Preparation method of refined rose extracting solution

Abstract

The invention relates to the technical field of rose extraction, in particular to a preparation method of a refined rose extracting solution, which comprises the following steps: step 1, uniformly laying rose petals on an active adsorbent; step 2, injecting deionized water into the distiller, heating to boiling, and enabling distillate to flow into an oil-water separator; 3, collecting an oil layer, and recording the oil layer as a component A; step 4, dipping the distilled rose petals and an active adsorbent; step 5, extracting oil-soluble components in the active adsorbent; step 6, extracting a component B; step 7, fully mixing the component A and the component B; according to the preparation method of the refined rose extracting solution, provided by the invention, the rose essential oil is prepared by combining a steam distillation method and an extraction method, the rose essential oil prepared by the method retains a large amount of non-volatile components, the quality of the rose essential oil can be effectively improved, and the method is relatively low in energy consumption and suitable for large-scale popularization and application.

Description

Technical Field

[0001] The present invention relates to the technical field of rose extraction, in particular to a method for preparing a refined rose extract. Background Art

[0002] Rose is a perennial, evergreen or deciduous shrub of the genus Rosa in the Rosaceae family. Its main product, rose essential oil, is an extremely valuable essential oil, known as "liquid gold." Rose essential oil possesses numerous benefits, including antioxidant, antibacterial, cell regeneration, and emotional soothing properties. It holds broad application and development potential in the cosmetics, food, and pharmaceutical industries. Rose essential oil is a complex mixture composed of hundreds of naturally occurring compounds, including trace components whose structures have yet to be determined. The unique fragrance and remarkable efficacy of natural rose essential oil are the result of the synergistic effect of these organic molecules, fully embodying the magical charm of nature's creation and exceeding the potential of synthetic methods. It is well known that extraction and processing techniques are the most critical factors affecting the quality of rose essential oil.

[0003] At present, the extraction methods of rose essential oil mainly include traditional extraction methods such as steam distillation, pressing, organic solvent extraction, as well as modern extraction processes such as supercritical CO2 extraction, molecular distillation purification technology, subcritical water extraction technology (SWE) and microwave distillation extraction.

[0004] To date, steam distillation is a common process for producing rose essential oil. Rose essential oil produced by steam distillation contains almost no non-volatile components. Non-volatile components include: long-chain fatty acids such as stearic acid, oleic acid, and linoleic acid, as well as waxes such as triacontanes, flavonoids, polyphenols, vitamin E, β-carotene, etc. The lack of these non-volatile components will reduce the moisturizing and repairing function of the essential oil, and the antioxidant properties of the essential oil will decrease.

[0005] Therefore, we proposed a preparation method of a refined rose extract to solve the above problems. Summary of the Invention

[0006] The purpose of the present invention is to solve the shortcomings of the prior art and to propose a method for preparing a refined rose extract.

[0007] A method for preparing a refined rose extract comprises the following steps:

[0008] Step 1: Wash the rose petals with deionized water, drain the surface moisture of the rose petals, then lay a layer of filter cloth on the sieve plate of the distiller, and lay a layer of active adsorbent on the filter cloth, and finally evenly lay the rose petals on the active adsorbent;

[0009] Step 2: Pour deionized water into the distiller, keep the water level in the distiller below the sieve plate, heat the deionized water to boiling, and then maintain the water temperature at 95-99°C. Continue distillation for 1.5-3 hours. The distillate is condensed in the condenser and flows into the oil-water separator.

[0010] Step 3: The distillate is allowed to stand for 30-60 minutes until the oil-water separation is complete, and the oil layer is collected and recorded as component A;

[0011] Step 4: Place the distilled rose petals and the active adsorbent in deionized water and soak for 1-2 hours. After the soaking, separate the active adsorbent from the rose petals through a sieve;

[0012] Step 5: drying the adsorbent. After drying, placing the active adsorbent into an organic solvent for extraction to extract the oil-soluble components in the active adsorbent;

[0013] Step 6: Separate the organic solvent from the active adsorbent, evaporate the organic solvent, and collect the remaining component, which is recorded as component B;

[0014] Step 7: Fully mix component A and component B to obtain a refined rose extract.

[0015] Preferably, the active adsorbent is prepared from rose petals as raw materials.

[0016] Preferably, the preparation method of the active adsorbent comprises the following steps: firstly subjecting rose petals to a porous treatment to remove volatile components and water-soluble components in the rose petals, then freeze-drying the rose petals after the porous treatment, placing the freeze-dried rose petals in a high-temperature furnace, maintaining the temperature at 450-500° C. in a nitrogen atmosphere, heat treating for 30-60 minutes, cooling, grinding into powder, and then soaking in hydrogen peroxide for 10-15 minutes. After soaking, filtering, washing, and drying to obtain the active adsorbent.

[0017] Preferably, the specific steps of performing pore-forming treatment on rose petals are as follows: washing the rose petals, boiling them in boiling water for 15-60 minutes, filtering them while they are hot, washing them, and drying them to obtain the product.

[0018] Preferably, the specific steps of performing pore-forming treatment on rose petals are as follows: washing and drying the rose petals in step 4 to obtain the pore-forming rose petals.

[0019] Preferably, the mass ratio of the rose petals to hydrogen peroxide is 1:0.1-0.4.

[0020] Preferably, in step 1, the thickness of the rose petals is controlled to be 10-15 cm, and the mass ratio of the rose petals to the active adsorbent is 1:0.05-0.2.

[0021] Preferably, in step 2, the mass ratio of rose petals to deionized water is 1:4-6.

[0022] Preferably, in step 2, when the oil yield in the distillate is lower than 0.03%, the distillation end point is reached and the distillation is stopped.

[0023] Preferably, in step 5, the organic solvent is one of petroleum ether, ethyl ether, n-hexane, dichloromethane and ethanol, and the extraction time is 1-2 hours.

[0024] The beneficial effects of the present invention are:

[0025] 1. The method for preparing a refined rose extract proposed in the present invention adopts a combination of steam distillation and extraction to prepare rose essential oil. Compared with the traditional steam distillation method for preparing rose essential oil, the rose essential oil prepared by this method retains a large amount of non-volatile components, can effectively improve the quality of rose essential oil, and has low energy consumption, making it suitable for large-scale promotion and use.

[0026] 2. The method for preparing the refined rose extract proposed by the present invention comprises the following steps: during the distillation process, rose petals are evenly spread on an active adsorbent. During the distillation process, a small amount of non-volatile components can be adsorbed by the active adsorbent, thereby improving the subsequent extraction efficiency.

[0027] 3. The method for preparing the refined rose extract proposed in the present invention comprises placing distilled rose petals and an active adsorbent in deionized water for immersion, then drying the adsorbent, and extracting the adsorbent with an organic solvent. During the extraction process, the organic solvent does not contact the rose petals, thereby preventing some impurities in the rose petals from entering the essential oil and affecting the product quality.

[0028] 4. In the preparation method of the refined rose extract proposed by the present invention, the organic solvent only extracts the non-volatile components, so that the final essential oil extract does not contain solvent impurities and the quality of the essential oil is high.

[0029] 5. The present invention proposes a method for preparing a refined rose extract, using rose petals as the starting material to prepare an active adsorbent. The prepared active adsorbent has abundant pores inside, and the pores are well compatible with non-volatile components and have good selectivity. During the preparation process, the active adsorbent is activated with hydrogen peroxide to increase its surface acidic groups, effectively improving the adsorption performance of the active adsorbent for organic matter. DETAILED DESCRIPTION

[0030] The present invention will be further explained below with reference to specific embodiments.

[0031] In the following examples, the experimental methods or test methods, unless otherwise specified, are conventional methods; reagents and materials, unless otherwise specified, are obtained from conventional commercial channels or prepared by conventional methods, among which: organic solvents were purchased from Shanghai Nanmu Chemical Co., Ltd.; hydrogen peroxide was purchased from Shanghai Haotian Industrial Co., Ltd.; the activated carbon in Comparative Example 2 was 5 mm columnar activated carbon, purchased from Liyang Zhucai Environmental Protection Technology Co., Ltd.

[0032] Pick the fully opened rose petals between 8:30 and 9:30 in the morning.

[0033] A method for preparing a refined rose extract comprises the following steps:

[0034] Step 1: Wash the rose petals with deionized water, drain the surface moisture of the rose petals, then lay a layer of filter cloth on the sieve plate of the distiller, and lay a layer of active adsorbent on the filter cloth, and finally evenly lay the rose petals on the active adsorbent;

[0035] Step 2: Pour deionized water into the distiller, keep the water level in the distiller below the sieve plate, heat the deionized water to boiling, and then maintain the water temperature at 95-99°C. Continue distillation for 1.5-3 hours. The distillate is condensed in the condenser and flows into the oil-water separator.

[0036] Step 3: The distillate is allowed to stand for 30-60 minutes until the oil-water separation is complete, and the oil layer is collected and recorded as component A;

[0037] Step 4: Place the distilled rose petals and the active adsorbent in deionized water and soak for 1-2 hours. After the soaking, separate the active adsorbent from the rose petals through a sieve;

[0038] Step 5, drying the adsorbent, and after drying, placing the active adsorbent into an organic solvent for extraction to extract the oil-soluble components in the active adsorbent, wherein the organic solvent is one of petroleum ether, ether, n-hexane, dichloromethane and ethanol;

[0039] Step 6: Separate the organic solvent from the active adsorbent, evaporate the organic solvent, and collect the remaining component, which is recorded as component B;

[0040] Step 7: Fully mix component A and component B to obtain a refined rose extract.

[0041] In Example 1,

[0042] In step 1, the thickness of the rose petals is controlled at 10 cm, and the mass ratio of the rose petals to the active adsorbent is 1:0.05.

[0043] In step 2, the mass ratio of rose petals to deionized water is 1:4, the water temperature is maintained at 95° C., and distillation is continued for 1.5 hours. When the oil yield in the distillate decreases to 0.02%, the distillation is stopped.

[0044] Step 3: Let the distillate stand for 30 minutes.

[0045] Step 4: Place the distilled rose petals and the active adsorbent in deionized water and soak for 1 hour.

[0046] In step 5, the organic solvent is petroleum ether, and the extraction time is 1 hour.

[0047] The active adsorbent is prepared from rose petals as raw materials. The preparation method of the active adsorbent comprises the following steps: firstly performing a pore treatment on the rose petals to remove volatile components and water-soluble components in the rose petals, then freeze-drying the rose petals after the pore treatment, placing the freeze-dried rose petals in a high-temperature furnace, maintaining the temperature at 450°C in a nitrogen atmosphere, heat-treating for 30 minutes, cooling, grinding into powder, and then soaking in hydrogen peroxide for 10 minutes. After soaking, filtering, washing, and drying to obtain the active adsorbent.

[0048] The specific steps of performing pore-forming treatment on rose petals are as follows: washing and drying the rose petals in step 4 to obtain the pore-forming treatment.

[0049] The mass ratio of rose petals to hydrogen peroxide is 1:0.1.

[0050] In Example 2,

[0051] In step 1, the thickness of the rose petals is controlled at 15 cm, and the mass ratio of the rose petals to the active adsorbent is 1:0.2.

[0052] In step 2, the mass ratio of rose petals to deionized water is 1:6, the water temperature is maintained at 99° C., and distillation is continued for 3 hours. When the oil yield in the distillate decreases to 0.03%, the distillation is stopped.

[0053] Step 3: let the distillate stand for 60 minutes.

[0054] Step 4: Place the distilled rose petals and the active adsorbent in deionized water and soak for 2 hours.

[0055] In step 5, the organic solvent is diethyl ether, and the extraction time is 2 hours.

[0056] The active adsorbent is prepared from rose petals as raw materials.

[0057] The preparation method of the active adsorbent comprises the following steps: firstly performing a porous treatment on rose petals to remove volatile components and water-soluble components in the rose petals, then freeze-drying the rose petals after the porous treatment, placing the freeze-dried rose petals in a high-temperature furnace, maintaining the temperature at 500°C in a nitrogen atmosphere, heat treating for 60 minutes, cooling, grinding into powder, and then soaking in hydrogen peroxide for 15 minutes. After soaking, filtering, washing, and drying, the active adsorbent is obtained.

[0058] The specific steps of performing pore-forming treatment on rose petals are as follows: washing and drying the rose petals in step 4 to obtain the pore-forming treatment.

[0059] The mass ratio of rose petals to hydrogen peroxide is 1:0.4.

[0060] In Example 3,

[0061] In step 1, the thickness of the rose petals is controlled at 12 cm, and the mass ratio of the rose petals to the active adsorbent is 1:0.1.

[0062] In step 2, the mass ratio of rose petals to deionized water is 1:5, the water temperature is maintained at 98° C., and distillation is continued for 2 hours. When the oil yield in the distillate decreases to 0.025%, the distillation is stopped.

[0063] Step 3: Let the distillate stand for 45 minutes.

[0064] Step 4: Place the distilled rose petals and the active adsorbent in deionized water and soak for 1.5 hours.

[0065] In step 5, the organic solvent is n-hexane, and the extraction time is 1.5 hours.

[0066] The active adsorbent is prepared from rose petals as raw materials.

[0067] The preparation method of the active adsorbent includes the following steps: firstly performing a pore treatment on rose petals to remove volatile components and water-soluble components in the rose petals, then freeze-drying the rose petals after the pore treatment, placing the freeze-dried rose petals in a high-temperature furnace, maintaining the temperature at 480°C in a nitrogen atmosphere, and heat treating for 45 minutes. After cooling, the rose petals are ground into powder, and then soaked in hydrogen peroxide for 12 minutes. After soaking, the active adsorbent is obtained after filtering, washing, and drying.

[0068] The specific steps of performing pore-forming treatment on rose petals are as follows: washing and drying the rose petals in step 4 to obtain the pore-forming treatment.

[0069] The mass ratio of rose petals to hydrogen peroxide is 1:0.3.

[0070] In Example 4, compared with Example 3, the specific steps of the pore-opening treatment of rose petals are different. The specific steps of the pore-opening treatment of rose petals are as follows: wash the rose petals, place them in boiling water and steam them for 15 minutes, filter them while they are hot, wash them and dry them to obtain.

[0071] In Example 5, compared with Example 3, the specific steps of the pore-opening treatment of rose petals are different. The specific steps of the pore-opening treatment of rose petals are as follows: after washing the rose petals, placing them in boiling water and steaming them for 60 minutes, filtering them while hot, washing and drying them to obtain.

[0072] Compared with Example 3, Comparative Example 1 only includes steps 1 to 3, and the rest is the same as Example 3.

[0073] In Comparative Example 2, compared with Example 3, an equal mass of activated carbon was used to replace the active adsorbent, and the rest of the steps were the same as those in Example 3.

[0074] In Comparative Example 3, the following steps were adopted:

[0075] Step 1: Wash the rose petals with deionized water, drain the moisture from the surface of the rose petals, then lay a layer of filter cloth on the sieve plate of the distiller, and evenly spread the rose petals on the filter cloth;

[0076] Step 2: Pour deionized water into the distiller, keep the water level in the distiller below the sieve plate, heat the deionized water to boiling, and then maintain the water temperature at 98°C for 2 hours. The distillate is condensed in the condenser and flows into the oil-water separator.

[0077] Step 3: The distillate was allowed to stand for 45 minutes until the oil-water separation was complete, and the oil layer was collected and recorded as component A;

[0078] Step 4: drying the distilled rose petals. After drying, the rose petals are placed in an organic solvent for extraction to extract the oil-soluble components in the active adsorbent;

[0079] Step 5, separating the organic solvent from the rose petals, evaporating the organic solvent, and collecting the remaining component, which is recorded as component B;

[0080] Step 6: Fully mix component A and component B to obtain a refined rose extract.

[0081] In step 1, the thickness of the rose petals is controlled at 12 cm.

[0082] In step 2, the mass ratio of rose petals to deionized water is 1:5, and the distillation is stopped when the oil yield in the distillate decreases to 0.025%.

[0083] In step 4, the organic solvent is n-hexane, and the extraction time is 1.5 hours.

[0084] In Comparative Example 4, the following steps were adopted:

[0085] Step 1: Wash the rose petals with deionized water, drain the surface moisture of the rose petals, then lay a layer of filter cloth on the sieve plate of the distiller, and lay a layer of active adsorbent on the filter cloth, and finally evenly lay the rose petals on the active adsorbent;

[0086] Step 2: Pour deionized water into the distiller, keep the water level in the distiller below the sieve plate, heat the deionized water to boiling, and then maintain the water temperature at 98°C for 2 hours. The distillate is condensed in the condenser and flows into the oil-water separator.

[0087] Step 3: The distillate was allowed to stand for 45 minutes until the oil-water separation was complete, and the oil layer was collected and recorded as component A;

[0088] Step 4: Separate the active adsorbent from the rose petals through a sieve;

[0089] Step 5: drying the adsorbent. After drying, placing the active adsorbent into an organic solvent for extraction to extract the oil-soluble components in the active adsorbent;

[0090] Step 6: Separate the organic solvent from the active adsorbent, evaporate the organic solvent, and collect the remaining component, which is recorded as component B;

[0091] Step 7: Fully mix component A and component B to obtain a refined rose extract.

[0092] In step 1, the thickness of the rose petals is controlled at 12 cm, and the mass ratio of the rose petals to the active adsorbent is 1:0.1.

[0093] In step 2, the mass ratio of rose petals to deionized water is 1:5, and the distillation is stopped when the oil yield in the distillate decreases to 0.025%.

[0094] Step 4: Place the distilled rose petals and the active adsorbent in deionized water and soak for 1.5 hours.

[0095] In step 5, the organic solvent is n-hexane, and the extraction time is 1.5 hours.

[0096] The yield and color of the rose essential oil obtained in Examples 1-5 and Comparative Examples 1-4 were compared. 200 kg of Centifolia rose was used for extraction. The extraction rate and color of the rose essential oil are shown in Table 1.

[0097] Table 1

[0098]

[0099] As can be seen from Table 1, Examples 1-5 achieved high rose essential oil extraction rates (above 0.058%), and the essential oils exhibited a pure and rich aroma. Comparative Example 1, which did not include an extraction step, contained almost no non-volatile components in its essential oil, resulting in a significantly lower rose essential oil extraction rate. Comparative Example 2, in which an equal mass of activated carbon was used in place of the activated adsorbent, resulted in a slightly lower rose essential oil extraction rate than that of Example 3. In Comparative Example 3, in which no activated adsorbent was added and the organic solvent and rose petals were directly extracted, a small amount of impurities were incorporated during the extraction process, resulting in incomplete extraction and a lower rose essential oil extraction rate than that of Comparative Example 1. In Comparative Example 4, in which the activated adsorbent and the rose petals were not immersed in deionized water, the quality of the resulting rose essential oil was higher than that of Comparative Example 1, indicating that the activated adsorbent had already absorbed a small amount of non-volatile components during the distillation process.

[0100] The above description is only a preferred specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any technician familiar with the technical field, within the technical scope disclosed by the present invention, who makes equivalent replacements or changes based on the technical solution and inventive concept of the present invention, should be covered by the scope of protection of the present invention.

Claims

1. A method for preparing a refined rose extract, characterized in that: The following steps are involved: Step 1: Wash the rose petals with deionized water, drain the surface moisture of the rose petals, then lay a layer of filter cloth on the sieve plate of the distiller, and lay a layer of active adsorbent on the filter cloth, and finally evenly lay the rose petals on the active adsorbent; Step 2: Pour deionized water into the distiller, keep the water level in the distiller below the sieve plate, heat the deionized water to boiling, and then maintain the water temperature at 95-99°C. Continue distillation for 1.5-3 hours. The distillate is condensed in the condenser and flows into the oil-water separator. Step 3: The distillate is allowed to stand for 30-60 minutes until the oil-water separation is complete, and the oil layer is collected and recorded as component A; Step 4: Place the distilled rose petals and the active adsorbent in deionized water and soak for 1-2 hours. After the soaking, separate the active adsorbent from the rose petals through a sieve; Step 5: drying the adsorbent. After drying, placing the active adsorbent into an organic solvent for extraction to extract the oil-soluble components in the active adsorbent; Step 6: Separate the organic solvent from the active adsorbent, evaporate the organic solvent, and collect the remaining component, which is recorded as component B; Step 7: Fully mix component A and component B to obtain a refined rose extract.

2. The method for preparing a refined rose extract according to claim 1, characterized in that: The active adsorbent is prepared by using rose petals as raw materials.

3. The method for preparing a refined rose extract according to claim 2, characterized in that: The preparation method of the active adsorbent comprises the following steps: firstly performing a porous treatment on rose petals to remove volatile components and water-soluble components in the rose petals, then freeze-drying the rose petals after the porous treatment, placing the freeze-dried rose petals in a high-temperature furnace, maintaining the temperature at 450-500° C. under a nitrogen atmosphere, heat treating the rose petals for 30-60 minutes, cooling the petals, grinding the petals into powder, and then soaking them in hydrogen peroxide for 10-15 minutes. After the soaking is complete, filtering, washing, and drying the petals to obtain the active adsorbent.

4. The method for preparing a refined rose extract according to claim 3, characterized in that: The specific steps of making pores of rose petals are as follows: wash the rose petals, place them in boiling water and steam for 15-60 minutes, filter them while they are hot, wash them and dry them to obtain the pores.

5. The method for preparing a refined rose extract according to claim 3, characterized in that: The specific steps of performing pore-forming treatment on rose petals are as follows: washing and drying the rose petals in step 4 to obtain the pore-forming treatment.

6. The method for preparing a refined rose extract according to claim 4 or 5, characterized in that: The mass ratio of the rose petals to the hydrogen peroxide is 1:0.1-0.

4.

7. The method for preparing a refined rose extract according to claim 6, characterized in that: In step 1, the thickness of the rose petals is controlled to be 10-15 cm, and the mass ratio of the rose petals to the active adsorbent is 1:0.05-0.

2.

8. The method for preparing a refined rose extract according to claim 6, characterized in that: In step 2, the mass ratio of rose petals to deionized water is 1:4-6.

9. The method for preparing a refined rose extract according to claim 6, characterized in that: In the step 2, when the oil yield in the distillate is lower than 0.03%, the distillation end point is reached and the distillation is stopped.

10. The method for preparing a refined rose extract according to claim 6, characterized in that: In step 5, the organic solvent is one of petroleum ether, ethyl ether, n-hexane, dichloromethane and ethanol, and the extraction time is 1-2 hours.

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