Method for extracting geraniene B extract from bauhinia championii
By combining drying and supercritical CO2 extraction with molecular distillation of Bauhinia flowers, the problem of low extraction efficiency of geraniol B in existing technologies has been solved, achieving the extraction of high-content geraniol B and meeting the raw material needs of food additives, cosmetics and pharmaceuticals.
Patent Information
- Application Number
- CN202511176069.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-08-21
- Publication Date
- 2025-11-18
AI Technical Summary
Existing technologies make it difficult to efficiently extract geraniol B from natural sources, which limits its application in food additives, cosmetics, and pharmaceuticals.
A high-content extract of geraniol B was obtained by vacuum freeze-drying or constant temperature drying at normal pressure using dried Bauhinia flowers, combined with supercritical CO2 extraction and molecular distillation techniques.
The efficient extraction of geraniol B from Bauhinia flowers has been achieved, with the extract containing more than 50% geraniol B, meeting the raw material requirements for the preparation of geraniol B monomer.
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Abstract
Description
Technical Field
[0001] This application relates to the field of plant extraction technology, specifically to a method for extracting vetiverene B extract from Bauhinia flowers. Background Technology
[0002] Germacrene B is a naturally occurring sesquiterpene compound with unique aroma characteristics and bioactivity. It is widely found in various plants, especially aromatic and medicinal plants, such as Atractylodes lancea, Atractylodes macrocephala, Michelia champaca, and Michelia purpurea. In recent years, with the increasing demand for natural products, germacrene B has attracted much attention in the food additive, cosmetic, and pharmaceutical fields due to its various physiological functions, including antioxidant, anti-inflammatory, and antibacterial properties. Due to its complex molecular structure and low content, efficient extraction of germacrene B from natural sources has become a key technical challenge.
[0003] Analysis of the volatile oil components of Bauhinia purpurea revealed that geraniol B is one of the main components. Therefore, it is necessary to study the optimal extraction process of volatile components from Bauhinia purpurea to obtain a high content of geraniol B, thus providing high-quality raw materials for the extraction of geraniol B monomer. Summary of the Invention
[0004] This invention provides a method for extracting geraniol B extract from Bauhinia flowers. This method is simple to operate, safe, and has high extraction efficiency, effectively solving the technical problem of efficiently extracting geraniol B from natural sources.
[0005] To achieve the above objectives, the technical solution of the present invention is as follows: The method for extracting vetiverene B extract from Bauhinia flowers includes the following steps: A. After drying, Bauhinia flowers are crushed, they are subjected to supercritical CO2 extraction to obtain crude oil. B. The crude oil is subjected to molecular distillation to evaporate the water, and the remaining crude oil is separated into heavy oil and light oil. The light oil is the extract of geraniol B.
[0006] Preferably, in step A, the drying method for Bauhinia flowers is vacuum freeze-drying or constant temperature drying at normal pressure.
[0007] Preferably, the atmospheric pressure and constant temperature drying conditions are: drying at 50℃ or below for 24-48 hours.
[0008] Preferably, the vacuum freeze-drying process includes the following steps: Wash the fresh Bauhinia flowers with purified water, drain the water, and spread them evenly in a tray with a thickness of 6-8 cm. Perform vacuum freeze-drying on the tray containing the Bauhinia flowers according to the freeze-drying temperature control program with a vacuum degree of 10-30 Pa to obtain the freeze-dried Bauhinia. The freeze-drying temperature control program is as follows: Freeze-dry at -60℃ to -35℃ for 1-3 hours, then raise the temperature to -34℃ to -25℃ and dry for 0.7-1.3 hours, then raise the temperature to -24℃ to -15℃ and dry for 0.7-1.3 hours, then raise the temperature to -14℃ to -5℃ and dry for 0.7-1.3 hours, then raise the temperature to -4℃ to 5℃ and dry for 0.7-1.3 hours, then raise the temperature to 6℃ to 15℃ and dry for 1-3 hours, then raise the temperature to 16℃ to 25℃ and dry for 1-3 hours, then raise the temperature to 26℃ to 35℃ and dry for 1-3 hours, then raise the temperature to 36℃ to 45℃ and dry for 20-40 hours.
[0009] Preferably, in step A, after the Bauhinia flowers are pulverized, they are passed through a 10-30 mesh sieve and then subjected to supercritical CO2 extraction.
[0010] Preferably, in step A, the supercritical CO2 extraction conditions are as follows: Extraction pressure 300-500 bar, oil discharge valve temperature 70-90℃, fixed extraction temperature 45-60℃, extraction time 1-3 h, CO2 flow rate 10-20 mL / min.
[0011] Preferably, in step B, the crude oil molecular distillation is carried out using a scraped-film molecular distillation apparatus, and the molecular distillation conditions are as follows: Feed temperature: 50-70℃, condensation temperature: 8-13℃, distillation temperature: 70-85℃, vacuum degree: 1-3pa, scraping speed: 100-300r / min.
[0012] The light oil contains more than 50% geraniol B.
[0013] Geraniol B, the compound of this invention, is a naturally occurring sesquiterpene compound widely found in plants of the Apiaceae family. Its chemical structure contains multiple double bonds and cyclic structures, which contributes to its good stability and broad biological activity in nature. Geraniol B exhibits a wide range of biological activities, including anti-inflammatory, antioxidant, and antibacterial effects. Its anti-inflammatory effect is the most significant, particularly demonstrating a good alleviating effect in an arthritis model. Furthermore, its antioxidant properties help combat cell damage caused by oxidative stress. In the antibacterial field, it exhibits strong inhibitory activity against various pathogenic bacteria, making it a potential drug candidate molecule.
[0014] The advantages of this invention are as follows: This invention solves the problem of complex production processes for geraniol B in existing methods. Through a scientifically designed preparation method, high-content geraniol B volatile oil is extracted from Bauhinia flowers, serving as a high-quality raw material for preparing geraniol B monomer. The volatile oil extracted using this invention can contain over 50% geraniol B, and the volatile oil extracted using the optimal process can contain over 60% geraniol B. Attached Figure Description
[0015] Figure 1 Total ion chromatogram for the extraction of volatile oil from Bauhinia flowers by steam distillation; Figure 2 The total ion chromatogram for supercritical extraction of light oil in Example 5 is shown. Figure 3 The image shows the total ion chromatogram of supercritical extraction of light oil in Example 6. Detailed Implementation
[0016] The present invention will now be described in detail through specific embodiments. Example 1
[0017] The method for extracting geraniol B extract from Bauhinia flowers is as follows: A. After drying the Bauhinia flowers at normal pressure and constant temperature, crush them, pass them through a 10-mesh sieve, and then perform supercritical CO2 extraction to obtain crude oil. The drying conditions under normal pressure and constant temperature are: drying at 50℃ for 24 hours.
[0018] The supercritical CO2 extraction conditions are as follows: Extraction pressure 300 bar, oil drain valve temperature 70℃, fixed extraction temperature 45℃, extraction time 1 h, CO2 flow rate 10 mL / min.
[0019] B. The crude oil is subjected to molecular distillation to evaporate the water, and the remaining crude oil is separated into heavy oil and light oil. The light oil is the extract of geraniol B.
[0020] Crude oil molecular distillation was carried out using a scraped-film molecular distillation apparatus, and the molecular distillation conditions were as follows: Feed temperature: 5℃, condensation temperature: 8℃, distillation temperature: 70℃, vacuum degree: 1pa, scraping speed: 100r / min. Example 2
[0021] The method for extracting geraniol B extract from Bauhinia flowers is as follows: A. After drying the Bauhinia flowers at normal pressure and constant temperature, crush them, pass them through a 30-mesh sieve, and then perform supercritical CO2 extraction to obtain crude oil. The atmospheric pressure and constant temperature drying conditions are: drying at 40℃ for 48 hours.
[0022] The supercritical CO2 extraction conditions are as follows: Extraction pressure 500 bar, oil drain valve temperature 85℃, fixed extraction temperature 55℃, extraction time 1 h, CO2 flow rate 10 mL / min.
[0023] B. The crude oil is subjected to molecular distillation to evaporate the water, and the remaining crude oil is separated into heavy oil and light oil. The light oil is the extract of geraniol B.
[0024] Crude oil molecular distillation was carried out using a scraped-film molecular distillation apparatus, and the molecular distillation conditions were as follows: Feed temperature: 70℃, condensation temperature: 13℃, distillation temperature: 85℃, vacuum degree: 3pa, scraping speed: 300r / min. Example 3
[0025] The method for extracting geraniol B extract from Bauhinia flowers is as follows: A. After vacuum freeze-drying, the Bauhinia flowers are crushed, passed through a 20-mesh sieve, and then subjected to supercritical CO2 extraction to obtain crude oil. The vacuum freeze-drying process includes the following steps: Wash the fresh Bauhinia flowers with purified water, drain off the water, and spread them evenly in a tray with a thickness of 6 cm. The tray containing the Bauhinia flowers is then subjected to vacuum freeze-drying according to the freeze-drying temperature control program with a vacuum degree of 10 Pa to obtain the freeze-dried Bauhinia. The freeze-drying temperature control program is as follows: Freeze-dry at -60°C for 1 hour, then raise the temperature to -34°C and dry for 0.7 hours, then raise the temperature to -24°C and dry for 0.7 hours, then raise the temperature to -14°C and dry for 0.7 hours, then raise the temperature to -4°C and dry for 0.7 hours, then raise the temperature to 6°C and dry for 1 hour, then raise the temperature to 16°C and dry for 1 hour, then raise the temperature to 26°C and dry for 1 hour, then raise the temperature to 36°C and dry for 20 hours.
[0026] The supercritical CO2 extraction conditions are as follows: Extraction pressure 300 bar, oil drain valve temperature 70℃, fixed extraction temperature 45℃, extraction time 1 h, CO2 flow rate 10 mL / min.
[0027] B. The crude oil is subjected to molecular distillation to evaporate the water, and the remaining crude oil is separated into heavy oil and light oil. The light oil is the extract of geraniol B.
[0028] Crude oil molecular distillation was carried out using a scraped-film molecular distillation apparatus, and the molecular distillation conditions were as follows: Feed temperature: 60℃, condensation temperature: 10℃, distillation temperature: 75℃, vacuum degree: 2pa, scraping speed: 200r / min. Example 4
[0029] The method for extracting geraniol B extract from Bauhinia flowers is as follows: A. Take the vacuum freeze-dried Bauhinia flowers, crush them, sieve them through a 30-mesh sieve, and then perform supercritical CO2 extraction to obtain crude oil. The vacuum freeze-drying process includes the following steps: Wash the fresh Bauhinia flowers with purified water, drain the water, and spread them evenly in a tray with a thickness of 8cm. The tray containing the Bauhinia flowers is then subjected to vacuum freeze-drying according to the freeze-drying temperature control program at a vacuum degree of 30Pa to obtain the freeze-dried Bauhinia. The freeze-drying temperature control program is as follows: Freeze-dry at -35℃ for 3 hours, then raise the temperature to -25℃ and dry for 1.3 hours, then raise the temperature to -15℃ and dry for 1.3 hours, then raise the temperature to -5℃ and dry for 1.3 hours, then raise the temperature to 5℃ and dry for 1.3 hours, then raise the temperature to 15℃ and dry for 3 hours, then raise the temperature to 25℃ and dry for 3 hours, then raise the temperature to 35℃ and dry for 3 hours, then raise the temperature to 45℃ and dry for 40 hours.
[0030] The supercritical CO2 extraction conditions are as follows: Extraction pressure 500 bar, oil drain valve temperature 90℃, fixed extraction temperature 60℃, extraction time 3 h, CO2 flow rate 20 mL / min.
[0031] B. The crude oil is subjected to molecular distillation to evaporate the water, and the remaining crude oil is separated into heavy oil and light oil. The light oil is the extract of geraniol B.
[0032] Crude oil molecular distillation was carried out using a scraped-film molecular distillation apparatus, and the molecular distillation conditions were as follows: Feed temperature: 70℃, condensation temperature: 13℃, distillation temperature: 85℃, vacuum degree: 3pa, scraping speed: 300r / min. Example 5
[0033] The method for extracting geraniol B extract from Bauhinia flowers is as follows: A. After vacuum freeze-drying, the Bauhinia flowers are crushed, passed through a 20-mesh sieve, and then subjected to supercritical CO2 extraction to obtain crude oil. The vacuum freeze-drying process includes the following steps: Wash the fresh Bauhinia flowers with purified water, drain the water, and spread them evenly in a tray with a thickness of 7cm. The tray containing the Bauhinia flowers is then subjected to vacuum freeze-drying according to the freeze-drying temperature control program with a vacuum degree of 20Pa to obtain the freeze-dried Bauhinia. The freeze-drying temperature control program is as follows: Freeze-dry at -40℃ for 2 hours, then raise the temperature to -30℃ and dry for 1 hour, then raise the temperature to -20℃ and dry for 1 hour, then raise the temperature to -10℃ and dry for 1 hour, then raise the temperature to -0℃ and dry for 1 hour, then raise the temperature to 10℃ and dry for 2 hours, then raise the temperature to 20℃ and dry for 2 hours, then raise the temperature to 30℃ and dry for 2 hours, then raise the temperature to 35℃ and dry for 30 hours.
[0034] The supercritical CO2 extraction conditions are as follows: Extraction pressure 400 bar, oil drain valve temperature 80℃, fixed extraction temperature 50℃, extraction time 2 h, CO2 flow rate 15 mL / min.
[0035] B. The crude oil is subjected to molecular distillation to evaporate the water, and the remaining crude oil is separated into heavy oil and light oil. The light oil is the vetiverene B extract. The yield of light oil is 0.97%.
[0036] Crude oil molecular distillation was carried out using a scraped-film molecular distillation apparatus, and the molecular distillation conditions were as follows: Feed temperature: 60℃, condensation temperature: 10℃, distillation temperature: 80℃, vacuum degree: 22pa, scraping speed: 200r / min. Example 6
[0037] The method for extracting geraniol B extract from Bauhinia flowers is as follows: A. After drying the Bauhinia flowers at normal pressure and constant temperature, crush them, pass them through a 20-mesh sieve, and then perform supercritical CO2 extraction to obtain crude oil. The atmospheric pressure and constant temperature drying conditions are: drying at 45℃ for 48 hours.
[0038] The supercritical CO2 extraction conditions are as follows: Extraction pressure 400 bar, oil drain valve temperature 80℃, fixed extraction temperature 50℃, extraction time 2 h, CO2 flow rate 15 mL / min.
[0039] B. The crude oil is subjected to molecular distillation to evaporate the water, and the remaining crude oil is separated into heavy oil and light oil. The light oil is the geraniol B extract. The yield of light oil is 0.80%.
[0040] Crude oil molecular distillation was carried out using a scraped-film molecular distillation apparatus, and the molecular distillation conditions were as follows: Feed temperature: 60℃, condensation temperature: 10℃, distillation temperature: 80℃, vacuum degree: 22pa, scraping speed: 200r / min.
[0041] Example 7 Determination of the percentage of geraniol B in geraniol I. Instruments and Apparatus 7890B Gas Chromatograph - 5977B MSD Mass Spectrometer (Agilent Technologies); BSA224S-CW Electronic Analytical Balance (Sartorius). II. Reagents Anhydrous ethanol (Chengdu Kelong Chemical Co., Ltd.) III. Chromatographic Conditions Gas chromatography conditions: Column: Agilent HP-5ms (30 m x 250 μm x 0.25 μm), injection port temperature: 250℃, carrier gas: high-purity helium, column flow rate: 1 ml / min, split ratio: 200:1, injection volume: 1 μl, temperature program: initial temperature 50℃, hold for 5 min, increase to 130℃ at a rate of 10℃ / min, hold for 15 min, then increase to 250℃ at a rate of 10℃ / min, hold for 5 min.
[0042] Mass spectrometry conditions: Ionization method: EI; Electron energy: 70 eV; Interface temperature: 250 °C; Ion source temperature: 230 °C Quadrupole temperature: 150℃, solvent delay: 3.5min, scan range: 35~550amu.
[0043] IV. Preparation of Comparative Samples Steam distillation method: Weigh 1500g of fresh Bauhinia flowers, add 4500ml of drinking water, juice and break the cell wall, transfer the flower residue and juice to a 10L round-bottom flask, heat to boiling, keep simmering for about 6 hours, collect 1500ml of aromatic water for later use; transfer the aromatic water to a 2L round-bottom flask for redistillation, the distillation time is about 3 hours, collect the volatile oil.
[0044] V. Sample Preparation Weigh 0.1 g of the volatile oil from the comparative example, and 0.1 g of the light oil prepared in Examples 5 and 6 respectively. Place each in a 5 ml volumetric flask, dissolve and dilute to the mark with anhydrous ethanol, and filter through a 0.22 μm microporous membrane. Take 1 μl of each and inject directly for analysis.
[0045] VI. Test Results The above experimental steps were followed to obtain... Figure 1 Total ion chromatogram of volatile oil extracted from Bauhinia flowers by steam distillation. Figure 2 Example 5: Total ion chromatogram of supercritical extraction of light oil. Figure 3 Example 6: Total ion chromatogram of supercritical extraction of light oil. In the figure, the retention time of geraniol B is 26.216 min.
[0046] The test results show that: The content of geraniol B in the water-extracted Bauhinia flower volatile oil was 38.16%. Example 5: The content of geraniol B in the light oil extracted by supercritical extraction was 53.31%; In Example 6, the content of geraniol B in the light oil extracted by supercritical extraction was 60.04%.
[0047] The extraction results show that the content of geraniol B in the light oil obtained after drying and supercritical extraction of Bauhinia flowers and subsequent molecular distillation is significantly higher than that in the volatile oil prepared by traditional steam distillation.
[0048] Freeze-dried Bauhinia flowers, when further processed using supercritical carbon dioxide extraction and molecular distillation techniques, can more fully extract volatile substances from Bauhinia flowers and maintain their biological activity. The content of geraniol B in the light oil extracted from Bauhinia flowers is also significantly better than that of samples dried at constant temperature and low temperature and then processed using supercritical carbon dioxide extraction and molecular distillation techniques.
Claims
1. A method for extracting geraniol B extract from Bauhinia flowers, characterized in that, Includes the following steps: A. After drying, Bauhinia flowers are crushed, they are subjected to supercritical CO2 extraction to obtain crude oil. B. The crude oil is subjected to molecular distillation to evaporate the water, and the remaining crude oil is separated into heavy oil and light oil. The light oil is the extract of geraniol B.
2. The method for extracting vetiverene B extract from Bauhinia flowers according to claim 1, characterized in that: In step A, the drying method for Bauhinia flowers is vacuum freeze-drying or constant temperature drying at normal pressure.
3. The method for extracting geraniol B extract from Bauhinia flowers according to claim 2, characterized in that, The aforementioned constant temperature and atmospheric pressure drying conditions are: drying at 50℃ or below for 24-48 hours.
4. The method for extracting geraniol B extract from Bauhinia flowers according to claim 2, characterized in that, The vacuum freeze-drying process includes the following steps: Wash the fresh Bauhinia flowers with purified water, drain the water, and spread them evenly in a tray with a thickness of 6-8 cm. Perform vacuum freeze-drying on the tray containing the Bauhinia flowers according to the freeze-drying temperature control program with a vacuum degree of 10-30 Pa to obtain the freeze-dried Bauhinia. The freeze-drying temperature control program is as follows: Freeze-dry at -60℃ to -35℃ for 1-3 hours, then raise the temperature to -34℃ to -25℃ and dry for 0.7-1.3 hours, then raise the temperature to -24℃ to -15℃ and dry for 0.7-1.3 hours, then raise the temperature to -14℃ to -5℃ and dry for 0.7-1.3 hours, then raise the temperature to -4℃ to 5℃ and dry for 0.7-1.3 hours, then raise the temperature to 6℃ to 15℃ and dry for 1-3 hours, then raise the temperature to 16℃ to 25℃ and dry for 1-3 hours, then raise the temperature to 26℃ to 35℃ and dry for 1-3 hours, then raise the temperature to 36℃ to 45℃ and dry for 20-40 hours.
5. The method for extracting vetiverene B extract from Bauhinia flowers according to claim 1, characterized in that: In step A, the Bauhinia flowers are pulverized, passed through a 10-30 mesh sieve, and then subjected to supercritical CO2 extraction.
6. The method for extracting vetiverene B extract from Bauhinia flowers according to claim 1, characterized in that: In step A, the supercritical CO2 extraction conditions are as follows: Extraction pressure 300-500 bar, oil discharge valve temperature 70-90℃, fixed extraction temperature 45-60℃, extraction time 1-3 h, CO2 flow rate 10-20 mL / min.
7. The method for extracting vetiverene B extract from Bauhinia flowers according to claim 1, characterized in that: In step B, the crude oil molecular distillation is carried out using a scraped-film molecular distillation apparatus, and the molecular distillation conditions are as follows: Feed temperature: 50-70℃, condensation temperature: 8-13℃, distillation temperature: 70-85℃, vacuum degree: 1-3pa, scraping speed: 100-300r / min.
8. The method for extracting geraniol B extract from Bauhinia flowers according to claim 1, characterized in that: The light oil contains more than 50% geraniol B.