CN113862083A - Method for improving oil yield and quality of rosa damascena essential oil - Google Patents
Method for improving oil yield and quality of rosa damascena essential oil Download PDFInfo
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- CN113862083A CN113862083A CN202111171418.5A CN202111171418A CN113862083A CN 113862083 A CN113862083 A CN 113862083A CN 202111171418 A CN202111171418 A CN 202111171418A CN 113862083 A CN113862083 A CN 113862083A
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
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Abstract
The invention provides a method for improving the oil yield and quality of Damascus rose essential oil, and relates to the technical field of rose essential oil production. A method for improving the oil yield and quality of Damascus rose essential oil is characterized by comprising the following steps: s1: picking up fresh rosa damascena flowers, cleaning, crushing, and carrying out enzymolysis by using enzymolysis liquid to obtain fresh flower raw pulp; s2: freezing fresh flower primary pulp into ice blocks; s3: carrying out first-stage vacuum condensation extraction on ice blocks frozen with fresh flower primary pulp, and then carrying out second-stage vacuum condensation extraction to obtain fresh flower primary liquid; s4: performing three-stage circulating oil-water separation treatment on the flower stock solution, and collecting to obtain crude Damascus rose essential oil; s5: filtering, dehydrating and aging the crude Damascus rose essential oil to obtain a Damascus rose essential oil product. The invention can also extract essential oil from the Damascus rose without distillation and extraction, thereby reducing the damage to aromatic substances, improving the oil yield of the rose essential oil and ensuring high quality of the rose essential oil.
Description
Technical Field
The invention relates to the technical field of rose essential oil production, in particular to a method for improving the oil yield and quality of Damascus rose essential oil.
Background
Roses are deciduous shrubs of the genus Rosa of the family Rosaceae, and rose essential oil extracted from petals thereof concentrates various aromatic substances in flowers. The rose essential oil is widely used in the fields of pharmacy, health care, edible essence, high-grade perfume, tobacco essence and the like; the rose essential oil has small molecules, is convenient for human body to absorb, soothes liver, activates blood circulation and induces resuscitation with fragrance, contains 38.8 mug/Kg of selenium element, and has the effects of preventing and resisting cancer and delaying senility.
At present, the method for extracting the rose essential oil comprises the following steps: distillation and extraction processes; the distillation method is used for production at a high temperature, the process energy consumption is large, aromatic substances are damaged, and the oil yield is low; the extraction method has high requirement on production safety coefficient, the process is complex, and the obtained rose essential oil is impure and has low quality.
Disclosure of Invention
The invention aims to provide a method for improving the oil yield and quality of essential oil of Damascus roses, which can extract the essential oil of Damascus roses without distillation and extraction, reduce damage to aromatic substances, improve the oil yield of the essential oil of the roses and improve the quality of the essential oil of the roses.
The embodiment of the invention is realized by the following technical scheme:
a method for improving the oil yield and quality of Damascus rose essential oil comprises the following steps:
s1: picking up fresh rosa damascena flowers, cleaning, crushing, and carrying out enzymolysis by using enzymolysis liquid to obtain fresh flower raw pulp;
s2: freezing fresh flower primary pulp into ice blocks;
s3: carrying out first-stage vacuum condensation extraction on ice blocks frozen with fresh flower primary pulp for 2-4 h to obtain first-stage fresh flower stock solution, carrying out second-stage vacuum condensation extraction for 0.5-1.5 h to obtain second-stage fresh flower stock solution, and mixing the first-stage fresh flower stock solution and the second-stage fresh flower stock solution to obtain fresh flower stock solution;
s4: performing three-stage circulating oil-water separation treatment on the flower stock solution obtained by extraction, and collecting to obtain crude Damascus rose essential oil;
s5: and filtering, dehydrating and aging the collected crude Damascus rose essential oil to obtain a Damascus rose essential oil product.
Further, the enzymolysis liquid in the step S1 is a mixed liquid of plant decomposition enzyme and cellulase, the adding amount of the plant decomposition enzyme is 0.1-0.3% of the total weight of the rosa damascena flowers, and the adding amount of the cellulase is 0.04-0.06% of the total weight of the rosa damascena flowers.
Further, in the step S2, the fresh flower puree is frozen at-55 to-45 ℃ for 2 to 4 hours, and the thickness of the frozen ice blocks is not more than 3 cm.
Further, in the first stage of the step S3, a vacuum extraction tank is used for heating to 25-35 ℃, the vacuum pressure is-0.09-0.095 Mpa, and a capillary low-temperature condensing device is used for condensing at the temperature of-55-50 ℃ to obtain the first-stage fresh flower stock solution.
Further, in the step S3, the second stage vacuum extraction tank is heated to 40-50 ℃, the vacuum pressure is-0.09 to-0.095 Mpa, and the temperature is controlled to be-55 to-50 ℃ by using a capillary low-temperature condensing device to condense to obtain the second stage flower stock solution.
Further, in the step S3, the first stage flower stock solution and the second stage flower stock solution are mixed and heated at 30 to 35 ℃ to obtain a flower stock solution.
Further, in the step S4, the heating temperature of the primary oil-water separation is 38-42 ℃, the vibration frequency of the oil-water separator is controlled to be 4-6 Hz, the discharging temperature of the material liquid after the oil-water separation is 26-30 ℃, the crude essential oil is collected, and the separated liquid is subjected to secondary oil-water separation; the heating temperature of the second-stage oil-water separation is 42-46 ℃, the vibration frequency of the oil-water separator is controlled to be 8-12 Hz, the discharging temperature of the material liquid after the oil-water separation is 31-35 ℃, the crude essential oil is collected, and the separated liquid is subjected to third-stage oil-water separation; and the heating temperature of the three-stage oil-water separation is 46-50 ℃, the vibration frequency of the oil-water separator is controlled to be 14-16 Hz, the discharging temperature of the material liquid after the oil-water separation is 36-40 ℃, the crude essential oil is collected, and the separated liquid flows back into the flower stock solution.
Further, in the step S4, the flower stock solution is subjected to three-stage circulating oil-water separation and repeated circulation for 2-3 hours.
Further, the crude Damascus rose essential oil obtained in the step S5 is filtered, dehydrated and aged at 2-8 ℃ for 8-9 weeks.
The technical scheme of the embodiment of the invention at least has the following advantages and beneficial effects:
1. the method does not use distillation and extraction, the overall temperature is controlled to be not more than 50 ℃, the damage to the aromatic substances of the rose essential oil can be effectively reduced, the aromatic substance content of the rose essential oil is improved, and the quality of the rose essential oil is ensured.
2. The method does not use distillation and extraction, uses enzymolysis liquid for enzymolysis and crushing by a crusher, can improve the oil yield of the subsequent rose essential oil, and quickly freezes at low temperature, thereby reducing the loss of aromatic substances, improving the aromatic substance content of the rose essential oil and ensuring the quality of the rose essential oil.
3. The rose essential oil extraction method can effectively improve the oil yield of the rose essential oil by two-stage heating vacuum extraction.
4. Through three-stage circulating oil-water separation treatment, the volatilization, waste and loss of the rose essential oil can be avoided, and the oil yield of the rose essential oil is effectively improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The method for improving the oil yield and quality of Rosa damascena essential oil provided by the embodiment of the invention is specifically described below.
Example 1
The embodiment provides a method for improving the oil yield and quality of Damascus rose essential oil, which comprises the following steps:
s1: picking up half-opened fresh Damascus rose flowers before 8 o' clock in the morning, cleaning, crushing, performing enzymolysis by using mixed enzymolysis liquid of plant decomposition enzyme and cellulase to obtain fresh flower primary pulp, wherein the addition amount of the plant decomposition enzyme is 0.1% of the total weight of the Damascus rose flowers, and the addition amount of the cellulase is 0.06% of the total weight of the Damascus rose flowers;
s2: freezing fresh flower puree at-45 deg.C for 4h to obtain ice block with thickness not more than 3 cm;
s3: heating an ice block with frozen fresh flower puree to 25 ℃ in a first stage by using a vacuum extraction tank, wherein the vacuum pressure is-0.09 Mpa, the temperature of a capillary low-temperature condensing device is controlled to be-50 ℃, vacuum condensation is carried out for 4 hours to obtain fresh flower stock solution in the first stage, then, the ice block is heated to 40 ℃ in a second stage by using the vacuum extraction tank, the vacuum pressure is-0.09 Mpa, the temperature of the capillary low-temperature condensing device is controlled to be-50 ℃, vacuum condensation is carried out for 1.5 hours to obtain fresh flower stock solution in the second stage, the fresh flower stock solution in the first stage and the fresh flower stock solution in the second stage are mixed, and the mixture is heated at 30 ℃ to obtain fresh flower stock solution;
s4: carrying out three-stage circulating oil-water separation treatment on the flower stock solution obtained by extraction for 2 h; the heating temperature of the first-stage oil-water separation is 38 ℃, the vibration frequency of the oil-water separator is controlled to be 4Hz, the discharging temperature of the material liquid after the oil-water separation is 26 ℃, the crude essential oil is collected, and the separated liquid is subjected to second-stage oil-water separation; the heating temperature of the second-stage oil-water separation is 46 ℃, the vibration frequency of the oil-water separator is controlled to be 8Hz, the discharging temperature of the material liquid after the oil-water separation is 31 ℃, the crude essential oil is collected, and the separated liquid is subjected to third-stage oil-water separation; the three-stage oil-water separation heating temperature is 50 ℃, the vibration frequency of the oil-water separator is controlled to be 14Hz, the discharging temperature of the material liquid after oil-water separation is 36 ℃, crude and essential oil is collected, and the separated liquid flows back into the flower stock solution; mixing the crude essential oil collected in the third stage to obtain crude Damascus rose essential oil;
s5: and filtering, dehydrating and aging the collected crude Damascus rose essential oil at 2 ℃ for 8 weeks to obtain a Damascus rose essential oil product.
Example 2
The embodiment provides a method for improving the oil yield and quality of Damascus rose essential oil, which comprises the following steps:
s1: picking up half-opened fresh Damascus rose flowers before 8 o' clock in the morning, cleaning, crushing, performing enzymolysis by using mixed enzymolysis liquid of plant decomposition enzyme and cellulase to obtain fresh flower primary pulp, wherein the addition amount of the plant decomposition enzyme is 0.3% of the total weight of the Damascus rose flowers, and the addition amount of the cellulase is 0.04% of the total weight of the Damascus rose flowers;
s2: freezing fresh flower puree at-55 deg.C for 2h to obtain ice block with thickness not more than 3 cm;
s3: heating the ice cake with fresh flower protoplasm at 35 deg.C under-0.095 Mpa in the first stage by using vacuum extraction tank, controlling the temperature to-55 deg.C by using capillary low-temperature condensing device, vacuum condensing for 2 hr to obtain fresh flower stock solution in the first stage, heating to 50 deg.C under-0.095 Mpa in the second stage by using vacuum extraction tank, vacuum condensing for 0.5 hr at-55 deg.C by using capillary low-temperature condensing device to obtain fresh flower stock solution in the second stage, mixing the fresh flower stock solution in the first stage and the fresh flower stock solution in the second stage, and heating at 35 deg.C to obtain fresh flower stock solution;
s4: carrying out three-stage circulating oil-water separation treatment on the flower stock solution obtained by extraction for 3 h; the heating temperature of the first-stage oil-water separation is 42 ℃, the vibration frequency of the oil-water separator is controlled to be 6Hz, the discharging temperature of the material liquid after the oil-water separation is 30 ℃, the crude essential oil is collected, and the separated liquid is subjected to second-stage oil-water separation; the heating temperature of the second-stage oil-water separation is 46 ℃, the vibration frequency of the oil-water separator is controlled to be 12Hz, the discharging temperature of the material liquid after the oil-water separation is 35 ℃, the crude essential oil is collected, and the separated liquid is subjected to third-stage oil-water separation; the three-stage oil-water separation heating temperature is 50 ℃, the vibration frequency of the oil-water separator is controlled to be 16Hz, the discharging temperature of the material liquid after oil-water separation is 40 ℃, crude essential oil is collected, and the separated liquid flows back into the flower stock solution; mixing the crude essential oil collected in the third stage to obtain crude Damascus rose essential oil;
s5: and filtering, dehydrating and aging the collected crude Damascus rose essential oil at 8 ℃ for 9 weeks to obtain a Damascus rose essential oil product.
Example 3
The embodiment provides a method for improving the oil yield and quality of Damascus rose essential oil, which comprises the following steps:
s1: picking up half-opened fresh Damascus rose flowers before 8 o' clock in the morning, cleaning, crushing, performing enzymolysis by using mixed enzymolysis liquid of plant decomposition enzyme and cellulase to obtain fresh flower primary pulp, wherein the addition amount of the plant decomposition enzyme is 0.2% of the total weight of the Damascus rose flowers, and the addition amount of the cellulase is 0.05% of the total weight of the Damascus rose flowers;
s2: freezing fresh flower puree at-50 deg.C for 3h to obtain ice block with thickness not more than 3 cm;
s3: heating an ice block with frozen fresh flower puree to 30 ℃ by using a vacuum extraction tank at a first stage, wherein the vacuum pressure is-0.09 Mpa, the temperature of a capillary low-temperature condensation device is controlled to be-52 ℃, vacuum condensation is carried out for 3 hours to obtain fresh flower stock solution at the first stage, then heating the ice block to 45 ℃ by using the vacuum extraction tank at a second stage, wherein the vacuum pressure is-0.09 Mpa, the temperature of the capillary low-temperature condensation device is controlled to be-52 ℃, vacuum condensation is carried out for 1 hour to obtain fresh flower stock solution at the second stage, mixing the fresh flower stock solution at the first stage and the fresh flower stock solution at the second stage, and heating the mixture at 32 ℃ to obtain the fresh flower stock solution;
s4: carrying out three-stage circulating oil-water separation treatment on the flower stock solution obtained by extraction for repeated circulation for 2.5 h; the heating temperature of the first-stage oil-water separation is 40 ℃, the vibration frequency of the oil-water separator is controlled to be 5Hz, the discharging temperature of the material liquid after the oil-water separation is 28 ℃, the crude essential oil is collected, and the separated liquid is subjected to second-stage oil-water separation; the heating temperature of the second-stage oil-water separation is 45 ℃, the vibration frequency of the oil-water separator is controlled to be 10Hz, the discharging temperature of the material liquid after the oil-water separation is 32 ℃, the crude essential oil is collected, and the separated liquid is subjected to third-stage oil-water separation; the three-stage oil-water separation heating temperature is 48 ℃, the vibration frequency of the oil-water separator is controlled to be 15Hz, the discharging temperature of the material liquid after oil-water separation is 38 ℃, crude essential oil is collected, and the separated liquid flows back into the flower stock solution; mixing the crude essential oil collected in the third stage to obtain crude Damascus rose essential oil;
s5: and filtering, dehydrating and aging the collected crude Damascus rose essential oil at 4 ℃ for 9 weeks to obtain a Damascus rose essential oil product.
Example 4
The embodiment provides a method for improving the oil yield and quality of Damascus rose essential oil, which comprises the following steps:
s1: picking up half-opened fresh Damascus rose flowers before 8 o' clock in the morning, cleaning, crushing, performing enzymolysis by using mixed enzymolysis liquid of plant decomposition enzyme and cellulase to obtain fresh flower primary pulp, wherein the addition amount of the plant decomposition enzyme is 0.3% of the total weight of the Damascus rose flowers, and the addition amount of the cellulase is 0.06% of the total weight of the Damascus rose flowers;
s2: freezing fresh flower puree at-55 deg.C for 4h to obtain ice blocks with thickness not more than 3 cm;
s3: heating an ice block with frozen fresh flower puree to 28 ℃ in a first stage by using a vacuum extraction tank, wherein the vacuum pressure is-0.095 Mpa, the temperature of a capillary low-temperature condensation device is controlled to be-55 ℃, vacuum condensation extraction is carried out for 2h to obtain fresh flower stock solution in the first stage, then heating the ice block with the vacuum extraction tank to 46 ℃ in a second stage, wherein the temperature of the capillary low-temperature condensation device is controlled to be-50 ℃, vacuum condensation extraction is carried out for 1.5h to obtain fresh flower stock solution in the second stage, mixing the fresh flower stock solution in the first stage and the fresh flower stock solution in the second stage, and heating the mixture at 35 ℃ to obtain fresh flower stock solution;
s4: carrying out three-stage circulating oil-water separation treatment on the flower stock solution obtained by extraction for 2 h; the heating temperature of the first-stage oil-water separation is 38 ℃, the vibration frequency of the oil-water separator is controlled to be 4Hz, the discharging temperature of the material liquid after the oil-water separation is 28 ℃, the crude essential oil is collected, and the separated liquid is subjected to second-stage oil-water separation; the heating temperature of the second-stage oil-water separation is 45 ℃, the vibration frequency of the oil-water separator is controlled to be 12Hz, the discharging temperature of the material liquid after the oil-water separation is 31 ℃, the crude essential oil is collected, and the separated liquid is subjected to third-stage oil-water separation; the three-stage oil-water separation heating temperature is 50 ℃, the vibration frequency of the oil-water separator is controlled to be 15Hz, the discharging temperature of the material liquid after oil-water separation is 38 ℃, crude essential oil is collected, and the separated liquid flows back into the flower stock solution; mixing the crude essential oil collected in the third stage to obtain crude Damascus rose essential oil;
s5: filtering the collected crude Damascus rose essential oil, dehydrating, and aging at 6 deg.C for 8 weeks to obtain Damascus rose essential oil product.
Comparative example 1
The comparative example provides an extraction method of essential oil of rosa damascena, which comprises the following steps:
picking up fresh Damascus rose flowers in half-opened mode before 8 o' clock in the morning, cleaning, adding water, distilling to form oil-water mixed steam at 95-100 ℃, cooling at 40 ℃ to obtain distillate, standing the distillate, performing oil-water separation, and collecting to obtain Damascus rose essential oil.
Comparative example 2
The comparative example provides an extraction method of essential oil of rosa damascena, which comprises the following steps:
picking up half-opened fresh Rosa damascena flowers before 8 am in the morning, cleaning, extracting with petroleum ether, and separating to obtain Rosa damascena essential oil.
Comparative example 3
The comparative example provides an extraction method of essential oil of rosa damascena, which comprises the following steps:
s1: picking up half-opened fresh Damascus rose flowers before 8 o' clock in the morning, cleaning, crushing, performing enzymolysis by using mixed enzymolysis liquid of plant decomposition enzyme and cellulase to obtain fresh flower primary pulp, wherein the addition amount of the plant decomposition enzyme is 0.1% of the total weight of the Damascus rose flowers, and the addition amount of the cellulase is 0.06% of the total weight of the Damascus rose flowers;
s2: heating flower protoplasm in a first stage by using a vacuum extraction tank at 25 ℃, vacuum pressure of-0.09 Mpa, controlling the temperature by using a capillary low-temperature condensing device at-50 ℃, carrying out vacuum condensation extraction for 4h to obtain flower primary liquid in the first stage, then carrying out a second stage by using the vacuum extraction tank at 40 ℃, vacuum pressure of-0.09 Mpa, controlling the temperature by using the capillary low-temperature condensing device at-50 ℃, carrying out vacuum condensation extraction for 1.5h to obtain flower primary liquid in the second stage, mixing the flower primary liquid in the first stage and the flower primary liquid in the second stage, and heating at 30 ℃ to obtain the flower primary liquid;
s4: carrying out three-stage circulating oil-water separation treatment on the flower stock solution obtained by extraction for 2 h; the heating temperature of the first-stage oil-water separation is 38 ℃, the vibration frequency of the oil-water separator is controlled to be 4Hz, the discharging temperature of the material liquid after the oil-water separation is 26 ℃, the crude essential oil is collected, and the separated liquid is subjected to second-stage oil-water separation; the heating temperature of the second-stage oil-water separation is 46 ℃, the vibration frequency of the oil-water separator is controlled to be 8Hz, the discharging temperature of the material liquid after the oil-water separation is 31 ℃, the crude essential oil is collected, and the separated liquid is subjected to third-stage oil-water separation; the three-stage oil-water separation heating temperature is 50 ℃, the vibration frequency of the oil-water separator is controlled to be 14Hz, the discharging temperature of the material liquid after oil-water separation is 36 ℃, crude and essential oil is collected, and the separated liquid flows back into the flower stock solution; mixing the crude essential oil collected in the third stage to obtain crude Damascus rose essential oil;
s5: and filtering, dehydrating and aging the collected crude Damascus rose essential oil at 2 ℃ for 8 weeks to obtain a Damascus rose essential oil product.
Comparative example 4
The comparative example provides an extraction method of essential oil of rosa damascena, which comprises the following steps:
s1: picking up half-opened fresh rosa damascena flowers before 8 am in the morning, cleaning and soaking in water;
s2: heating rose soaked in water at 30 deg.C under-0.09 Mpa in vacuum extraction tank at the first stage, vacuum condensing at-50 deg.C for 3 hr to obtain first stage flower stock solution, heating at 40 deg.C under-0.09 Mpa in vacuum extraction tank at-50 deg.C in vacuum condensation extraction tank at the second stage to obtain second stage flower stock solution, mixing the first and second stage flower stock solutions, and heating at 30 deg.C to obtain flower stock solution;
s4: carrying out three-stage circulating oil-water separation treatment on the flower stock solution obtained by extraction for 2 h; the heating temperature of the first-stage oil-water separation is 38 ℃, the vibration frequency of the oil-water separator is controlled to be 4Hz, the discharging temperature of the material liquid after the oil-water separation is 26 ℃, the crude essential oil is collected, and the separated liquid is subjected to second-stage oil-water separation; the heating temperature of the second-stage oil-water separation is 46 ℃, the vibration frequency of the oil-water separator is controlled to be 8Hz, the discharging temperature of the material liquid after the oil-water separation is 31 ℃, the crude essential oil is collected, and the separated liquid is subjected to third-stage oil-water separation; the three-stage oil-water separation heating temperature is 50 ℃, the vibration frequency of the oil-water separator is controlled to be 14Hz, the discharging temperature of the material liquid after oil-water separation is 36 ℃, crude and essential oil is collected, and the separated liquid flows back into the flower stock solution; mixing the crude essential oil collected in the third stage to obtain crude Damascus rose essential oil;
s5: and filtering, dehydrating and aging the collected crude Damascus rose essential oil at 2 ℃ for 8 weeks to obtain a Damascus rose essential oil product.
Comparative example 5
The comparative example provides an extraction method of essential oil of rosa damascena, which comprises the following steps:
s1: picking up half-opened fresh Damascus rose flowers before 8 o' clock in the morning, cleaning, crushing, performing enzymolysis by using mixed enzymolysis liquid of plant decomposition enzyme and cellulase to obtain fresh flower primary pulp, wherein the addition amount of the plant decomposition enzyme is 0.3% of the total weight of the Damascus rose flowers, and the addition amount of the cellulase is 0.04% of the total weight of the Damascus rose flowers;
s2: freezing fresh flower puree at-55 deg.C for 2h to obtain ice block with thickness not more than 3 cm;
s3: heating ice block of frozen fresh flower primary pulp with vacuum extraction tank at 50 deg.C under-0.095 Mpa, and vacuum condensing with capillary low-temperature condensing device at-55 deg.C for 2 hr to obtain fresh flower stock solution;
s4: carrying out three-stage circulating oil-water separation treatment on the flower stock solution obtained by extraction for 3 h; the heating temperature of the first-stage oil-water separation is 42 ℃, the vibration frequency of the oil-water separator is controlled to be 6Hz, the discharging temperature of the material liquid after the oil-water separation is 30 ℃, the crude essential oil is collected, and the separated liquid is subjected to second-stage oil-water separation; the heating temperature of the second-stage oil-water separation is 46 ℃, the vibration frequency of the oil-water separator is controlled to be 12Hz, the discharging temperature of the material liquid after the oil-water separation is 35 ℃, the crude essential oil is collected, and the separated liquid is subjected to third-stage oil-water separation; the three-stage oil-water separation heating temperature is 50 ℃, the vibration frequency of the oil-water separator is controlled to be 16Hz, the discharging temperature of the material liquid after oil-water separation is 40 ℃, crude essential oil is collected, and the separated liquid flows back into the flower stock solution; mixing the crude essential oil collected in the third stage to obtain crude Damascus rose essential oil;
s5: and filtering, dehydrating and aging the collected crude Damascus rose essential oil at 8 ℃ for 9 weeks to obtain a Damascus rose essential oil product.
Comparative example 6
The comparative example provides an extraction method of essential oil of rosa damascena, which comprises the following steps:
s1: picking up half-opened fresh Damascus rose flowers before 8 o' clock in the morning, cleaning, crushing, performing enzymolysis by using mixed enzymolysis liquid of plant decomposition enzyme and cellulase to obtain fresh flower primary pulp, wherein the addition amount of the plant decomposition enzyme is 0.2% of the total weight of the Damascus rose flowers, and the addition amount of the cellulase is 0.05% of the total weight of the Damascus rose flowers;
s2: freezing fresh flower puree at-50 deg.C for 3h to obtain ice block with thickness not more than 3 cm;
s3: heating an ice block with frozen fresh flower puree to 30 ℃ by using a vacuum extraction tank at a first stage, wherein the vacuum pressure is-0.09 Mpa, the temperature of a capillary low-temperature condensation device is controlled to be-52 ℃, vacuum condensation is carried out for 3 hours to obtain fresh flower stock solution at the first stage, then heating the ice block to 45 ℃ by using the vacuum extraction tank at a second stage, wherein the vacuum pressure is-0.09 Mpa, the temperature of the capillary low-temperature condensation device is controlled to be-52 ℃, vacuum condensation is carried out for 1 hour to obtain fresh flower stock solution at the second stage, mixing the fresh flower stock solution at the first stage and the fresh flower stock solution at the second stage, and heating the mixture at 32 ℃ to obtain the fresh flower stock solution;
s4: standing the flower stock solution obtained by extraction, performing oil-water separation, and collecting to obtain crude Damascus rose essential oil;
s5: and filtering, dehydrating and aging the collected crude Damascus rose essential oil at 4 ℃ for 9 weeks to obtain a Damascus rose essential oil product.
Experimental example 1
The essential oil of the Damascus roses is prepared by the methods of examples 1-4 and comparative examples 1-6, the oil yield of each group is calculated respectively, three parallel experiments are set for each group, and the average oil yield of each group is calculated, and the results are shown in Table 1.
Oil yield (%). oil mass (Kg)/total mass of Damascus rose flowers (Kg). 100%
TABLE 1 average oil yield
As can be seen from Table 1, the oil yield of the essential oil of Damascus roses prepared by the method is improved compared with that of the essential oil of Damascus roses prepared by a comparative method; comparative example 1 a distillation method was used; comparative example 2 solvent extraction was used; comparative example 3 the fresh flower puree is directly extracted in vacuum without being frozen into ice blocks; comparative example 4 without crushing and enzymolysis of Damascus rose flowers, fresh flower puree was frozen into ice cubes; comparative example 5 one-time vacuum condensation extraction is carried out on the ice blocks frozen by the fresh flower puree; comparative example 6 the flower stock solution was not subjected to three-stage circulating oil-water separation treatment, and was directly subjected to standing oil-water separation treatment; according to the invention, firstly, Damascus rose flowers are crushed and subjected to enzymolysis to obtain fresh flower raw pulp, so that the oil yield of subsequent rose essential oil can be improved, then the fresh flower raw pulp is rapidly frozen into ice blocks, the loss of aromatic substances can be reduced, the oil yield of the rose essential oil can be effectively improved through two-stage heating and vacuum extraction, and the volatilization, waste and loss of the rose essential oil can be avoided through three-stage circulating oil-water separation treatment, so that the oil yield of the rose essential oil can be effectively improved.
Experimental example 2
The essential oil of Rosa damascena prepared by the methods of examples 1-4 and comparative examples 1-6 was subjected to GC-MS detection to detect the content of main aromatic components, and the results are shown in Table 2.
TABLE 2 Main fragrance component content
As can be seen from Table 2, the essential oil of Damascus roses prepared by the method has the main aromatic content within the standard range of ISO 9842:2003, and has higher main aromatic content than the essential oil of Damascus roses prepared by the comparative method; comparative example 1 a distillation method was used; comparative example 2 solvent extraction was used; comparative example 3 the fresh flower puree is directly extracted in vacuum without being frozen into ice blocks; comparative example 4 without crushing and enzymolysis of Damascus rose flowers, fresh flower puree was frozen into ice cubes; comparative example 5 one-time vacuum condensation extraction is carried out on the ice blocks frozen by the fresh flower puree; comparative example 6 the flower stock solution was not subjected to three-stage circulating oil-water separation treatment, and was directly subjected to standing oil-water separation treatment; according to the invention, firstly, Damascus rose flowers are crushed and subjected to enzymolysis to obtain fresh flower raw pulp, so that the oil yield of subsequent rose essential oil can be improved, then the fresh flower raw pulp is rapidly frozen into ice blocks, the loss of aromatic substances can be reduced, the oil yield of the rose essential oil can be effectively improved through two-stage heating and vacuum extraction, and the volatilization, waste and loss of the rose essential oil can be avoided through three-stage circulating oil-water separation treatment, so that the quality of the rose essential oil is effectively improved.
In conclusion, the method for improving the essential oil yield and quality of the Damascus roses provided by the application extracts essential oil from Damascus roses without distillation and extraction, improves the oil yield of the rose essential oil, reduces damage to aromatic substances, improves the content of aromatic substances in the rose essential oil to a certain extent, and improves the quality of the rose essential oil.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A method for improving the oil yield and quality of Damascus rose essential oil is characterized by comprising the following steps:
s1: picking up fresh rosa damascena flowers, cleaning, crushing, and carrying out enzymolysis by using enzymolysis liquid to obtain fresh flower raw pulp;
s2: freezing fresh flower primary pulp into ice blocks;
s3: carrying out first-stage vacuum condensation extraction on ice blocks frozen with fresh flower primary pulp for 2-4 h to obtain first-stage fresh flower stock solution, carrying out second-stage vacuum condensation extraction for 0.5-1.5 h to obtain second-stage fresh flower stock solution, and mixing the first-stage fresh flower stock solution and the second-stage fresh flower stock solution to obtain fresh flower stock solution;
s4: performing three-stage circulating oil-water separation treatment on the flower stock solution obtained by extraction, and collecting to obtain crude Damascus rose essential oil;
s5: and filtering, dehydrating and aging the collected crude Damascus rose essential oil to obtain a Damascus rose essential oil product.
2. The method according to claim 1, wherein the enzymolysis solution in step S1 is a mixture of plant decomposition enzyme and cellulase, the amount of the plant decomposition enzyme added is 0.1-0.3% of the total weight of the Rosa damascena flowers, and the amount of the cellulase added is 0.04-0.06% of the total weight of the Rosa damascena flowers.
3. The method for improving the oil yield and quality of essential oil of rosa damascena according to claim 1, wherein the raw juice of fresh flowers is frozen at-55 to-45 ℃ for 2 to 4 hours in step S2, and the thickness of the frozen ice blocks is not more than 3 cm.
4. The method for improving the oil yield and quality of essential oil of rosa damascena according to claim 1, wherein in the first stage of step S3, a vacuum extraction tank is used to heat the rose damascena to 25-35 ℃, the vacuum pressure is-0.09-0.095 Mpa, and a capillary low-temperature condensing device is used to control the temperature to-55-50 ℃ for condensation to obtain the flower stock solution in the first stage.
5. The method for improving the oil yield and quality of essential oil of rosa damascena according to claim 1, wherein the second-stage vacuum extraction tank is heated to 40-50 ℃ in the step S3, the vacuum pressure is-0.09-0.095 Mpa, and the temperature is controlled to-55-50 ℃ by using a capillary low-temperature condensation device to obtain the second-stage flower stock solution through condensation.
6. The method according to claim 1, wherein in step S3, the first stage flower stock solution and the second stage flower stock solution are mixed and heated at 30-35 ℃ to obtain a flower stock solution.
7. The method for improving the oil yield and the quality of the essential oil of the rosa damascena according to claim 1, wherein in the step S4, the heating temperature of the primary oil-water separation is 38-42 ℃, the vibration frequency of the oil-water separator is controlled to be 4-6 Hz, the discharging temperature of the material liquid after the oil-water separation is 26-30 ℃, the crude essential oil is collected, and the separated liquid is subjected to secondary oil-water separation; the heating temperature of the second-stage oil-water separation is 42-46 ℃, the vibration frequency of the oil-water separator is controlled to be 8-12 Hz, the discharging temperature of the material liquid after the oil-water separation is 31-35 ℃, the crude essential oil is collected, and the separated liquid is subjected to third-stage oil-water separation; and the heating temperature of the three-stage oil-water separation is 46-50 ℃, the vibration frequency of the oil-water separator is controlled to be 14-16 Hz, the discharging temperature of the material liquid after the oil-water separation is 36-40 ℃, the crude essential oil is collected, and the separated liquid flows back into the flower stock solution.
8. The method for improving essential oil yield and quality of Rosa damascena according to claim 1, wherein the flower stock solution is subjected to three-stage circulation oil-water separation and repeated circulation for 2-3 h in step S4.
9. The method for preparing essential oil of Damascus rose in accordance with claim 1, wherein the crude Damascus rose oil obtained in step S5 is filtered, dehydrated, and aged at 2-8 deg.C for 8-9 weeks.
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