability and reproducibility. In conclusion, the supercritical CO2 fluid extraction method established in this study is suitable for the extraction of aroma substances from Wuyi rock tea and can provide reliable technical support for subsequent aroma component analysis and comparison of differences between varieties.

[0066] Example 2: Optimal Application of Wuyi Rock Tea Aroma Extract in Perfume Enhancement

[0067] This embodiment uses supercritical fluid extracts prepared from different varieties of lightly roasted Wuyi rock tea as raw materials. A systematic analysis of the volatile compounds in five supercritical fluid extracts was conducted using electronic nose, two-dimensional gas chromatography / time-of-flight mass spectrometry (GC×GC-TOFMS), combined with multivariate statistical analysis and relative odor activity value (rOAV). Furthermore, the aroma-enhancing potential of Wuyi rock tea extracts was evaluated by adding them to perfumes at gradient concentrations using sensory analysis and GC-MS. The aim is to deepen the understanding of key aroma characteristic substances through a systematic analysis of the aroma components of Wuyi rock tea supercritical fluid extracts, laying a scientific foundation for the high-value-added utilization of tea.

[0068] (1) Materials and Instruments

[0069] Cinnamon extract (RG-E), Qidan extract (QD-E), Beidou extract (BD-E), 105HGY extract (105HGY-E), and Narcissus extract (SX-E) were prepared in Example 1. n-Alkanes (C7~C30, 99% purity) were obtained from Shanghai Maclean Biochemical Technology Co., Ltd. Sodium chloride (analytical grade) and n-hexane (chromatographic grade) were also used. The required instruments and equipment are shown in Table 6.

[0070] Table 6 Experimental Instruments and Equipment

[0071] ,

[0072] (2) Experimental method:

[0073] Five tea samples were analyzed using a PEN3 portable electronic nose system. 0.02 g of extract was accurately weighed into an odorless 50 mL centrifuge tube, covered with plastic wrap, and allowed to stand at room temperature for 30 minutes. After aroma enrichment, the volatiles were injected into the electronic nose sensor at a rate of 0.60 L / min for 90 s, with three replicates per sample. The types of volatiles were identified using semiconductors R1 (aromatic hydrocarbons); R2 (nitrogen oxides); R3 (aromatic amines); R4 (hydrogen); R5 (aromatic aldehydes); R6 (methane); R7 (sulfides, terpenes); R8 (broad-range alcohols); R9 (organosulfides); and R10 (alkanes).

[0074] HS-SPME method: Weigh 0.50 g (accurate to 0.01 g) of Wuyi rock tea supercritical extract into a 20 mL magnetic headspace vial, add saturated NaCl solution and 10 μL of internal standard ethyl decanoate (8.63 mg / L), and seal with a magnetic headspace cap. After equilibration in an 80 ℃ water bath for 10 min, extract for 30 min using an SPME50 / 30μm SFIB-DVB / C-WR-80 / 10-P1 extraction head. After extraction, desorb at 250 ℃ for 5 min.

[0075] GC×GC conditions: Column type: SV (C6~C40); one-dimensional column HP-5MS (30 m × 0.25 mm × 0.25 μm), two-dimensional column DB-17MS (2.32 m × 0.18 mm × 0.18 μm); temperature program: initial temperature 40 ℃, hold for 1 min; increase to 180 ℃ at 3 ℃ / min, hold for 1 min; increase to 250 ℃ at 20 ℃ / min, hold for 5 min; injection port temperature 250 ℃; MSD transfer line temperature 280 ℃; carrier gas: helium (99.999%); split ratio 30:1; column flow rate 1.10 mL / min; modulation period 10 s.

[0076] TOFMS conditions: EI source, ion source temperature 230 °C, EI source energy 70 eV, mass scan range: 45~500 u.

[0077] Qualitative and quantitative methods for volatile components in extracts: Qualitative analysis was performed using Canvas software on a two-dimensional gas chromatography data processing workstation. The minimum peak detection signal-to-noise ratio was set to 10. The mass spectrometry information of each chromatographic peak was compared with the NIST20 mass spectrometry library. 3 μl of n-alkanes were detected under the same instrument conditions, and the retention times of the corresponding n-alkanes were recorded. The retention index of volatile compounds was calculated. Compounds with forward matching >700, reverse matching >700, and retention indices (RI) within ±30 were selected for retention. Quantitative analysis was performed using the internal standard method to quantify aroma compounds in Wuyi rock tea. The relative content was calculated by the ratio of the peak area of ​​the volatile component to the peak area of ​​the internal standard ethyl decanoate. Each sample was analyzed three times, and the average value was taken. The calculation formula is as follows:

[0078] ;

[0079] ;

[0080] Where: C1, relative content of compounds in the original tea; C2, relative content of compounds in the extract, μg / kg; R1, ratio of peak area of ​​compounds in the original tea to peak area of ​​the internal standard; R2, ratio of peak area of ​​compounds in the extract to peak area of ​​the internal standard; M, amount of sample added, g; y, yield of Wuyi rock tea by supercritical extraction, %.

[0081] To evaluate the aroma-enhancing potential of Wuyi rock tea extract, aroma enhancement experiments were conducted using RG-E as the raw material, with a commercially available light and delicate perfume (Burberry Brit Sheer) as the base. Five concentration levels of extract samples (0.05%, 0.15%, 0.40%, 0.80%, and 2.00%, by weight) were prepared and named 0.05% RG-E, 0.15% RG-E, 0.40% RG-E, 0.80% RG-E, and 2.00% RG-E, respectively. The preparation method involved directly mixing the powdered extract into the base, or precisely adding the extract stock solution to 10.00 mL of perfume base. After vortex mixing and sonication, all samples were equilibrated at 25°C in the dark for 24 hours. The perfume without added extract served as a blank control group (CK) for subsequent sensory and instrumental analyses.

[0082] Aroma Evaluation of Fragrance Enhancement Samples: The sensory panel consisted of seven professionally trained experts (4 men and 3 women, aged 25-50). Prior to the formal evaluation, all panel members underwent two weeks of standardized training (3 hours daily). The training included exposure to a series of reference standards with clearly defined aroma attributes and varying intensities to calibrate their olfactory perception and descriptive vocabulary. The training concluded after the judges successfully passed blinded identification tests. During the evaluation, 0.5 mL of each perfume sample was evenly applied to strips of fabric of the same size and material. The sensory evaluation was conducted in two consecutive phases. In the first round, all samples were presented in random order, and an overall sensory preference was assessed using a 100-point scale to select the best sample. In the second round, each aroma attribute (e.g., floral, fruity, woody) of the selected samples was scored on a 10-point scale for intensity. All sensory data are presented as mean ± standard deviation.

[0083] Detection of volatile compounds in fragrance-enhancing perfume samples and CK: Samples were removed from a -80℃ freezer and thawed on ice. 10 μL was pipetted into 9990 μL of n-hexane and vortexed until homogeneous. 100 μL of each sample was transferred to a vial, and 20 μL (10 μg / mL) of internal standard solution was added. The vials were stored at -20℃ for GC-MS analysis. Chromatographic conditions were: injection volume 1 μL, DB-5MS capillary column (30 m × 0.25 mm × 0.25 μm, Agilent J&W Scientific, Folsom, CA, USA), carrier gas high-purity helium (purity not less than 99.999%), constant flow rate 1.2 mL / min, injection port temperature 250℃, and solvent delay 3.5 min. Temperature program: Hold at 40℃ for 3.5 min, increase to 100℃ at 10℃ / min, then increase to 180℃ at 7℃ / min, and finally increase to 280℃ at 25℃ / min, hold for 5 min. Mass spectrometry conditions: Electron impact ionization (EI) source, ion source temperature 230℃, quadrupole temperature 150℃, mass spectrometer interface temperature 280℃, electron energy 70 eV, scan mode selected ion detection (SIM), qualitative and quantitative ion precise scan (GB23200.8-2016).

[0084] rOAV calculation method: Based on quantitative analysis, the reported thresholds of aroma active ingredients in the literature are consulted, and the rOAV value is calculated. In previous studies, aroma active ingredients with rOAV ≥ 1 are often considered to make a significant contribution to the overall aroma formation. rOAV calculation formula:

[0085] ;

[0086] In the formula: rOAV, relative odor activity value; C, relative content of compound, μg / kg; OT, compound threshold, μg / kg.

[0087] Data processing

[0088] (3) Results: As an analytical tool capable of rapidly determining aroma intensity, the electronic nose can be effectively applied to the aroma intensity assessment of Wuyi rock tea extract samples. For example... Figure 7As shown in the radar chart, the maximum response intensity of the 10 sensors is closely related to the concentration of volatile compounds. The differences in these response values ​​indicate the diversity of volatile compound composition in the extract samples. Among the 10 sensors, the Wuyi rock tea extract showed the strongest response to the W1W sensor, followed by W1S and W2W. These three types of sensors are sensitive to sulfides, methane and aromatic compounds, and organosulfur compounds, respectively. The W5S sensor, in particular, showed the highest response value and exhibited high sensitivity to nitrogen oxides. The unique response characteristics of different Wuyi rock tea extracts in the sensor array reveal the inherent diversity of Wuyi rock tea varieties. This analysis provides a preliminary understanding of the aroma intensity characteristics of Wuyi rock tea extracts.

[0089] Supercritical fluid extracts prepared from five types of Wuyi rock tea were analyzed using HS-SPME-GC×GC-TOFMS technology. A total of 275 volatile compounds were detected in the five Wuyi rock tea extracts. RG-E, QD-E, BD-E, 105HGY-E, and SX-E contained 151, 137, 163, 184, and 172 volatile compounds, respectively. 105HGY-E had the highest number of volatile compounds, while QD-E had the lowest, which is similar to the distribution pattern of volatile compounds in dry tea. The 275 volatile compounds were classified into 37 alcohols, 21 aldehydes, 36 ketones, 61 esters, 6 phenols, 5 acids, 3 ethers, 18 aromatics, 30 alkanes, 42 alkenes, 3 alkynes, and 13 heterocyclic compounds. Figure 8 (A) Among them, esters, alkenes, and alcohols account for the largest proportion. Esters, alkenes, and alcohols typically impart floral, fruity, and sweet aromas, laying an important foundation for the pleasant floral and fruity aromas in Wuyi rock tea extracts. Figure 8 As shown in Figure B, there are significant differences in the total relative content of volatile compounds among different Wuyi rock tea extracts. Furthermore, the distribution of the relative content of various volatile compounds in different extracts also varies considerably. This may be the fundamental reason for the differences in aroma among the five Wuyi rock tea extracts. Figure 8As shown in Figures C and D, among the 275 volatile compounds, alcohols, esters, heterocyclic compounds, and ketones have relatively high contents, and 74 compounds are common to the five Wuyi rock tea extracts. In terms of compound categories, these common components mainly consist of alcohols, aldehydes, ketones, esters, alkanes, and alkenes. Analysis of aroma characteristics shows that most compounds exhibit floral, fruity, and woody properties, such as linalool (floral aroma), phenylethyl alcohol (rose aroma), β-ionone (dry powder floral aroma), and α-farnesene (citrus and lavender aroma), which together constitute the aroma basis of Wuyi rock tea extracts. Regarding the distribution of compounds specific to each extract, the number of unique components in RG-E, QD-E, BD-E, 105HGY-E, and SX-E are 16, 7, 14, 23, and 17, respectively. This difference is likely closely related to factors such as tea variety, production environment, processing technology, and storage conditions. Different tea varieties accumulate secondary metabolites differently. The microclimate and soil conditions of the producing area influence the formation of aroma precursors, while processing steps such as shaking and roasting, as well as chemical transformations during subsequent storage, further shape the unique flavor characteristics of each sample. Overall, common compounds lay the foundation for the shared aroma of Wuyi rock tea extracts, while differences in unique components reflect the individual characteristics of different samples in terms of varietal origin and processing techniques, reflecting the complexity and diversity of tea aroma formation.

[0090] This invention explores the differences in volatile compounds among different Wuyi rock tea extracts. For example... Figure 9 As shown in Figure A, the principal component analysis (PCA) score plot indicates good sample repeatability, with significant separation among the five Wuyi rock tea extracts, suggesting significant differences in the composition and distribution of their volatile components. These differences constitute the unique aroma basis of each extract. To screen for differentially expressed volatile compounds, this study further employed PLS-DA analysis. Figure 9 As shown in B, R 2 The Y value reached 0.998, Q 2 The value reached 0.996, indicating that the five groups of samples had good differentiation, and the results of 200 permutation tests ( Figure 9 (C) Confirms that the model did not exhibit overfitting, indicating the reliability of the results. The supervised pattern recognition method PLS-DA was used to reduce the dimensionality of the high-dimensional metabolomics data to maximize the separation between samples. Volatile compounds with an importance score (VIP) greater than 1.0 were selected as key factors influencing sample differences and included in subsequent analysis. A total of 64 differentially expressed volatile compounds were identified. These 64 compounds were used to distinguish five Wuyi rock tea extracts, and their relative abundance was visualized using a heatmap, showing the compositional differences between samples. Figure 9Based on their chemical structures, these 64 volatile compounds were classified into esters (18), alcohols (11), ketones (8), heterocyclic compounds (5), aldehydes (5), aromatics (5), alkenes (4), alkanes (4), acids (3), and alkynes (1). Esters accounted for the largest proportion, which may be due to genetic differentiation among different varieties of Wuyi rock tea. (In the heatmap...) Figure 9 (D) The color depth corresponds to the abundance of volatile compounds, with dark green indicating lower content and dark red indicating higher content. Based on the distribution patterns of 64 differentially volatile compounds in five Wuyi rock tea extracts, they were clustered into five groups. Notably, the compounds in each cluster were mainly enriched in a single extract, suggesting that they may be characteristic volatile compounds originating from the specific genetic background of the tea variety. From a broader perspective, QD-E generally had relatively low content in most differentially volatile compounds, consistent with its previously recorded lowest total volatile compound content. Group I differentially volatile compounds were mainly enriched in the BD-E sample, with significantly higher content than other samples. These volatile compounds constitute the unique aroma characteristics of BD-E. Most of these compounds have floral and fruity characteristics, such as geraniol, methyl heptenone, and phenylacetaldehyde, which together form the core floral and fruity flavor profile of BD-E. Other components, such as methyl palmitate and caryophyllin, have subtle woody or spicy notes, which may be the key source of the woody aroma in BD-E. Group II differentially volatile compounds are mainly concentrated in RG-E, laying the material foundation for the formation of RG-E's unique aroma. The aroma characteristics of RG-E are influenced by a variety of floral and sweet compounds, including cis-3-hexenol benzoate, coumarin, and E-β-ionone, which together contribute to the distinctive floral and sweet characteristics of RG-E. Group III differentially volatile compounds are significantly enriched in SX-E, a pattern that may stem from the unique metabolic background of the Narcissus tea variety. According to literature research, Group III contains four aromatic differentially volatile compounds: ethyl phenylacetate with a sweet floral aroma, dibutyl phthalate with a delicate aroma, ethyl hexanoate with a honey-like aroma, and 2-acetylpyrrole with a roasted aroma. The significant characteristic of 105HGY-E is the significant enrichment of Group IV differentially volatile compounds, which constitute its signature aroma. These compounds are characterized by fruity aromas, contrasting sharply with the floral and sweet aromas emphasized in the previous categories. This class includes compounds with coconut-like aromas. - Pentylbutyrolactone, fruit-scented dihydroactinolactone, and cucumber-scented 3-(4-isopropylphenyl)isobutyraldehyde. Group V differentially volatile compounds were relatively abundant in 105HGY-E and SX-E, while a few differentially volatile compounds, such as β-cyclocitral, linalool, diethyl succinate, dimethyl phthalate, and jasmine lactone, were relatively abundant in RG-E.

[0091] like Figure 10 As shown, seven compounds made particularly significant contributions to the overall aroma, with average rOAV values ​​exceeding 1000. Sorted from highest to lowest rOAV value, they are: E-β-ionone (3,837,894.77; floral, fruity), (E,E)-3,5-octadien-2-one (2,241,525.61; fruity, green), linalool (16,529.28; floral), (2-nitroethyl)benzene (8,976.71; floral), indole (5,471.93; floral, fruity), β-cyclocitral (1,796.18; sweet, herbal, baked), methyl palmitate (1,257.00; fresh), and α-ionone (1,163.06; sweet, floral, fruity). These varietal-specific compounds are crucial for the formation of unique varietal aromas and lay the foundation for the development of differentiated flavor products.

[0092] This invention constructs a flavor wheel of Wuyi rock tea extract (e.g. Figure 11 (As shown). The 34 key aroma active compounds were divided into 14 floral aroma categories, 6 fruity aroma categories, 6 complex floral aroma types (floral-woody, floral-fruity, floral-sweet), and other categories. Most key aroma active compounds are dominated by floral properties, which is the core aroma characteristic of Wuyi rock tea extract. The 6 complex floral volatile organic compounds include cis-linalool oxide (furans) and caryophyllein, which have floral and woody aromas; jasmine lactone and indole, which have floral and fruity aromas; and hexanoate and jasmine lactone, which have sweet and floral aromas. These components significantly enrich the aroma spectrum of Wuyi rock tea extract.

[0093] All 34 key aroma-active compounds exhibited binding interactions with both types of olfactory receptors, and the binding energy values ​​reflected their binding affinity (as shown in Table 7).

[0094] Table 7 Binding energies between key aroma-active compounds and olfactory receptors

[0095] ,

[0096] Eight key aroma compounds with the highest affinity for olfactory receptors were selected for visual analysis (e.g.) Figure 12 (as shown) Figure 12Key aroma active components interacting with olfactory receptors (ORs): A represents the interaction between coumarin and OR1A1; B represents the interaction between E-nerolidol and OR1A1; C represents the interaction between coumarin and OR1D2; D represents the interaction between caryophyllin and OR1D2; E represents the interaction between jasmine lactone and OR1A1; F represents the interaction between β-cyclic citral and OR1A1; G represents the interaction between jasmone and OR1A1; H represents the interaction between β-cyclic citral and OR1D2.

[0097] As shown in Table 8, aroma enhancement experiments were conducted using RG-E as the raw material. RG-E was added to Burberry Brit Sheer Eau de Toilette at five different concentrations (0.05%, 0.15%, 0.40%, 0.80%, and 2.00%, by mass) to evaluate its aroma enhancement potential and to screen for the optimal additive dosage. Wuyi rock tea extract RG-E significantly enhanced the overall aroma of the perfume. The optimal aroma enhancement effect was achieved when the Wuyi rock tea extract addition was 0.40%. With the gradual addition of Wuyi rock tea extract, the aroma of the perfume showed significant changes. No significant change was observed at a concentration of 0.05%; at concentrations of 0.15% and 0.40%, a significant enhancement of floral and sweet notes was perceived, accompanied by a fresh quality. The enhancement effect tended to plateau within the concentration range of 0.40% to 0.80%, with the latter showing only a slight advantage. Given the negligible sensory benefits at high doses, 0.40% was ultimately selected as the cost-optimal concentration for practical application. At a concentration of 2.00%, the sensory experience deteriorated drastically, with a strong, pungent sweet floral scent, and off-flavors completely overwhelmed the base notes, utterly negating any enhancing effects.

[0098] Table 8 Sensory Evaluation of Fragrance Enhancement from Extracts

[0099] ,

[0100] like Figure 13 As shown, the results indicate that floral and sweet aromas significantly increased compared to the control group (CK). This suggests that the aroma characteristics of RG-E are primarily composed of floral and sweet attributes. Furthermore, RG-E introduces a distinctly fresh character to the aroma spectrum. However, at higher concentrations, the original milky and citrusy aromas of the control group are gradually masked.

[0101] like Figure 14 As shown in Figure A, the 896 compounds are categorized as follows: 140 esters, 79 heterocyclic compounds, 113 ketones, 58 hydrocarbons, 210 terpenes, 33 acids, 53 aldehydes, 21 ethers, 6 halogenated hydrocarbons, 5 sulfur-containing compounds, 18 nitrogen-containing compounds, 24 phenols, 15 aromatic hydrocarbons, 82 alcohols, and 39 amines. Figure 14As shown in Figure B, the total relative content of volatile compounds in CK was 53937.30 μg / mL, while the total relative content of volatile compounds in 0.40% RG-E was 58048.54 μg / mL. The addition of 0.40% RG-E significantly increased the relative content of volatile compounds in CK, which is the fundamental reason for its improved aroma and flavor. The relative content percentages and distributions of different types of volatile compounds are shown in Figure B. Figure 14 As shown in Figure C, the addition of 0.40% RG-E uniformly increased the relative content of various volatile compounds, thereby enhancing the aroma. (PCA score chart) Figure 14 The results (D) show that the CK and 0.40%RG-E samples are clearly distinguishable, indicating that the addition of 0.40%RG-E significantly alters the composition and distribution of volatile compounds in the CK sample. To further clarify the differences brought about by the addition of 0.40%RG-E, OPLS-DA analysis was performed on the CK and 0.40%RG-E samples, and the results are as follows: Figure 14 As shown in E, the two groups of samples are significantly different, and the substitution test results ( Figure 14 The F-square test indicates that the model is reliable and there is no overfitting, demonstrating its reliability. Substances with a VIP > 1 were defined as differentially volatile compounds distinguishing between the two samples. Through screening, 291 differentially volatile compounds with a VIP > 1 were obtained, accounting for one-third of the total number of volatile compounds, further demonstrating the effect of adding 0.40% RG-E on the distribution of volatile compounds in the control group (CK). A visualization heatmap was created for 33 differentially volatile compounds with a VIP > 2. Figure 14 (G) to visually demonstrate the differences in volatile compounds between the two groups of samples. For example... Figure 14 According to G, the relative content of volatile compounds in 0.40%RG-E was significantly higher than that in CK. The rOAV value calculation results showed that among the 33 differentially volatile compounds, 8 compounds had rOAV values ​​greater than 1, and were considered key flavoring compounds, such as... Figure 14As shown in Figure H, the eight compounds are 2-methylpentanal (fruity, fresh), nerol acetate (rose, citrus, pear), geraniol acetate, 2-undecone (fruity, creamy, iris), 1-propenylhexyl propionate, 3-decone (banana, sweet), E-farnesene epoxide, and nonanal (citrus). The increased rOAV values ​​of these volatile compounds, which mainly exhibit floral, sweet, and fruity aromas, are a significant reason for the enhanced floral and sweet aromas in the 0.4% RG-E sample. Overall, the addition of RG-E significantly altered the distribution of volatile compounds in the CK, enhancing its floral, sweet, and fresh aroma properties, thereby improving its overall aroma quality. These results indicate that Wuyi rock tea extract has promising applications in the cosmetics or beverage fragrance enhancement field. Therefore, adding 0.40% RG-E can significantly alter the distribution of volatile compounds in perfumes, effectively enhancing their floral, sweet, and fresh aroma properties, and thus improving the overall aroma quality of the perfume. The results validate the feasibility of Wuyi rock tea extract as a natural flavoring ingredient and demonstrate its application potential in the food flavoring and fragrance industry.

[0102] Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Anyone skilled in the art can make various modifications and alterations without departing from the spirit and scope of the present invention. Therefore, the scope of protection of the present invention should be defined by the claims.

Claims

1. A supercritical CO2 extraction method for aroma components of Wuyi rock tea, characterized in that, Includes the following steps: (1) Raw material pretreatment: Lightly roasted Wuyi rock tea is crushed; (2) Loading and system balancing: Tea powder is loaded into the extraction vessel, and the temperature of separation vessel I is set to 45-50℃ and the pressure to 6-8 MPa, and the temperature of separation vessel II is set to 25-35℃ and the pressure to 4-6 MPa. The system is then stabilized; (3) Supercritical extraction: CO2 is used as the extractant and anhydrous ethanol is used as the entrainer. The extraction temperature is 45-55℃, the extraction pressure is 10-20 MPa, the extraction time is 40-60 min, the CO2 flow rate is 10-22 L / h, and the entrainer dosage is 140-160 mL / 150 g of raw tea powder; (4) Separation and concentration: After extraction, the oil phase extract is separated and collected. The extract is concentrated under reduced pressure to obtain the aroma extract of Wuyi rock tea.

2. The method according to claim 1, characterized in that, Lightly roasted Wuyi rock tea is an oolong tea processed using a light roasting technique. The variety is selected from at least one of the following: Rougui, Qidan, Beidou, 105 Huang Guanyin, or Shui Xian.

3. The method according to claim 1, characterized in that, The entrainer is anhydrous ethanol.

4. The method according to claim 1, characterized in that, The optimal extraction parameters are: extraction temperature 50℃, extraction pressure 20 MPa, extraction time 58 min, CO2 flow rate 20 L / h, and entrainer anhydrous ethanol volume 150 mL.

5. The method according to claim 1, characterized in that, The aroma extract prepared contains one or more of the following: ionone, 3,5-octadien-2-one, damascene, linalool, geraniol, tea ketone, and indole.

6. The application of a Wuyi rock tea aroma extract prepared by the method according to any one of claims 1-5 in perfume flavoring.

7. The application according to claim 6, characterized in that, Wuyi rock tea aroma extract was added to the perfume base as a natural fragrance enhancer. After mixing, sonication, and equilibration in the dark, the fragrance-enhanced perfume was obtained.

8. The application according to claim 7, characterized in that, Based on the total mass of the perfume, the amount of Wuyi rock tea aroma extract added is 0.05% to 2.00%.

9. The application according to claim 8, characterized in that, The optimal addition amount of the Wuyi rock tea aroma extract is 0.40%.

10. A method for enhancing the fragrance of a perfume, characterized in that, The method includes taking the aroma extract of Wuyi rock tea prepared by the method according to any one of claims 1-5, adding it to the perfume base, and after mixing, sonicating, and standing in the dark to achieve equilibrium, a fragrance-enhancing perfume with the characteristic aroma of Wuyi rock tea is obtained.

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