Preparation method of non-chemically reproducible euphorbia lathyris (gufu) essential oil

Abstract

This invention discloses a method for preparing wild jujube (Gnaphalium affine) essential oil that cannot be chemically replicated, belonging to the field of natural plant essential oil extraction technology. The method includes whole-plant cleaning pretreatment, low-temperature slicing, low-temperature fine crushing, low-pressure fractional distillation, graded condensation collection of aromatic fractions, separation, low-temperature aging, and filtration steps. This invention, through low-temperature slicing and fine crushing pretreatment combined with low-pressure fractional distillation at 0.02–0.08 MPa and no higher than 45°C, along with gradient condensation and low-temperature aging at 2–8°C, maximizes the preservation of natural synergistic trace components in the wild jujube essential oil. In gas chromatography-mass spectrometry (GC-MS) analysis, the obtained essential oil exhibits a characteristic aroma component retention rate ≥90% and contains at least three undisclosed natural synergistic trace components, whose aroma and activity cannot be completely replicated through chemical flavoring. This invention's process is mild and efficient, suitable for large-scale production, and provides a high-value-added pathway for the deep processing of wild jujube.

Description

Technical Field

[0001] This invention relates to the field of natural plant essential oil extraction technology, specifically to a method for preparing wild radish (ground fruit) essential oil that cannot be chemically replicated. Background Technology

[0002] Wild ground melon (also known as ground fruit) is a wild economic plant belonging to the genus Ficus of the Moraceae family. It is widely distributed in southwestern my country. Its plants and fruits have a unique and rich fruity and herbal aroma, and it has extremely high development value in the fields of daily chemical fragrances, food additives, and pharmaceutical intermediates.

[0003] Most plant essential oils on the market are extracted using high-temperature steam distillation. Although this method is simple, the high temperature can easily cause the heat-sensitive aroma components in wild radish essential oil to decompose and oxidize, resulting in aroma distortion and loss of active ingredients.

[0004] Furthermore, chemically synthesized fragrances can only mimic a single or a few main aroma components, failing to replicate the complex natural synergistic trace component system of wild radish essential oil. This results in significant deficiencies in the aroma complexity and bioactivity of the products. Therefore, developing a feasible method for preparing essential oils that fully preserves the natural characteristics of wild radish is of great practical importance. Summary of the Invention

[0005] The purpose of this invention is to overcome the defects of existing technologies, such as high-temperature extraction leading to component destruction and the inability of chemical fragrances to replicate natural characteristics, and to provide a method for preparing wild gourd (ground fruit) essential oil that cannot be chemically replicated.

[0006] This invention is achieved through the following technical solution: a method for preparing wild jujube (ground fruit) essential oil that cannot be chemically replicated, comprising the following steps: (1) The whole plant of wild ground melon (ground fruit) is cleaned and pretreated by rinsing with clean water and air drying at low temperature to remove surface impurities and residual moisture; (2) Low temperature slicing: The pretreated wild melon plant is sliced ​​into uniform thin slices with a thickness of 1-3 mm at 0-10℃ to avoid loss of heat-sensitive components. (3) Low-temperature fine crushing: further crush the slices to 20-60 mesh particles to increase the specific surface area and improve distillation efficiency; (4) Low-pressure fractional distillation: Under conditions of 0.02 to 0.08 MPa and no higher than 45°C, distillation is carried out in three temperature ranges to collect different fractions. (5) Collect the aroma-rich fraction by staged condensation. Collect the top note, middle note and base note fractions by condensation in two or more stages, and combine them to obtain the crude aroma-rich essential oil. (6) Separation, low-temperature aging, and filtration: After centrifugation, the crude aromatic essential oil is aged at 2-8℃ for 7-15 days and then filtered through 0.22μm micropores to obtain high-fidelity natural essential oil.

[0007] Preferably, the three temperature ranges of the low-pressure fractional distillation are 25–30°C, 32–38°C, and 40–45°C, respectively.

[0008] Preferably, the gradient temperatures of the staged condensation are 10-15℃ (top notes), 0-5℃ (body notes), and -5-0℃ (base notes).

[0009] The present invention also protects the wild jujube (ground fruit) essential oil prepared by the above method. Because the essential oil contains natural synergistic trace components unique to wild jujube, its aroma and activity cannot be completely replicated by chemical fragrance blending. In gas chromatography-mass spectrometry (GC-MS) analysis, the retention rate of characteristic aroma components is ≥90%, and it contains at least 3 undisclosed natural synergistic trace components. Beneficial effects

[0010] This invention employs a combined pretreatment process of low-temperature slicing and low-temperature fine crushing, which makes the material particle size uniform. Compared with traditional direct crushing, it effectively avoids the volatilization of aroma components caused by local overheating, while increasing the specific surface area of ​​the material, thus making the distillation mass transfer more complete.

[0011] The entire process employs a low-pressure fractional distillation process at a temperature not exceeding 45℃, which effectively protects the heat-sensitive and easily oxidized components in wild radish essential oil, ensuring the natural quality of the essential oil.

[0012] The top, middle, and base aroma fractions are collected in stages by gradient condensation and combined with low-temperature aging treatment, which allows the natural synergistic trace components in the essential oil to fully integrate, forming aroma characteristics and biological activities that cannot be replicated by chemical fragrances.

[0013] The process steps of this invention are clear, the parameters are well-defined, and the equipment requirements are moderate. It is suitable for both large-scale industrial production and deep processing and transformation by small and medium-sized enterprises and planting bases, and has broad application prospects. Detailed Implementation

[0014] The present invention will be further described in detail below with reference to specific embodiments, but the scope of protection of the present invention is not limited to the following embodiments. Example

[0015] (1) Take 10kg of fresh wild melon whole plant, rinse it 3 times with running water to remove soil and impurities, and then place it in a 4℃ environment to air dry until there is no visible moisture on the surface. (2) At a low temperature of 5℃, use a slicer to cut the whole wild melon plant into uniform thin slices with a thickness of 2mm; (3) Use a low-temperature pulverizer to further pulverize the flakes into 40-mesh particles; (4) The finely crushed material is put into a vacuum distillation kettle, and the vacuum degree is controlled at 0.05MPa for fractional distillation: the first stage is heated to 28℃ to collect the top aroma fraction, the second stage is heated to 35℃ to collect the body aroma fraction, and the third stage is heated to 42℃ to collect the base aroma fraction. (5) The steam obtained from distillation is sequentially passed into a three-stage condenser for gradient condensation: the temperature of the first-stage condenser is controlled at 12℃ to collect the top aroma, the temperature of the second-stage condenser is controlled at 2℃ to collect the body aroma, and the temperature of the third-stage condenser is controlled at -3℃ to collect the base aroma. The three-stage fractions are combined to obtain a crude product of rich aroma essential oil. (6) Place the crude product of the aroma essential oil in a centrifuge and centrifuge at 3000 rpm for 10 minutes to remove moisture and impurities. Then transfer it to a cold storage at 4℃ for aging for 10 days. Finally, filter it through a 0.22μm microporous membrane to obtain the finished product of wild jujube natural essential oil.

[0016] Gas chromatography-mass spectrometry (GC-MS) analysis showed that the retention rate of characteristic aroma components in the essential oil obtained in this embodiment was 92%, and three natural synergistic trace components not disclosed in the prior art were detected. According to professional perfumers, the essential oil has a rich and layered aroma with a strong natural feel, and cannot be completely replicated using existing chemical fragrance formulations. Example

[0017] (1) Take 5 kg of fresh wild melon whole plant, rinse twice with running water, and then air dry in an environment of 5℃; (2) Under a low temperature of 0℃, the whole wild melon plant was cut into uniform thin slices with a thickness of 1mm; (3) Crush the thin slices into 20-mesh particles; (4) Control the vacuum degree to 0.02MPa and carry out fractional distillation, collecting different fractions at 25℃, 32℃ and 40℃ respectively; (5) Gradient condensation is carried out through a two-stage condenser, and the fractions are collected at 15℃ and 0℃ respectively, and combined to obtain crude product; (6) After centrifugation, the product is aged in a cold storage at 2℃ for 7 days and then filtered through a 0.22μm microporous membrane to obtain the finished product.

[0018] Tests showed that the retention rate of characteristic aroma components was over 90%, and it also contained at least three undisclosed natural synergistic trace components.

Claims

1. A method for preparing wild radish (ground fruit) essential oil that cannot be chemically replicated, characterized in that, Includes the following steps: (1) The whole plant of wild ground melon (ground fruit) is cleaned and pretreated by rinsing with clean water and air drying at low temperature to remove surface impurities and residual moisture; (2) Low temperature slicing: The pretreated wild melon plant is sliced ​​into uniform thin slices with a thickness of 1-3 mm at 0-10℃ to avoid loss of heat-sensitive components. (3) Low-temperature fine crushing: further crush the slices to 20-60 mesh particles to increase the specific surface area and improve distillation efficiency; (4) Low-pressure fractional distillation: Under conditions of 0.02~0.08 MPa and no higher than 45℃, distillation is carried out in three temperature ranges to collect different fractions. (5) Collect the aroma-rich fraction by graded condensation. Collect the top, middle, and base aroma fractions separately by graded condensation of two or more stages, and combine them to obtain the crude aroma-rich essential oil. (6) Separation and low-temperature aging filtration: After centrifugation, the crude essential oil is aged at 2~8℃ for 7~15 days and then filtered through 0.22μm micropores to obtain high-fidelity natural essential oil.

2. The method according to claim 1, characterized in that, The three temperature ranges for the low-pressure fractional distillation are 25~30℃, 32~38℃, and 40~45℃, respectively.

3. The method according to claim 1, characterized in that, The gradient temperatures of the staged condensation are 10~15℃ for top notes, 0~5℃ for body notes, and -5~0℃ for base notes.

4. The method according to claim 1, characterized in that, Because the essential oil contains natural synergistic trace components unique to wild jujube, its aroma and activity cannot be completely replicated by chemical fragrance blending.

5. A wild gourd (ground fruit) essential oil prepared by the method according to any one of claims 1 to 3, characterized in that, The essential oil, when analyzed by gas chromatography-mass spectrometry (GC-MS), exhibited a retention rate of ≥90% for characteristic aroma components and contained at least three undisclosed natural synergistic trace components.