Method for refining water-soluble components and fat-soluble components in grapefruit peel essential oil, and products and applications thereof

By using the mixing, ultrasonic and enzymatic treatment of pomelo peel and water in the preparation process of pomelo peel essential oil, combined with edible alcohol extraction and molecular distillation technology, the water-soluble and fat-soluble components in pomelo peel essential oil were successfully separated, solving the problems of low separation efficiency and insufficient solvent safety in the existing technology, and achieving efficient, green and safe essential oil separation and application expansion.

CN119736122APending Publication Date: 2025-04-01LUZHOU PINCHUANG TECH CO LTD
View PDF 2 Cites 0 Cited by

Patent Information

Application Number
CN202510040572.0
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-01-10
Publication Date
2025-04-01

AI Technical Summary

Technical Problem

The existing preparation methods for pomelo peel essential oil cannot effectively separate terpenes and terpene oxides, and the extraction solvent used is not green and safe enough, limiting the application scope of the product.

Method used

The pomelo peel is mixed with water and is subjected to crushing, ultrasonic and enzymatic treatment, and then the pomelo peel essential oil is obtained by steam distillation. Then, using edible alcohol as the extraction solvent, mixed with pomelo peel essential oil and crude oil, centrifuged to obtain a mixed liquid of aqueous phase and oil phase. Finally, molecular distillation is performed separately to obtain water-soluble and fat-soluble components.

Benefits of technology

The efficient separation of terpene oxides and terpenes was achieved, and the content of terpene oxides in the water-soluble components increased from 8.21% to 77.49%, while the content of terpene oxides in the fat-soluble components decreased from 87.15% to 7.36%. At the same time, the solvent used is safe and easy to peel, expanding the application field of pomelo peel essential oil.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN119736122A_ABST
    Figure CN119736122A_ABST
Patent Text Reader

Abstract

The invention discloses a method for refining water-soluble components and fat-soluble components in grapefruit peel essential oil, and its products and applications, and belongs to the technical field of separation and purification of natural products. The refining method comprises the following steps: A. grapefruit peel is mixed with water, and after crushing, ultrasonication and enzymolysis treatment, steam distillation is performed to obtain grapefruit peel essential oil crude oil; B. grapefruit peel essential oil crude oil is mixed with extraction solvent, and centrifuged and separated to obtain upper aqueous phase mixed liquid and lower oil phase mixed liquid; C. molecular distillation treatment is performed on the aqueous phase mixed liquid and the oil phase mixed liquid respectively, and the heavy phase fraction of the aqueous phase mixed liquid is collected as the water-soluble component of grapefruit peel essential oil, and the light phase fraction of the oil phase mixed liquid is collected as the fat-soluble component of grapefruit peel essential oil. The invention carries out deep processing of grapefruit peel, improves the utilization rate of grapefruit resources, and the reagents used in the preparation process are safe, non-toxic and easy to peel, which expands the application field of grapefruit peel essential oil.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The invention belongs to the technical field of separation and purification of natural products, relates to a method for deep processing of plant essential oils, and specifically relates to a method for refining water-soluble components and fat-soluble components in grapefruit peel essential oil, and a product and application thereof. Background Art

[0002] Grapefruit peel essential oil is a natural fragrance extracted from grapefruit peel by steam distillation, supercritical CO2 and other methods. It is often used as a raw material or additive in food processing and other fields. However, most of the grapefruit peel essential oils on the market are still in the crude extract stage, with problems such as poor water solubility, easy emulsification and stratification, and insufficient stability, which limits its application range. These problems are mainly due to the differences in properties between the two main components (terpenes and terpene oxides) in the crude grapefruit peel essential oil. Terpenes are high in content in grapefruit peel essential oil and are a class of non-polar and highly volatile components that are sensitive to light, heat and oxygen, while terpene oxides are low in content in grapefruit peel essential oil. These components contain oxygen atoms, such as hydroxyl groups and carbonyl groups, and show relatively high polarity and low volatility. At present, deep-processed grapefruit peel essential oil products for different solvent matrices are relatively scarce. Therefore, exploring how to solve these problems caused by differences in ingredient properties through deep processing technology in order to expand the application areas of grapefruit peel essential oil crude oil and even plant essential oil crude oil has always been a hot topic in domestic research and a focus of attention for essential oil production companies.

[0003] CN118909698A discloses a method for simultaneously extracting water-soluble and fat-soluble essential oils from peony flowers, wherein peony flower powder is mixed with a sodium chloride aqueous solution, and the water-soluble and fat-soluble essential oils are simultaneously extracted by adding pure water and n-hexane, heating and distilling, collecting hydrosols, separating water-oil layers, and performing vacuum distillation. However, the method uses an inedible organic solvent as an extraction solvent during the extraction process, and it is difficult to effectively remove the solvent after the fat-soluble essential oil is mixed with n-hexane, and these factors limit the further application of the method.

[0004] CN115386429A discloses a classification and refining method of tangerine essential oil and its application. The method uses tangerine essential oil crude oil as raw material, and after freezing and centrifugation, uses molecular distillation technology to fractionate the essential oil to obtain four fractions. This technology can achieve the classification of tangerine essential oil, but it cannot effectively separate terpenes and terpene oxides in tangerine essential oil. Even the fraction IV with the lowest terpene content has a terpene content of more than 45%, which means that these four fractions still maintain a high fat-soluble characteristic and are difficult to be widely used in water-based and alcohol-based products.

[0005] CN116751633A discloses a plant essential oil deterpenization process and its application, which combines an adsorbent and supercritical CO2 technology to achieve effective separation of terpene oxides and terpenes in ginger essential oil. Through this process, the relative content of terpene oxides in the separation kettle can reach 70%, and the content of terpenes in the extraction kettle can also reach 70%. Nevertheless, there is still room for further improvement in the separation efficiency between terpene oxides and terpenes. In addition, the high cost of supercritical CO2 equipment also limits the industrial application of this process.

[0006] Therefore, there is an urgent need to develop a method that can effectively separate the water-soluble and fat-soluble components in grapefruit peel essential oil. Summary of the invention

[0007] The technical problems to be solved by the present invention are that the existing preparation method of grapefruit peel essential oil cannot effectively separate terpenes and terpene oxides; and the existing method for separating water-soluble essential oil and fat-soluble essential oil uses reagents that are not green and safe enough and cannot be completely stripped from the product, which limits the application of the final product.

[0008] The technical solution adopted by the present invention to solve its technical problem is:

[0009] In a first aspect, the present invention provides a method for refining water-soluble components and fat-soluble components in grapefruit peel essential oil, comprising the following steps:

[0010] A. Pomelo peel is mixed with water, crushed, ultrasonicated, and enzymatically treated, and then steam distilled to obtain pomelo peel essential oil crude oil;

[0011] B. mixing the grapefruit peel essential oil crude oil and the extraction solvent, centrifuging and separating to obtain an upper aqueous phase mixed liquid and a lower oil phase mixed liquid;

[0012] C. The aqueous phase mixture and the oil phase mixture are subjected to molecular distillation treatment respectively, and the heavy phase fraction of the aqueous phase mixture is collected as the water-soluble component of the grapefruit peel essential oil, and the light phase fraction of the oil phase mixture is collected as the fat-soluble component of the grapefruit peel essential oil.

[0013] In the above refining method, in step A, the pomelo peel and water are mixed in a mass ratio of 1:3 to 5.

[0014] In the above purification method, in step A, the ultrasonic treatment is specifically as follows: subjecting the crushed mixture to ultrasonic treatment at a power of 100 to 200 W for 30 to 50 minutes.

[0015] In the above refining method, in step A, the enzymatic hydrolysis treatment is specifically as follows: adjusting the pH of the mixture after ultrasound to 4-5 by food-grade citric acid or malic acid, then adding 1-3% pectinase by mass of the mixture, and enzymolyzing at 40-50° C. for 2-4 hours.

[0016] In the above refining method, in step A, the steam distillation is specifically as follows: pouring the enzymatically hydrolyzed mixture into an essential oil extraction device, heating to boiling, collecting the distillate, and cooling.

[0017] In the above refining method, in step B, the solid-liquid ratio of the extraction solvent to the grapefruit peel essential oil crude oil is 1:1-3.

[0018] In the above refining method, in step B, the above extraction solvent is edible alcohol with a concentration of 30-60%.

[0019] In the above purification method, in step B, the centrifugal speed is 4000-8000 rpm and the time is 5-10 min.

[0020] In the above-mentioned purification method, in step C, the conditions for molecular distillation are: incubation temperature 25-35°C, evaporation temperature 25-35°C, distillation pressure 100-300Pa, scraper speed 200-300rpm, feed rate 1-5mL / min, and condensed water temperatures are 0°C, -10°C, and -20°C, respectively.

[0021] In a second aspect, the present invention provides water-soluble components and / or fat-soluble components in the grapefruit peel essential oil prepared by the above-mentioned refining method.

[0022] The water-soluble components in the above-mentioned grapefruit peel essential oil include, but are not limited to, terpene oxides such as nerol, L-carveol, D-carvone, (-)-4-terpineol, and linalool.

[0023] The fat-soluble components in the above-mentioned grapefruit peel essential oil include, but are not limited to, terpenes such as (+)-limonene, myrcene and α-pinene.

[0024] In a third aspect, the present invention provides a composition comprising the water-soluble components and / or fat-soluble components in the grapefruit peel essential oil obtained by the above-mentioned refining method, or the water-soluble components and / or fat-soluble components in the above-mentioned grapefruit peel essential oil.

[0025] In a fourth aspect, the present invention provides the water-soluble components and / or fat-soluble components in the grapefruit peel essential oil obtained by the above-mentioned refining method, or the water-soluble components and / or fat-soluble components in the above-mentioned grapefruit peel essential oil, or the use of the above-mentioned composition in the fields of food, beverages, cosmetics, and daily chemical products.

[0026] The above application is: using the water-soluble components and fat-soluble components in the grapefruit peel essential oil to prepare a wine with grapefruit flavor, which specifically includes the following steps:

[0027] a. The highly fragrant liquor is diluted with water, adsorbed with activated carbon, and filtered to obtain a low-alcohol liquor;

[0028] b. mixing the water-soluble components and fat-soluble components in the grapefruit peel essential oil to obtain a mixed essential oil component;

[0029] c. The mixed essential oil component and the highly fragrant liquor are mixed to obtain a mixed solution;

[0030] d. Mix the low-alcohol liquor and the mixed solution to obtain a liquor with a grapefruit flavor.

[0031] Furthermore, in step a, the alcohol content of the high-fragrance liquor is 65% vol, and the alcohol content of the low-alcohol liquor is 20-30% vol.

[0032] Furthermore, in step b, the water-soluble component and the fat-soluble component are mixed in a w:w ratio of 10 to 50:1.

[0033] Furthermore, in step b, the water-soluble component and the fat-soluble component are mixed in a w:w ratio of 10:1.

[0034] Furthermore, in step c, the mixed essential oil component and the high-fragrance liquor are mixed in a w:w ratio of 1:100.

[0035] Furthermore, in step d, the low-alcohol liquor and the mixed solution are mixed in a w:w ratio of 1:10.

[0036] The beneficial effects of the present invention are:

[0037] 1. First, the present invention uses edible alcohol with high safety and little effect on aroma as a green and non-toxic extraction solvent. The extraction solvent concentration and mixing ratio defined by the present invention can make the extraction process show high selectivity, high distribution coefficient and high extraction rate, and the terpene oxides and terpenes are separated according to the polarity difference. Secondly, the present invention realizes the secondary separation of terpene oxides and terpenes by regulating the molecular distillation process. According to the molecular distillation conditions set by the present invention, terpene oxides and terpenes can be efficiently separated. Compared with the crude oil of grapefruit peel essential oil, the content of terpene oxides in the water-soluble component is significantly increased from 8.21% to 77.49%, while the terpene content is greatly reduced from 87.15% to 7.36%; the terpene oxide content of the fat-soluble component is reduced from 8.21% to 1.89%, and the terpene content is increased from 87.15% to 97.53%. In addition, this method is not only used for grapefruit peel essential oil, but also for other plant essential oils.

[0038] 2. The water-soluble component prepared by the present invention is rich in terpene oxides such as nerol, L-carveol, D-carvone, (-)-4-terpineol, linalool, etc., which have charming sweet fragrance, floral fragrance and fresh grapefruit fragrance. It is easily soluble and diffuses quickly in water-based and alcohol-based systems, achieving uniform and lasting release of fragrance. On the other hand, the fat-soluble component mainly contains (+)-limonene, myrcene and α-pinene, which have a typical fresh aroma of grapefruit peel and herbaceous fragrance, and its antioxidant property is superior to that of grapefruit peel essential oil crude oil, and is suitable for skin care oil, hair care oil and baked goods and other products. In addition, the water-soluble component and fat-soluble component obtained by the present invention both show good stability under normal temperature conditions.

[0039] 3. The present invention uses ultrasound combined with enzyme technology in the extraction process. Compared with the traditional steam distillation method, the extraction rate is increased by more than 30%, and non-thermal processing technology is used in the separation process to effectively protect heat-sensitive substances. The present invention performs deep processing on grapefruit peel, improves the utilization rate of grapefruit resources, and the reagents used in the preparation process are safe, non-toxic, and easy to peel, which expands the application field of grapefruit peel essential oil. BRIEF DESCRIPTION OF THE DRAWINGS

[0040] Figure 1 The relative content distribution of terpene oxides and terpenes in a total of 7 samples, including the grapefruit peel essential oil crude oil, water-soluble components and fat-soluble components prepared in Example 1, the aqueous phase mixed solution and the oil phase mixed solution prepared in Comparative Example 1, and the heavy phase fraction and the light phase fraction prepared in Comparative Example 2;

[0041] Figure 2 This is the total ion current diagram of the crude grapefruit peel essential oil, water-soluble components and fat-soluble components obtained in Example 2. DETAILED DESCRIPTION

[0042] The technical solution of the present invention can be specifically implemented in the following manner.

[0043] A method for refining water-soluble and fat-soluble components in grapefruit peel essential oil, the method comprising:

[0044] (1) Select grapefruits of uniform maturity and moderate size, wash them, rinse them with distilled water and air-dry them at room temperature. Then cut the grapefruit peel and keep only the yellow outer skin part rich in essential oil as the main raw material for extracting grapefruit peel essential oil.

[0045] Preferably, the varieties of pomelo include but are not limited to Hejiang Zhenlong pomelo, Shatian pomelo and other varieties.

[0046] (2) Mix the grapefruit peel with distilled water at a mass ratio of 1:3-5, crush it with a wall-breaking machine, and then perform ultrasonic and enzymatic hydrolysis treatments in sequence. Pour the mixture into an essential oil extraction device and extract it by steam distillation. Heat to boiling state, start timing from the time when liquid drips, and stop timing when no essential oil flows out. After cooling, collect the grapefruit peel essential oil crude oil (crude extract), dry it with anhydrous sodium sulfate to remove water, and store it in a dark environment at 4°C.

[0047] Preferably, the ultrasonic process parameters are power 100-200W and time 30-50min.

[0048] Preferably, the enzymatic hydrolysis process is to add 1-3% pectinase by mass to the mixture at a pH of 4-5, and perform enzymatic hydrolysis at 40-50° C. for 2-4 hours; more preferably, food-grade citric acid or malic acid is used to adjust the pH to 4.5.

[0049] (3) Distilled water and edible alcohol are mixed to prepare an extraction solvent, which is mixed with the grapefruit peel essential oil crude oil in a certain proportion in a conical flask, sealed, stirred at room temperature for 30 to 80 minutes, and then centrifuged using a centrifuge to separate the aqueous phase mixture (lower layer) and the oil phase mixture (upper layer), and stored at 4° C. in a dark environment for future use.

[0050] Preferably, the ratio of the distilled water to the edible alcohol is 30% to 60%, and the solid-liquid ratio to the grapefruit peel essential oil crude oil is 1:1 to 1:3.

[0051] Preferably, the centrifuge speed is 4000-8000 rpm, and the centrifugation time is 5-10 min.

[0052] (4) The aqueous phase mixed liquid and the oil phase mixed liquid prepared in step (3) are subjected to molecular distillation treatment respectively. During molecular distillation, the material forms a thin film, and the less volatile components enter the heavy phase fraction collection bottle corresponding to the primary condenser, while the more volatile components enter the light phase fraction collection bottle corresponding to the secondary condenser. The heavy phase fraction of the aqueous phase is collected, which is the water-soluble component, and the light phase fraction of the oil phase mixed liquid is collected, which is the fat-soluble component.

[0053] When the distillation pressure is lower than 300Pa, the boiling point of the compound can be significantly reduced. At this time, if the evaporation temperature is too high, it will lead to the loss of small molecular compounds; if the evaporation temperature is too low, it is difficult to separate terpene oxides and terpenes. Therefore, the preferred molecular distillation conditions are: incubation temperature 25-35°C, evaporation temperature 25-35°C, distillation pressure 100-300Pa, scraper speed 200-300rpm, feed speed 1-5mL / min, and condensed water temperatures of 0°C, -10°C, and -20°C, respectively.

[0054] The technical solution and effects of the present invention are further illustrated below through practical examples.

[0055] Example

[0056] Example 1

[0057] 1. Preparation of water-soluble and fat-soluble components in grapefruit peel essential oil

[0058] Select Zhenlong pomelo of uniform maturity and moderate size, wash them, rinse them with distilled water and air dry them at room temperature. Then cut the pomelo peel, leaving only the yellow outer skin rich in essential oil as the main raw material for extracting pomelo peel essential oil.

[0059] Embodiments 1 to 3: A specific method for preparing water-soluble and fat-soluble components in grapefruit peel essential oil comprises the following steps:

[0060] 1. Take 500g of grapefruit peel and distilled water in a mass ratio of 1:3, mix them with a wall breaking machine, and then ultrasonicate at 150W. Add citric acid to adjust its pH to 4.5, and add pectinase to hydrolyze at 45℃ for 2h. After the enzymolysis is completed, pour the mixture into the essential oil extraction device, heat the water to boiling, and start timing for 2h from when liquid drips in the essential oil collector until no essential oil flows out. After cooling, collect the grapefruit peel essential oil crude oil (crude extract), dry it with anhydrous sodium sulfate to remove water, and store it in a dark environment at 4℃. The specific process is shown in Table 1.

[0061] Table 1 Preparation process of grapefruit peel essential oil crude oil

[0062] Example 1 Example 2 Example 3 Ultrasonic time / min 50 40 30 Pectinase addition amount / wt.% 1 2 3

[0063] 2. The edible alcohol solution was mixed with the grapefruit peel essential oil crude oil in a triangular flask according to the solid-liquid ratio shown in Table 2, sealed, stirred at room temperature for 60 minutes, and then the mixture was placed in a centrifuge and centrifuged at 6000 rpm for 8 minutes to separate the aqueous phase mixture (lower layer) and the oil phase mixture (upper layer), and stored in a dark environment at 4°C for standby use. The specific process is shown in Table 2.

[0064] Table 2 Preparation process of water / oil phase mixture

[0065] Example 1 Example 2 Example 3 Concentration of edible alcohol solution / % 40 50 50 Material-liquid ratio 1:2 1:1.5 1:1

[0066] 3. Pour the aqueous phase mixture and the oil phase mixture prepared in step 2 into the molecular distiller respectively, seal and incubate. Set the feed rate to 2mL / min, open the feed valve, set the evaporation temperature, distillation pressure, and scraper speed, and perform molecular distillation at condensed water temperatures of 0°C, -10°C, and -20°C. Collect the heavy phase fraction of the aqueous phase mixture, which is the water-soluble component, and collect the light phase fraction of the oil phase mixture, which is the fat-soluble component. The specific process is shown in Table 3.

[0067] Table 3 Preparation process of water / fat-soluble components

[0068] Example 1 Example 2 Example 3 Incubation temperature / ℃ 30 35 30 Incubation time / min 30 30 30 Evaporation temperature / ℃ 30 35 30 Distillation pressure / Pa 200 300 100 Scraper speed / rpm 200 250 200

[0069] Comparative Example 1: The difference from Example 1 is that only the solvent extraction method is used to treat the grapefruit peel essential oil crude oil. That is, after the aqueous phase mixed liquid (lower layer) and the oil phase mixed liquid (upper layer) are separated in step 2, no subsequent treatment is performed. The process parameters involved are set the same as in Example 1.

[0070] Comparative Example 2: The difference from Example 2 is that only molecular distillation is used to treat the grapefruit peel essential oil crude oil. That is, the grapefruit peel essential oil crude oil collected in step 1 is not subjected to solvent extraction (step 2), but directly subjected to molecular distillation (step 3), and the light phase fraction and the heavy phase fraction are collected. The process parameters involved are all set the same as in Example 2.

[0071] 2. Detection of water-soluble and fat-soluble components in grapefruit peel essential oil

[0072] Test method: When performing HS-SPME analysis, first add 5mL of distilled water and saturated sodium chloride to a 20mL headspace bottle, then add 20μL of sample and seal and preheat at 45℃ for 5min. Then, use DVB / CAR / PDMS three-phase coated extraction head to extract at 45℃ for 45min, and finally analyze at 250℃ for 5min. Gas chromatography (GC) analysis uses HP-5 capillary column, the injection port temperature is set to 250℃, helium is used as carrier gas, the flow rate is 0.8mL / min, and the analysis is carried out according to a specific heating program. The mass spectrometry (MS) conditions are set to electron bombardment ion source (EI), 70eV electron energy, ion source and interface temperature are 240℃ and 250℃ respectively, solvent delay is 2min, full scan mode is used, and the mass scan range is 33~600m / z. Qualitative and quantitative analysis is carried out by determining the retention index (RI) and comparing it with the NIST mass spectral library and literature data to identify the compounds, and the relative content of each component is calculated according to the peak area.

[0073] The distribution of terpene oxides and terpene contents in different samples of Example 1 and Comparative Examples 1 to 2 is as follows: Figure 1 As shown. Figure 1It can be seen that the proportions of terpene oxides and terpenes in the grapefruit peel essential oil crude oil are 8.21% and 87.15% respectively. The terpene oxide content of the water-soluble component prepared in Example 1 is as high as 77.49%, which is higher than the aqueous phase mixture of Comparative Example 1 (53.41%) and the heavy phase fraction (44.33%) in Comparative Example 2, and is also higher than the oxygen-containing compounds (72.91%) in the extraction kettle essential oil prepared by Patent CN116751633A. On the other hand, the terpene content in the fat-soluble component accounts for as high as 97.53%, which is also higher than the oil phase mixture of Comparative Example 1, the light phase fraction in Comparative Example 2 and Patent CN116751633A. The present invention can more effectively separate terpene oxides and terpenes from grapefruit peel essential oil crude oil, thereby improving the purity of the essential oil product.

[0074] The total ion currents of the components in the different samples of Example 2 are shown in FIG. Figure 2 As shown. Figure 2 It can be seen that the terpene compounds in the grapefruit peel essential oil crude oil, especially the relatively high (+)-limonene, myrcene and α-pinene, mainly complete the chromatographic peak within the time window of 17 to 26 minutes. In contrast, the peak time of terpene oxides is distributed in a wider range of 26 to 65 minutes. When the grapefruit peel essential oil is treated by the present invention, the peak intensity of (+)-limonene (peak time 25.10 minutes) in its water-soluble component is significantly reduced, while the peak intensity of the compound peaking after 26 minutes is enhanced. At the same time, in the fat-soluble component, compared with the grapefruit peel essential oil crude oil, the compounds after 26 minutes are not only weakened in peak intensity, but also significantly reduced in type. This result shows that the present invention can effectively enrich the terpenes and terpene oxides in the grapefruit peel essential oil crude oil into the fat-soluble component and the water-soluble component, respectively, and achieve effective separation of the two.

[0075] 3. Preparation of wine with grapefruit flavor using water-soluble components and fat-soluble components in grapefruit peel essential oil

[0076] Preparation method: 1) reducing the alcohol content of 65%vol light-fragrance liquor to 20-30%vol by diluting with water, adsorbing with activated carbon, and filtering to obtain low-alcohol liquor; 2) mixing the water-soluble component and the fat-soluble component in the grapefruit peel essential oil obtained in Example 3 in a ratio of 1-50:1-5 (w:w) to obtain a mixed essential oil component; 3) mixing and dissolving the mixed essential oil component and 65%vol light-fragrance liquor in a ratio of 1:100 (w:w) to obtain a mixed solution; 4) blending the low-alcohol liquor and the mixed solution in a ratio of 1:10 (w:w) to obtain a wine with grapefruit flavor.

[0077] Sensory evaluation test: 10 sensory panelists (3 males and 7 females) scored the grapefruit-flavored liquor based on appearance, smell, and taste. The results are shown in Table 4.

[0078] Table 4 Sensory evaluation results of grapefruit wine

[0079]

[0080] When the proportion of water-soluble components in grapefruit peel essential oil is too high, its unique grapefruit aroma is not obvious; and when the proportion of fat-soluble components is too high, the mixed solution has poor solubility in low-alcohol liquor, and sometimes even produces a numbing taste. However, when the water-soluble components and fat-soluble components are mixed in a ratio of 10:1 and added to low-alcohol liquor, the resulting wine has a clear and transparent texture without oily suspended matter, and the flavors of grapefruit, flower and sweet aroma are harmoniously unified. After drinking, the taste is mild and comfortable, without abnormal flavors, and the overall sensory evaluation reaches the highest. This result shows that water-soluble and fat-soluble components in grapefruit peel essential oil can be used to prepare grapefruit-flavored wine.

Claims

1. A method for refining water-soluble components and fat-soluble components in grapefruit peel essential oil, characterized in that: The steps include: A. Pomelo peel is mixed with water, crushed, ultrasonicated, and enzymatically treated, and then steam distilled to obtain pomelo peel essential oil crude oil; B. mixing the grapefruit peel essential oil crude oil and the extraction solvent, centrifuging and separating to obtain an upper aqueous phase mixed liquid and a lower oil phase mixed liquid; C. The aqueous phase mixture and the oil phase mixture are subjected to molecular distillation treatment respectively, and the heavy phase fraction of the aqueous phase mixture is collected as the water-soluble component of the grapefruit peel essential oil, and the light phase fraction of the oil phase mixture is collected as the fat-soluble component of the grapefruit peel essential oil.

2. The method for refining water-soluble components and fat-soluble components in grapefruit peel essential oil according to claim 1, characterized in that: In step A, at least one of the following must be met: Mix grapefruit peel and water in a mass ratio of 1:3-5; The ultrasonic treatment is specifically as follows: subjecting the crushed mixture to ultrasonic treatment at a power of 100 to 200 W for 30 to 50 minutes; The enzymatic hydrolysis treatment is specifically as follows: adjusting the pH of the mixture after ultrasound to 4-5 by food-grade citric acid or malic acid, and then adding 1-3% pectinase by mass of the mixture, and performing enzymatic hydrolysis at 40-50° C. for 2-4 hours; The steam distillation is specifically as follows: pouring the enzymatically hydrolyzed mixture into an essential oil extraction device, heating to boiling, collecting the distillate, and cooling.

3. The method for refining water-soluble components and fat-soluble components in grapefruit peel essential oil according to claim 1, characterized in that: In step B, at least one of the following is met: The solid-liquid ratio of the extraction solvent to the crude oil of grapefruit peel essential oil is 1:1-3; The extraction solvent is edible alcohol with a concentration of 30 to 60%; The centrifugal speed is 4000-8000 rpm and the time is 5-10 minutes.

4. The method for refining water-soluble components and fat-soluble components in grapefruit peel essential oil according to claim 1, characterized in that: In step C, the conditions for molecular distillation are: incubation temperature 25-35°C, evaporation temperature 25-35°C, distillation pressure 100-300 Pa, scraper speed 200-300 rpm, feed speed 1-5 mL / min, and condensed water temperatures are 0°C, -10°C, and -20°C, respectively.

5. The water-soluble component and / or fat-soluble component in the grapefruit peel essential oil obtained by the refining method according to any one of claims 1 to 4, characterized in that: The water-soluble components include, but are not limited to, terpene oxides such as nerol, L-carveol, D-carvone, (-)-4-terpineol, and linalool; the fat-soluble components include, but are not limited to, terpenes such as (+)-limonene, myrcene, and α-pinene.

6. A composition, characterized in that: The invention comprises the water-soluble components and / or fat-soluble components in the grapefruit peel essential oil obtained by the refining method according to any one of claims 1 to 4, or the water-soluble components and / or fat-soluble components in the grapefruit peel essential oil according to claim 5.

7. Use of the water-soluble components and / or fat-soluble components in the grapefruit peel essential oil obtained by the refining method according to any one of claims 1 to 4, or the water-soluble components and / or fat-soluble components in the grapefruit peel essential oil according to claim 5, or the composition according to claim 6 in the fields of food, beverages, cosmetics, and daily chemical products.

8. The use according to claim 7, characterized in that: The method of preparing a wine with grapefruit flavor by using water-soluble components and fat-soluble components in grapefruit peel essential oil specifically comprises the following steps: a. The highly fragrant liquor is diluted with water, adsorbed with activated carbon, and filtered to obtain a low-alcohol liquor; b. mixing the water-soluble components and fat-soluble components in the grapefruit peel essential oil to obtain a mixed essential oil component; c. The mixed essential oil component and the highly fragrant liquor are mixed to obtain a mixed solution; d. Mix the low-alcohol liquor and the mixed solution to obtain a liquor with a grapefruit flavor.

9. The use according to claim 8, characterized in that: At least one of the following is met: In step a, the alcohol content of the high-flavor liquor is 65% vol, and the alcohol content of the low-alcohol liquor is 20-30% vol; In step b, the water-soluble component and the fat-soluble component are mixed in a w:w ratio of 10 to 50:1; In step c, the mixed essential oil component and the highly fragrant liquor are mixed at a w:w ratio of 1:100; In step d, the low-alcohol liquor and the mixed solution are mixed in a w:w ratio of 1:

10.

10. The use according to claim 9, characterized in that: In step b, the water-soluble component and the fat-soluble component are mixed in a w:w ratio of 10:1.

Citation Information

Patent Citations

  • Fractional refining method and application of tangerine essential oil

    CN115386429A

  • Plant essential oil terpenoid removal process method and application thereof

    CN116751633A