Production process of sauced agilawood essential oil

Abstract

The invention discloses a production process of Maotai-flavor agilawood essential oil, and relates to the technical field of essential oil production, and the process comprises the steps of raw material pretreatment, enzymolysis treatment, microwave-assisted extraction, separation and purification, Maotai-flavor endowing, secondary purification and refining. Raw material pretreatment controls crushing granularity and temperature to retain components; the enzymolysis treatment adopts a specific compound enzyme to improve the dissolution of effective components; microwave-assisted extraction accelerates dissolution and retains thermosensitive components; after separating and purifying to obtain a crude product, fermenting the crude product with a specific spice and a leavening agent to endow the sauce flavor, and performing secondary purification to obtain a finished product with the purity of 98% or above. The process avoids decomposition of thermosensitive components and solvent residues, and the produced essential oil is rich and unique in fragrance, excellent in quality, high in efficiency, low in cost and suitable for popularization and application.

Description

Technical Field

[0001] This invention relates to the field of essential oil production technology, and in particular to a production process for agarwood essential oil with a soy sauce aroma. Background Technology

[0002] Agarwood essential oil is widely used in the fields of fragrance, medicine, and cosmetics due to its unique aroma and numerous benefits. Currently, there are many methods for extracting agarwood essential oil, the most common being steam distillation, solvent extraction, and supercritical fluid extraction. However, these traditional methods have some drawbacks. For example, steam distillation requires a high-temperature environment, which can easily lead to the decomposition of heat-sensitive components in agarwood, affecting the quality and aroma of the essential oil. Furthermore, it has a long extraction cycle and high energy consumption. While solvent extraction can shorten the extraction time to some extent, the problem of solvent residue is difficult to completely resolve, affecting the purity and safety of the essential oil, and it also has a low extraction rate for certain low-polarity aromatic components.

[0003] Furthermore, the market demand for agarwood essential oil with unique aroma and high quality is growing, and existing production processes are struggling to meet this demand. This invention aims to provide a novel production process technology for agarwood essential oil with a distinctive aroma, to solve the problems existing in the prior art, improve the quality and production efficiency of agarwood essential oil, and meet the market demand for high-quality agarwood essential oil. Summary of the Invention

[0004] To address the technical problems existing in the background art, this invention proposes a production process for agarwood essential oil with a soy sauce aroma.

[0005] The present invention proposes a production process for agarwood essential oil with a soy sauce aroma, comprising the following steps: Raw material pretreatment: Select agarwood raw materials, remove impurities and grind them into powder. During the grinding process, control the temperature at 20-25℃. Enzymatic hydrolysis: Deionized water is added to the pulverized agarwood powder, the pH value is adjusted, and then a compound enzyme preparation is added. The enzymatic hydrolysis reaction is carried out at a specific temperature. Microwave-assisted extraction: After enzymatic hydrolysis, ethanol solution is added to the reaction system, and microwave-assisted extraction is performed using intermittent irradiation. Separation and purification: The mixture after microwave-assisted extraction was centrifuged, filtered, and purified by molecular distillation to obtain crude agarwood essential oil; The aroma of soy sauce is imparted by mixing crude agarwood essential oil with specific spices and fermenting agents, and then fermenting it at a specific temperature. Secondary purification and refining: The fermented agarwood essential oil was eluted and separated by silica gel column chromatography, and then subjected to vacuum distillation to obtain soy sauce-flavored agarwood essential oil.

[0006] Furthermore, in the raw material pretreatment, the particle size of the agarwood powder is 60 mesh.

[0007] Furthermore, in the enzymatic hydrolysis process, the mass ratio of deionized water to agarwood powder is 3:1, the pH value is adjusted to 5.0, the compound enzyme preparation is composed of cellulase and pectinase in a mass ratio of 2.5:1, the amount of compound enzyme preparation added is 1.0% of the mass of agarwood powder, the enzymatic hydrolysis reaction temperature is 50℃, and the reaction time is 3 hours.

[0008] Furthermore, in the microwave-assisted extraction, the concentration of the ethanol solution is 80% v / v, the mass-to-volume ratio of agarwood powder to ethanol solution is 1:10 g / mL, the microwave power is 400W, the intermittent irradiation cycle is 30 seconds of irradiation followed by 15 seconds of rest, and the total processing time is 20 minutes.

[0009] Furthermore, in the separation and purification process, the centrifugation speed is 10000 r / min, the time is 15 minutes, the filtration uses a 0.45 μm microporous membrane, and the molecular distillation temperature is 80℃ and the pressure is 0.1 Pa.

[0010] Furthermore, in the process of imparting the soy sauce flavor, the specific spices consist of Sichuan pepper, star anise, cinnamon, cloves, and fennel, with a mass ratio of 2:3:1:1:1, and the total amount added is 5% of the crude agarwood essential oil. The fermentation agent is a mixture of lactic acid bacteria and yeast, with a volume ratio of 3:2, and the amount added is 2% of the crude agarwood essential oil. The fermentation temperature is 30℃, and the fermentation time is 5 days.

[0011] Furthermore, in the secondary purification and refining process, the eluent used in the silica gel column chromatography is a mixed solution of petroleum ether and ethyl acetate with a volume ratio of 8:2.

[0012] Furthermore, in the secondary purification and refining process, the vacuum distillation temperature is 50°C and the pressure is 0.05 Pa.

[0013] Furthermore, in the raw material pretreatment, the selected agarwood raw material is high-quality agarwood.

[0014] Furthermore, the purity of the soy sauce-flavored agarwood essential oil reaches over 98%.

[0015] The beneficial effects of this invention are: 1. It can effectively retain the active ingredients in agarwood, reduce the decomposition of heat-sensitive components, and at the same time give agarwood essential oil a unique savory aroma, making its fragrance more rich and complex, and its quality far exceeds that of agarwood essential oil produced by traditional processes.

[0016] 2. By optimizing process parameters during enzymatic hydrolysis and microwave-assisted extraction, the dissolution rate and amount of effective components of agarwood were increased, greatly shortening the extraction time and improving production efficiency.

[0017] 3. The molecular distillation technology and silica gel column chromatography used in this invention can effectively remove residual solvents (including ethanol) and impurities, ensuring the purity and safety of agarwood essential oil and meeting relevant industry standards and regulations (including the standard of no ethanol residue).

[0018] 4. Under the premise of ensuring product quality, this invention improves the utilization rate of raw materials and reduces energy consumption and production costs by optimizing process steps and parameters, thus achieving good economic benefits and market competitiveness. Attached Figure Description

[0019] Figure 1 This is a process flow diagram of the present invention. Detailed Implementation Example 1

[0020] Reference Figure 1 The present invention proposes a production process for agarwood essential oil with a soy sauce aroma, comprising the following steps: 1) Raw material pretreatment 1000g of high-quality agarwood raw material is accurately weighed, and professional impurity removal equipment is used to carefully remove impurities such as soil and debris attached to the surface of the raw material to ensure its purity.

[0021] The processed agarwood raw material is placed in a low-temperature pulverizer, the pulverizer parameters are set, and it is pulverized into powder with a particle size of 60 mesh.

[0022] During the crushing process, the crusher's built-in circulating cooling system strictly controls the crushing environment temperature at 20-25℃ to prevent the heat-sensitive components in agarwood from being destroyed due to frictional heat during crushing. Tests show that the agarwood powder crushed under these conditions has a uniform particle size and a retention rate of over 95% for the heat-sensitive components.

[0023] 2) Enzymatic hydrolysis Add 3000g of deionized water to 1000g of crushed agarwood powder, in a ratio of 3:1 (mass ratio of deionized water to agarwood powder).

[0024] Start the stirring device to thoroughly mix the agarwood powder and deionized water to form a mixture.

[0025] Use a dilute hydrochloric acid solution to precisely adjust the pH of the mixture to 5.0.

[0026] A compound enzyme preparation is added, which consists of cellulase and pectinase in a mass ratio of 2.5:1, and the amount added is 1.0% of the mass of agarwood powder, i.e., 10g.

[0027] The above mixture was transferred to a constant-temperature reactor, and the reactor temperature was set at 50°C. Enzymatic hydrolysis was carried out at this temperature for 3 hours. During the enzymatic hydrolysis process, samples were taken periodically for testing. The results showed that the decomposition rate of agarwood cell walls reached over 80%, and the dissolution rate of effective components increased by 35% compared to the untreated mixture.

[0028] 3) Microwave-assisted extraction After the enzymatic hydrolysis reaction is complete, there is no need to remove the deionized water and compound enzyme preparation from the system. Instead, add an 80% (volume fraction) ethanol solution directly to the reaction system.

[0029] Add 10,000 mL of ethanol solution precisely according to the mass-to-volume ratio of agarwood powder to ethanol solution of 1:10 (g / mL).

[0030] The mixed solution was transferred to a microwave reactor, the microwave power was set to 400W, and an intermittent irradiation method was adopted. The working cycle was set to irradiate for 30 seconds and then stop for 15 seconds, with a total processing time of 20 minutes.

[0031] During microwave-assisted extraction, the changes in the content of effective components in the extract were monitored in real time. The results showed that under these conditions, the extraction rate of effective components of agarwood was increased by 52% compared with traditional direct soaking extraction, and the retention rate of heat-sensitive components reached 92%.

[0032] 4) Separation and purification The mixture after microwave-assisted extraction was transferred to a high-speed centrifuge, and the centrifugation speed was set to 10,000 r / min for 15 minutes to ensure that the solid residue was fully separated from the extract.

[0033] The supernatant after centrifugation was removed and filtered through a 0.45μm microporous membrane to remove tiny particulate impurities from the extract.

[0034] The filtered extract was transferred to a molecular distillation apparatus. The molecular distillation temperature was set to 80℃ and the pressure to 0.1Pa. Molecular distillation was performed to further remove impurities and residual solvents such as ethanol from the extract, resulting in high-purity crude agarwood essential oil. The purity of the crude agarwood essential oil was found to be 91%.

[0035] 5) The aroma of soy sauce imparts a rich flavor. Take the crude agarwood essential oil obtained above and mix it with specific spices and fermentation agents in a certain proportion.

[0036] The specific spices consist of Sichuan pepper, star anise, cinnamon, cloves, and fennel seeds, all of which are natural raw materials that have not undergone extensive processing. Sichuan pepper is the dried, mature pericarp of the Sichuan pepper plant (Rutaceae family); star anise is the dried, mature fruit of the star anise plant (Magnolia family); cinnamon is the dried bark of the cinnamon tree (Lauraceae family); cloves are the dried flower buds of the clove tree (Myrtaceae family); and fennel seeds are the dried, mature fruit of the anise plant (Apiaceae family). Their mass ratio is 2:3:1:1:1, and the total amount added is 5% of the crude agarwood essential oil. Assuming the crude agarwood essential oil weighs 100g, the amount of Sichuan pepper added would be 2g, star anise 3g, cinnamon 1g, cloves 1g, and fennel seeds 1g.

[0037] The starter culture is a mixture of lactic acid bacteria and yeast, with a volume ratio of 3:2, and is added at 2% of the crude agarwood essential oil mass. For example, when the crude agarwood essential oil mass is 100g, the added mixed starter culture is 2g, of which 1.2g is lactic acid bacteria and 0.8g is yeast.

[0038] The mixture was placed in a fermentation tank, the temperature was set at 30℃, and the fermentation time was 5 days. During the fermentation process, the mixture was stirred regularly every day to promote a full reaction between the spices, fermenting agent, and crude agarwood essential oil. Gas chromatography-mass spectrometry analysis showed that the fermented product contained a rich variety of soy sauce-like aroma compounds, which blended well with the original aroma of the agarwood essential oil, resulting in a high sensory evaluation score.

[0039] 6) Secondary purification and refining After fermentation, the agarwood essential oil containing soy sauce aroma undergoes a secondary purification process.

[0040] The silica gel column chromatography method was adopted. First, silica gel was packed into the chromatography column, and then the fermented agarwood essential oil was slowly added to the top of the silica gel column. A petroleum ether-ethyl acetate mixed solution with a volume ratio of 8:2 was used as the eluent for elution and separation to remove impurities and unreacted substances generated during the fermentation process.

[0041] The washed agarwood essential oil is collected and transferred to a vacuum distillation apparatus. The vacuum distillation temperature is set at 50℃ and the pressure at 0.05Pa to further remove residual solvents (including ethanol) and low-boiling-point impurities, thus obtaining the final high-quality soy sauce-flavored agarwood essential oil.

[0042] The final agarwood essential oil obtained was found to have a purity of 98.2%, agarwood tetraol content of 5.2%, and benzylacetone content of 3.1%. It has a rich and unique aroma, a long-lasting fragrance that can last for more than 8.5 hours in the diffusion experiment, and no ethanol residue. Example 2

[0043] 1) The production process of agarwood essential oil with soy sauce aroma proposed in this invention includes the following steps: Raw material pretreatment Select 1500g of high-quality agarwood raw material and use impurity removal equipment to remove impurities from the surface of the raw material.

[0044] The processed agarwood raw material is placed in a low-temperature pulverizer and pulverized into powder with a particle size of 80 mesh. The temperature is controlled at 20-25℃ during the pulverization process.

[0045] 2) Enzymatic hydrolysis Add 4500g of deionized water to the agarwood powder, stir well, and then adjust the pH of the mixture to 4.8 with dilute hydrochloric acid.

[0046] A compound enzyme preparation is added, which consists of cellulase and pectinase in a 3:1 mass ratio, and the amount added is 1.2% of the mass of agarwood powder.

[0047] The mixture was placed in a constant temperature reactor and enzymatic hydrolysis was carried out at 48°C for 3.5 hours.

[0048] 3) Microwave-assisted extraction After enzymatic hydrolysis, a 75% (volume fraction) ethanol solution was added directly to the reaction system, with a material-to-liquid ratio (mass-volume ratio of agarwood powder to ethanol solution) of 1:12 (g / mL).

[0049] The mixture was transferred to a microwave reactor, the microwave power was set to 350W, and an intermittent irradiation method was used (irradiation for 35 seconds - stop for 20 seconds), with a total processing time of 25 minutes.

[0050] 4) Separation and purification The mixture after microwave-assisted extraction was placed in a high-speed centrifuge, and the centrifugation speed was set to 11,000 r / min for 18 minutes to separate the solid residue from the extract.

[0051] After filtration, the extract was subjected to molecular distillation at a temperature of 85°C and a pressure of 0.08 Pa.

[0052] 5) The aroma of soy sauce imparts a rich flavor. The spices used are Sichuan pepper, star anise, cinnamon, cloves and fennel (in a weight ratio of 2:3:1:1:1), and the amount added is 6% of the crude weight of agarwood essential oil.

[0053] The fermentation agent is a mixture of lactic acid bacteria and yeast (volume ratio 3:2), and the amount added is 3% of the crude agarwood essential oil.

[0054] The mixture was placed in a fermentation tank and fermented at 32°C for 6 days.

[0055] 6) Secondary purification and refining Silica gel column chromatography was used, with a petroleum ether-ethyl acetate mixed solution of volume ratio 7:3 as the eluent for elution and separation.

[0056] The washed agarwood essential oil was subjected to vacuum distillation at a temperature of 55℃ and a pressure of 0.03Pa.

[0057] The obtained agarwood essential oil with soy sauce aroma was of excellent quality, with a purity of 98.5%. The aroma lasted for more than 8 hours in the diffusion experiment. All indicators met the expected requirements, and there was no ethanol residue.

[0058] Comparative Example 1 (using conventional steam distillation method) After crushing 1000g of high-quality agarwood raw material, put it directly into a steam distillation apparatus and add an appropriate amount of water.

[0059] Distillation is carried out at 100-120℃ for 24 hours, and the distillate is collected.

[0060] Agarwood essential oil was separated from the distillate using a separatory funnel.

[0061] Testing revealed that the agarwood essential oil obtained by this method had a relatively simple aroma, suffered severe loss of heat-sensitive components (40%-50%), had a low content of effective components (only about 2% agaritol), and had a long production cycle with energy consumption 3-4 times that of Example 1.

[0062] Comparative Example 2 (using traditional solvent extraction method) After crushing 1000g of agarwood raw material, add a 90% (volume fraction) ethanol solution. The material-to-liquid ratio (mass-volume ratio of agarwood powder to ethanol solution) is 1:8 (g / mL).

[0063] The agarwood essential oil was extracted by soaking at room temperature for 48 hours, and then the extract was filtered and concentrated to obtain crude agarwood essential oil.

[0064] Agarwood essential oil is obtained by removing residual solvent through vacuum distillation.

[0065] Testing revealed that the agarwood essential oil obtained by this method had solvent residue issues, with the amount exceeding industry standards by 2-3 times. Furthermore, the extraction rate of low-polarity aromatic components was insufficient, 30%-40% lower than in Example 1, and the aroma was not strong enough. Sensory evaluation showed that the aroma intensity and richness were significantly lower than the product of this invention.

[0066] As can be seen from the comparison of the above embodiments and comparative examples, the production process of the agarwood essential oil of the present invention can effectively retain the effective components in agarwood, produce agarwood essential oil with high purity, unique and rich aroma and excellent quality, and has the advantages of high production efficiency and low energy consumption, and has good application prospects and market value.

[0067] The above description is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.

Claims

1. A production process for aromatic agarwood essential oil, characterized in that, Includes the following steps: Raw material pretreatment: Select agarwood raw materials, remove impurities and grind them into powder. During the grinding process, control the temperature at 20-25℃. Enzymatic hydrolysis: Deionized water is added to the pulverized agarwood powder, the pH value is adjusted, and then a compound enzyme preparation is added. The enzymatic hydrolysis reaction is carried out at a specific temperature. Microwave-assisted extraction: After enzymatic hydrolysis, ethanol solution is added to the reaction system, and microwave-assisted extraction is performed using intermittent irradiation. Separation and purification: The mixture after microwave-assisted extraction was centrifuged, filtered, and purified by molecular distillation to obtain crude agarwood essential oil; The aroma of soy sauce is imparted by mixing crude agarwood essential oil with specific spices and fermenting agents, and then fermenting it at a specific temperature. Secondary purification and refining: The fermented agarwood essential oil was eluted and separated by silica gel column chromatography, and then subjected to vacuum distillation to obtain soy sauce-flavored agarwood essential oil.

2. The production process of soy sauce-flavored agarwood essential oil according to claim 1, characterized in that, In the raw material pretreatment, the particle size of the agarwood powder is 60 mesh.

3. The production process of soy sauce-flavored agarwood essential oil according to claim 1, characterized in that, In the enzymatic hydrolysis process, the mass ratio of deionized water to agarwood powder is 3:1, the pH value is adjusted to 5.0, the compound enzyme preparation is composed of cellulase and pectinase in a mass ratio of 2.5:1, the amount of compound enzyme preparation added is 1.0% of the mass of agarwood powder, the enzymatic hydrolysis reaction temperature is 50℃, and the reaction time is 3 hours.

4. The production process of soy sauce-flavored agarwood essential oil according to claim 1, characterized in that, In the microwave-assisted extraction, the concentration of the ethanol solution is 80% v / v, the mass-to-volume ratio of agarwood powder to ethanol solution is 1:10 g / mL, the microwave power is 400W, the working cycle of intermittent irradiation is 30 seconds of irradiation followed by 15 seconds of rest, and the total processing time is 20 minutes.

5. The production process of soy sauce-flavored agarwood essential oil according to claim 1, characterized in that, In the separation and purification process, the centrifugation speed was 10000 r / min for 15 minutes, the filtration was carried out using a 0.45 μm microporous membrane, and the molecular distillation temperature was 80 °C and the pressure was 0.1 Pa.

6. The production process of soy sauce-flavored agarwood essential oil according to claim 1, characterized in that, The soy sauce flavoring is imparted by a specific spice blend consisting of Sichuan peppercorns, star anise, cinnamon, cloves, and fennel seeds in a mass ratio of 2:3:1:1:1, with a total addition amount of 5% of the crude agarwood essential oil. The fermentation agent is a mixture of lactic acid bacteria and yeast in a volume ratio of 3:2, with an addition amount of 2% of the crude agarwood essential oil. The fermentation temperature is 30℃, and the fermentation time is 5 days.

7. The production process of soy sauce-flavored agarwood essential oil according to claim 1, characterized in that, In the secondary purification and refining process, the eluent used in the silica gel column chromatography is a mixed solution of petroleum ether and ethyl acetate with a volume ratio of 8:

2.

8. The production process of soy sauce-flavored agarwood essential oil according to claim 1, characterized in that, In the secondary purification and refining process, the temperature of vacuum distillation is 50℃ and the pressure is 0.05Pa.

9. The production process of soy sauce-flavored agarwood essential oil according to claim 1, characterized in that, In the raw material pretreatment, the selected agarwood raw material is high-quality agarwood.

10. The production process of soy sauce-flavored agarwood essential oil according to claim 1, characterized in that, The purity of the soy sauce-flavored agarwood essential oil reaches over 98%.

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