Preparation process for extracting wrinkled gianthyssop herb essential oil

Abstract

The invention discloses a preparation process for extracting wrinkled gianthyssop herb essential oil, and relates to the field of plant essential oil extraction. The preparation process comprises the steps of surface oxidation damage treatment, high penetrating fluid treatment pulping, osmotic pressure impact-ultrasonic wall breaking pretreatment, coalescence oil-water separation, adsorption decoloration and impurity removal, segmented steam condensation impurity removal and the like. The prepared essential oil is small in toxic and side effects and good in safety, plant cell walls are effectively destroyed by treating the raw materials through surface oxidation, osmotic pressure impact and ultrasonic wall breaking, and the release efficiency of the essential oil is improved. And the whole extraction process is simple to operate and high in extraction efficiency, and pure agastache rugosus essential oil can be rapidly obtained.

Description

Technical Field

[0001] The invention relates to the technical field of plant essential oil extraction, in particular to a preparation process for extracting patchouli essential oil. Background Art

[0002] Patchouli has many medicinal effects, such as depression, sedation, anti-inflammatory, antibacterial, etc., and is widely used in the fields of medicine and cosmetics. Traditional Patchouli essential oil extraction processes mostly use steam distillation, but this method has problems such as long extraction time, complicated steps, and high water content in the essential oil, resulting in low extraction efficiency and inability to quickly obtain pure Patchouli essential oil. Supercritical CO2 extraction equipment is expensive, and the solvent method has the risk of organic residues. In addition, during the extraction of essential oils, there are pesticide residues, heavy metal pollution, and a small amount of toxic and irritating substances. Therefore, it is particularly necessary to propose a process that is energy-saving, efficient, low-cost, and suitable for industrial production. Summary of the invention

[0003] The purpose of the present invention is to provide a preparation process for extracting Patchouli essential oil, which reduces the content of harmful substances in the extraction process, improves the extraction efficiency, and quickly obtains pure Patchouli essential oil by optimizing the extraction process and adopting a specific treatment method.

[0004] Technical solution: A preparation process for extracting Patchouli essential oil, comprising the following process steps:

[0005] A. Surface oxidation damage treatment: After irradiating fresh patchouli leaves with ultraviolet light, soak them in a food-grade hydrogen peroxide solution, stir, filter, and rinse with water;

[0006] B. High osmotic fluid treatment and beating: the patchouli leaves treated with surface oxidation destruction in step A are mixed with deionized water, sodium chloride is added and stirred, filtered, and after being rinsed, the patchouli leaves are placed in a pulper for beating and crushing to obtain patchouli leaf slurry;

[0007] C. Osmotic pressure shock-ultrasonic cell wall breaking pretreatment: the Patchouli leaf slurry obtained in step B is mixed with deionized water, stirred and ultrasonically treated, and intermittently heated to prevent overheating to obtain a cell wall breaking liquid;

[0008] D. Coagulation oil-water separation: centrifuge the broken liquid to obtain liquid 1, press the filter cake to obtain liquid 2, combine liquid 1 and liquid 2, filter with a titanium rod, add polyacrylamide and sodium dodecyl sulfate to the filtrate, stir for 30 minutes and let stand for separation. Polyacrylamide as a flocculant can make the oil droplets coagulate, and sodium dodecyl sulfate as a surfactant can make the coagulated oil droplets float to the upper layer more easily. The two work together to better separate the oil and water. Then the oil phase is separated from the oil by a coalescence oil-water separator to obtain an oil-containing liquid;

[0009] E. Adsorption decolorization and impurity removal: Add activated carbon and anhydrous magnesium sulfate to the oily liquid obtained in step D, stir for 4 hours, and filter to obtain an oily substance;

[0010] F. Segmented steam condensation and impurity removal: add the oily substance obtained in step E into the reactor, reduce the pressure and increase the temperature to make the oily substance boil and vaporize, condense the steam in sections through condensers of different temperatures, collect the condensed fraction in the middle section, and obtain the product.

[0011] Preferably, in step A, the ultraviolet light irradiation time is 8 hours, the volume of the food-grade hydrogen peroxide aqueous solution is 3 times the weight of the patchouli leaves, and the stirring is performed at 30-40° C. for 30 minutes.

[0012] Preferably, in step B, the patchouli leaves are mixed with deionized water at a ratio of 1:3-1:5 (g / mL), the weight of sodium chloride is 0.3 times the volume of deionized water, and the stirring time is 6 hours.

[0013] Preferably, in step C, the Patchouli leaf slurry is mixed with deionized water at a ratio of 1:6-1:8 (g / mL), the ultrasonic power is 400-600 W, the ultrasonic time is 20-30 minutes, and the intermittent heating maximum temperature is 45°C.

[0014] Preferably, in step D, the titanium rod filter element is a 0.45 μm pore size filter element, the weight of polyacrylamide added to the filtrate is 1 / 50 of the weight of Patchouli leaves, the weight of sodium dodecyl sulfate added to the filtrate is 1 / 200 of the weight of Patchouli leaves, and the standing separation time is 6 hours.

[0015] Preferably, in step E, the weight of activated carbon added is 1 / 100 of the volume of the oil, and the weight of anhydrous magnesium sulfate added is 1 / 20 of the volume of the oil.

[0016] Preferably, in step F, the temperature of the reduced pressure gasification is 260°C, the pressure is -0.09 MPa, the temperature of the front condenser is 200°C, the temperature of the middle condenser 1 is 150°C, the temperature of the middle condenser 2 is 120°C, the temperature of the last condenser is 50°C, and the collected liquid is the condensed oil of the middle condenser 1 and the middle condenser 2.

[0017] The beneficial effects of the present invention are:

[0018] 1. The essential oil prepared by the preparation process for extracting Patchouli essential oil provided by the present invention has small toxic and side effects and good safety.

[0019] 2. The present invention provides a preparation process for extracting Patchouli essential oil, which effectively destroys plant cell walls and improves the release efficiency of essential oil by using surface oxidation, osmotic pressure shock and ultrasonic wall breaking to treat raw materials.

[0020] 3. The invention provides a preparation process for extracting Patchouli essential oil. The entire extraction process is simple to operate and has high extraction efficiency, and pure Patchouli essential oil can be quickly obtained. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 The infrared spectrum of Patchouli essential oil extracted by the present invention.

[0022] Figure 2 This is the GC / MS total ion map of Patchouli essential oil extracted by the present invention.

[0023] Figure 3 The present invention is a cumulative permeation amount-time curve of the Patchouli essential oil extracted by the present invention and the Patchouli essential oil prepared by organic solvent extraction, ordinary steam extraction and supercritical extraction in a skin test plate.

[0024] Figure 4 The present invention is used to extract Patchouli essential oil and organic solvent extraction, common steam extraction and supercritical extraction to prepare Patchouli essential oil to irritate rat skin pathological sections.

[0025] Among them, A is the pathological section of Patchouli essential oil extracted in Comparative Example 1, B is the pathological section of Patchouli essential oil extracted in Comparative Example 3, C is the pathological section of Patchouli essential oil extracted in Comparative Example 2, and D is the pathological section of Patchouli essential oil extracted in Example 1. DETAILED DESCRIPTION

[0026] The technical solutions in the embodiments of the present invention will be described clearly and completely below in conjunction with the drawings of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0027] Embodiment 1:

[0028] 10 kg of fresh patchouli leaves were irradiated with ultraviolet light for 8 hours, then soaked in 30 L of food-grade hydrogen peroxide solution, stirred at 30 ° C for 30 minutes, filtered, rinsed with water, mixed with 30 L of deionized water, added with 9 kg of sodium chloride, stirred for 6 hours, filtered, rinsed, and then placed in a pulper to pulp and crush the patchouli leaves to obtain patchouli leaf slurry;

[0029] The slurry of Patchouli leaves was mixed with 60L of deionized water, and ultrasonically treated with a power of 400W for 20min, and intermittent heating was used to prevent overheating to obtain a wall-breaking liquid. The wall-breaking liquid was centrifuged and filtered to obtain liquid 1. The filter cake was squeezed by a press to obtain liquid 2. Liquid 1 and liquid 2 were combined and filtered with a 0.45μm titanium rod. 200g of polyacrylamide and 50g of sodium dodecyl sulfate were added to the filtrate and stirred for 30min. The filtrate was allowed to stand for 6h and the oil phase was separated by a coalescence oil-water separator. The oil and water were separated to obtain 201 g of oil-containing liquid, to which 2 g of activated carbon and 10 g of anhydrous magnesium sulfate were added and stirred for 4 h, filtered, and the filtrate was decompressed by -0.09 MPa and heated to 260°C to make the oil boil and vaporize. The steam passed through the 200°C front condenser, the 150°C middle condenser 1, the 120°C middle condenser 2 and the 50°C final condenser in sequence. The collected liquid was the condensed oil of the middle condenser 1 and the middle condenser 2. The middle condensation fraction was collected to obtain 60.3 g.

[0030] Embodiment 2:

[0031] 10 kg of fresh patchouli leaves were irradiated with ultraviolet light for 8 hours, then soaked in 30 L of food-grade hydrogen peroxide solution, stirred at 35° C. for 30 minutes, filtered, rinsed with water, mixed with 40 L of deionized water, added with 12 kg of sodium chloride, stirred for 6 hours, filtered, rinsed, and then placed in a pulper to pulp and crush the patchouli leaves to obtain patchouli leaf slurry;

[0032] The slurry of Patchouli leaves was mixed with 70L of deionized water, and ultrasonically treated with a power of 500W for 25min, and intermittent heating was used to prevent overheating to obtain a wall-breaking liquid. The wall-breaking liquid was centrifuged and filtered to obtain liquid 1. The filter cake was squeezed by a press to obtain liquid 2. Liquid 1 and liquid 2 were combined and filtered with a 0.45μm titanium rod. 200g of polyacrylamide and 50g of sodium dodecyl sulfate were added to the filtrate and stirred for 30min. The filtrate was allowed to stand for 6h and the oil phase was separated by oil-water separation by a coalescence oil-water separator. After separation, 213 g of oil-containing liquid was obtained. 2.1 g of activated carbon and 10.65 g of anhydrous magnesium sulfate were added and stirred for 4 h. After filtering, the filtrate was decompressed by -0.09 MPa and heated to 260°C to make the oil boil and vaporize. The steam passed through the 200°C front condenser, the 150°C middle condenser 1, the 120°C middle condenser 2 and the 50°C final condenser in sequence. The collected liquid was the condensed oil of the middle condenser 1 and the middle condenser 2. The middle condensation fraction was collected to obtain 62.1 g.

[0033] Embodiment 3:

[0034] 10 kg of fresh patchouli leaves were irradiated with ultraviolet light for 8 hours, then soaked in 30 L of food-grade hydrogen peroxide solution, stirred at 40° C. for 30 minutes, filtered, rinsed with water, mixed with 50 L of deionized water, added with 15 kg of sodium chloride, stirred for 6 hours, filtered, rinsed, and then placed in a pulper to pulp and crush the patchouli leaves to obtain patchouli leaf slurry;

[0035] The slurry of Patchouli leaves was mixed with 80L of deionized water, and ultrasonically treated with a power of 600W for 30min, and intermittent heating was used to prevent overheating to obtain a wall-breaking liquid. The wall-breaking liquid was centrifuged and filtered to obtain liquid 1. The filter cake was squeezed by a press to obtain liquid 2. Liquid 1 and liquid 2 were combined and filtered with a 0.45μm titanium rod. 200g of polyacrylamide and 50g of sodium dodecyl sulfate were added to the filtrate and stirred for 30min. The filtrate was allowed to stand for 6h and the oil phase was separated by oil-water separation by a coalescence oil-water separator. After separation, 215g of oil-containing liquid was obtained. 2.2g of activated carbon and 10.75g of anhydrous magnesium sulfate were added and stirred for 4h. After filtering, the filtrate was decompressed by -0.09MPa and heated to 260℃ to make the oil boil and vaporize. The steam passed through the 200℃ front condenser, the 150℃ middle condenser 1, the 120℃ middle condenser 2 and the 50℃ final condenser in sequence. The collected liquid was the condensed oil of the middle condenser 1 and the middle condenser 2. The middle condensation fraction was collected to obtain 62.3g.

[0036] Comparative Example 1:

[0037] 10 kg of fresh patchouli leaves were irradiated with ultraviolet light for 8 hours, then soaked in 30 L of food-grade hydrogen peroxide solution, stirred at 40° C. for 30 minutes, filtered, rinsed with water, mixed with 50 L of deionized water, added with 15 kg of sodium chloride, stirred for 6 hours, filtered, rinsed, and then placed in a pulper to pulp and crush the patchouli leaves to obtain patchouli leaf slurry;

[0038] Mix the Agastache rugosa leaf slurry with 60 L of deionized water, stir and ultrasonically treat at 400 W power for 20 min, and heat intermittently to prevent overheating to obtain a broken liquid. Centrifuge the broken liquid to obtain liquid 1, and press the filter cake to obtain liquid 2. Combine liquid 1 and liquid 2, filter with a 0.45 μm titanium rod, add 10 L of ethyl acetate to the filtrate, stir and extract for 1 h, separate the liquids, add 10 L of ethyl acetate to the aqueous phase again, stir and extract for 1 h, separate the liquids, combine the ethyl acetate phases, and concentrate at 50°C under reduced pressure to constant weight to obtain 268 g of an oily substance.

[0039] Comparative Example 2:

[0040] 10 kg of fresh patchouli leaves were irradiated with ultraviolet light for 8 hours, then soaked in 30 L of food-grade hydrogen peroxide solution, stirred at 40° C. for 30 minutes, filtered, rinsed with water, mixed with 50 L of deionized water, added with 15 kg of sodium chloride, stirred for 6 hours, filtered, rinsed, and then placed in a pulper to pulp and crush the patchouli leaves to obtain patchouli leaf slurry;

[0041] Mix the Agastache rugosa leaf slurry with 60 L of deionized water, stir and ultrasonically treat at 400 W power for 20 min, and heat intermittently to prevent overheating to obtain a broken liquid. Centrifuge the broken liquid to obtain liquid 1, and press the filter cake to obtain liquid 2. Combine liquid 1 and liquid 2, filter with a 0.45 μm titanium rod, add the filtrate into an extraction kettle, inject CO2 with a high-pressure pump, adjust the pressure in the kettle to 35 MPa, and extract at 40°C for 4 hours. The CO2 fluid after extraction enters the decompression kettle, and is decomposed by reduced pressure to obtain 102 g of an oily substance.

[0042] Comparative Example 3:

[0043] After 10 kg of fresh patchouli leaves were irradiated with ultraviolet light for 8 hours, they were soaked in 30 L of food-grade hydrogen peroxide aqueous solution, stirred at 40 ° C for 30 minutes, filtered, and rinsed with water. The patchouli leaves were mixed with 50 L of deionized water, 15 kg of sodium chloride was added and stirred for 6 hours, filtered, and rinsed. The patchouli leaf slurry was mixed with 60 L of deionized water, stirred and ultrasonically treated at a power of 400 W for 20 minutes, intermittent heating was used to prevent overheating, and the microwave-treated material was transferred to a distillation kettle and saturated steam was introduced; initially 100 ° C was maintained for 30 minutes, and then the temperature was lowered to 80 ° C to collect high-boiling components. The condensate was cyclically distilled through an oil-water separator, and the total time was shortened to 1.5-2 hours to obtain 3 L of oil-containing distillate. The oil-containing distillate was placed in a reactor, 1 L of ethyl acetate was added and stirred, and the liquid was separated. 10 g of activated carbon and 50 g of anhydrous magnesium sulfate were added and stirred for 4 hours, filtered, and the filtrate was concentrated at 45 ° C under reduced pressure to obtain 98.4 g of an oily substance.

[0044] Evaluation of skin irritation of Patchouli essential oil extracted by different methods: The rats were depilated on the abdomen, fed normally for 24 h, anesthetized and fixed by intraperitoneal injection of 10% chloral hydrate (dosage 4 μL / g), and then fixed at the same position 4 cm 2 0.2 ml of Patchouli essential oil was evenly applied on the skin of the rats. After 5 hours, the residual essential oil was removed. The rats were killed after 24 hours of conventional feeding. The skin of the applied part was taken, fixed with 10% formaldehyde, embedded in conventional paraffin, sliced ​​to a thickness of 4-5 μm, and stained with hematoxylin-eosin. The test results are statistically shown in the following table:

[0045] Table 1 Comparative Examples and Implementation Comparison List

[0046] Group Crusting, parakeratosis Inflammatory cell infiltration Thinning of the stratum spinosum Thickening of the stratum spinosum Bleeding Example 1 - - 1 - - Example 2 - - 1 - - Example 3 - - 1 - - Comparative Example 1 1 1 2 - 1 Comparative Example 2 1 1 1 - - Comparative Example 3 1 - 1 -

[0047] Note: According to the severity of the lesion, mild is scored as 1 point, moderate is scored as 2 points, severe is scored as 3 points, and no lesion tissue is scored as "-".

[0048] Test results: It can be seen from Examples 1-3 and Comparative Examples 1-3 that the Patchouli essential oil prepared by the present invention has high purity and few toxic and irritating substances. In the in vivo skin irritation evaluation experiment, the essential oil of the present invention only causes mild thinning of the stratum spinosum, which is far superior to the organic solvent extraction of Comparative Example 1, the supercritical CO2 extraction of Comparative Example 2, and the steam extraction of Comparative Example 3.

[0049] The above-mentioned embodiments only express several implementation methods of the present invention, and the description thereof is relatively specific and detailed, but it cannot be understood as limiting the scope of the patent of the present invention. It should be pointed out that, for ordinary technicians in this field, several variations and improvements can be made without departing from the concept of the present invention, which all belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention shall be subject to the attached claims.

Claims

1. A preparation process for extracting Patchouli essential oil, characterized in that: The process steps include: A. Surface oxidation damage treatment: After irradiating fresh patchouli leaves with ultraviolet light, soak them in a food-grade hydrogen peroxide solution, stir, filter, and rinse with water; B. High osmotic fluid treatment and beating: the patchouli leaves treated with surface oxidation destruction in step A are mixed with deionized water, sodium chloride is added and stirred, filtered, and after being rinsed, the patchouli leaves are placed in a pulper for beating and crushing to obtain patchouli leaf slurry; C. Osmotic pressure shock-ultrasonic cell wall breaking pretreatment: the Patchouli leaf slurry obtained in step B is mixed with deionized water, stirred and ultrasonically treated, and intermittently heated to prevent overheating to obtain a cell wall breaking liquid; D. Coalescing oil-water separation: centrifuge and filter the broken liquid to obtain liquid 1, press the filter cake to obtain liquid 2, combine liquid 1 and liquid 2, filter with a titanium rod, add polyacrylamide and sodium dodecyl sulfate to the filtrate, stir for 30 minutes, let stand and separate the liquids, and separate the oil phase into oil-water by a coalescing oil-water separator to obtain an oil-containing liquid; E. Adsorption decolorization and impurity removal: Add activated carbon and anhydrous magnesium sulfate to the oily liquid obtained in step D, stir for 4 hours, and filter to obtain an oily substance; F. Segmented steam condensation and impurity removal: add the oily substance obtained in step E into the reactor, reduce the pressure and increase the temperature to make the oily substance boil and vaporize, condense the steam in sections through condensers of different temperatures, collect the condensed fraction in the middle section, and obtain the product.

2. The preparation process for extracting Patchouli essential oil according to claim 1, characterized in that: In step A, the ultraviolet light irradiation is 265 nm ultraviolet light at 90 μW / cm 2 The irradiation was carried out for 8 hours, the volume of the food-grade hydrogen peroxide solution was 3 times the weight of the patchouli leaves, and the stirring was carried out at 30-40°C for 30 minutes.

3. The preparation process for extracting Patchouli essential oil according to claim 1, characterized in that: In the step B, the patchouli leaves are mixed with deionized water at a ratio of 1:3-1:5 (g / mL), the weight of sodium chloride is 0.3 times the volume of deionized water, and the stirring time is 6 hours.

4. The preparation process for extracting Patchouli essential oil according to claim 1, characterized in that: In the step C, the Patchouli leaf slurry is mixed with deionized water at a ratio of 1:6-1:8 (g / mL), the ultrasonic power is 400-600 W, the ultrasonic time is 20-30 minutes, and the intermittent heating is used to control the temperature at 35-45°C.

5. The preparation process for extracting Patchouli essential oil according to claim 1, characterized in that: In the step D, the titanium rod filter element is a 0.45 μm pore size filter element, the weight of polyacrylamide added to the filtrate is 1 / 50 of the weight of Patchouli leaves, the weight of sodium dodecyl sulfate added is 1 / 200 of the weight of Patchouli leaves, and the standing separation time is 6 hours.

6. The preparation process for extracting Patchouli essential oil according to claim 1, characterized in that: In the step E, the weight of activated carbon added is 1 / 100 of the volume of the oil, and the weight of anhydrous magnesium sulfate added is 1 / 20 of the volume of the oil.

7. The preparation process for extracting Patchouli essential oil according to claim 1, characterized in that: In the step F, the temperature of the reduced pressure gasification is 260°C, the pressure is -0.09MPa, the temperature of the front condenser is 200°C, the temperature of the middle condenser 1 is 150°C, the temperature of the middle condenser 2 is 120°C, the temperature of the last condenser is 50°C, and the collected liquid is the condensed oil of the middle condenser 1 and the middle condenser 2.

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