Extraction method and application of plant aroma extract
Through the combination of rotary cone distillation tower and reverse osmosis, the problems of insufficient aroma concentration and high moisture content in the prior art are solved, efficient concentration and moisture removal of aroma extracts are achieved, and the use value of aroma extracts is enhanced.
Patent Information
- Application Number
- CN202311036853.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2023-08-16
- Publication Date
- 2025-02-21
AI Technical Summary
Existing plant aroma extraction technology is difficult to effectively increase aroma concentration and reduce moisture content, resulting in limited use range and effect of aroma extracts.
The plant slurry was extracted using a rotary cone distillation tower, and the preliminary extract was concentrated by reverse osmosis to reduce the moisture content and increase the concentration of aroma components.
The rapid separation and retention of aroma components is achieved, which significantly increases the aroma concentration of aroma extracts and reduces the moisture content, making the extract more suitable for high-demand products such as electronic cigarettes.
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Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of plant extraction, and more specifically, to an extraction method of a plant aroma extract and application thereof. Background Art
[0002] At present, the fruit flavors used in food, medicine or other industries are basically made by blending chemically synthesized monomers. Chemically synthesized flavors are low in cost, easy to obtain, high in concentration, and small in addition, so they are widely used. However, the chemical smell is strong, the fragrance is not coordinated enough, and there are residual by-products in the synthesis process, which are harmful to the human body. With the improvement of people's requirements for health, natural products are becoming more and more popular, and the research and production of natural fruit aroma products are imminent. However, there is currently little research on natural fruit aroma extraction in the field of plant extraction, and even fewer products that can be industrialized. There are almost no natural fruit aroma products on sale in the market. The main reasons are: 1. The aroma component content in fruits is very low (less than 0.001%); 2. The aroma in fruits is mostly head aroma substances, which are volatile and difficult to collect; 3. Plant aroma is difficult to concentrate. Since plant aroma components are more volatile than water, conventional aroma extraction equipment easily causes the aroma to evaporate with water vapor and cannot be retained in the concentrate, making it difficult to extract and concentrate the fruit aroma; 4. Using fruits or fruit pulp as raw materials, the raw material cost, storage and preservation costs are all high; 5. The experimental cycle is long and the trial and error cost is high. The above reasons have led to slow progress in the field of natural fruit aroma extraction.
[0003] The aroma extraction technology of the spinning cone distillation tower (SCC) is a cutting-edge technology used in natural flavor extraction in recent years. It is an efficient liquid-gas contact device that can extract volatile components from liquid or slurry by steam under vacuum, and is suitable for stripping and preserving aroma substances. The main advantages of this extraction technology are: the composition and characteristics of the extracted aroma substances can be flexibly controlled, and slurry or high-viscosity pulp can be processed. At present, the industrial equipment SCC10000 and SCC1000 can process liquid or slurry, and the experimental equipment SCC100 processes pure liquid without residue. However, because the aroma product extracted by SCC contains a large amount of condensed water, the aroma concentration of the product is not strong enough, which limits its scope of use and effect. Especially for products with high requirements for aroma concentration, such as electronic cigarettes, the water content needs to be further reduced. First, the high water content leads to low effective content of aroma; second, the high water content leads to a decrease in the viscosity of the e-liquid; third, the high water content will affect the quality of the e-liquid, and it will easily deteriorate after being placed for a long time.
[0004] Therefore, in view of the above shortcomings of the existing plant aroma extraction, it is urgent to develop a method for extracting plant aroma extracts to increase the aroma concentration of the aroma extracts and reduce the water content. Summary of the invention
[0005] The present invention aims to solve at least one of the technical problems existing in the above-mentioned prior art. To this end, the present invention provides a method for extracting plant aroma extract and its application. The method provided by the present invention is used to extract the aroma extract of the plant, which can increase the aroma concentration of the aroma extract and reduce the water content.
[0006] A first aspect of the present invention provides a method for extracting a plant aroma extract.
[0007] Specifically, a method for extracting a plant aroma extract comprises the following steps:
[0008] (1) Pretreatment: pulping the plants to obtain plant pulp;
[0009] (2) Extraction: extracting the plant slurry obtained in step (1) using a rotating cone distillation tower to obtain a preliminary plant aroma extract;
[0010] (3) Concentration: The preliminary plant aroma extract obtained in step (2) is concentrated by reverse osmosis to obtain the plant aroma extract.
[0011] After the plant is pulped, the present invention first uses a rotating cone distillation tower to extract the plant pulp. After continuous distillation in the rotating cone distillation tower, the aroma components can be quickly separated to avoid damage to the aroma components. The aroma components are fully retained and the types are more complete. Since the water content in the preliminary plant aroma extract obtained after extraction is relatively high, the preliminary plant aroma extract is concentrated by reverse osmosis, which can intercept substances other than water molecules in the solution (i.e., separated water), further reduce the water content in the aroma extract, and thus increase the concentration of the aroma components.
[0012] Reverse osmosis mainly uses membrane filtration separation technology to selectively separate mixtures of molecules of different particle sizes at the molecular level. According to the size of the membrane pores, it can be divided into: microfiltration membrane (MF), ultrafiltration membrane (UF), nanofiltration membrane (NF), reverse osmosis membrane (RO), etc.
[0013] Preferably, in step (2), the feed rate of extracting the plant slurry obtained in step (1) by using a rotating cone distillation tower is 400L / h to 600L / h, and / or the feed temperature is 40°C to 80°C, and / or the vacuum degree is -0.03MPa to -0.07MPa, and / or the steam flow rate is 20kg / hr to 50kg / hr. The present invention uses a rotating cone distillation tower and performs low-temperature (low feed temperature) and high-speed (fast feed rate) extraction, which can separate aroma components at a lower temperature, avoid damage to the aroma components, and improve the extraction efficiency.
[0014] Further preferably, in step (2), the feed rate for the first extraction of the plant slurry using a rotating cone distillation tower is 400 L / h to 500 L / h, and / or the feed temperature is 40°C to 60°C, and / or the vacuum degree is -0.04 MPa to -0.07 MPa, and / or the steam flow rate is 20 kg / hr to 30 kg / hr.
[0015] More preferably, in step (2), the feed rate for the first extraction of the plant slurry using a rotating cone distillation tower is 400 L / h to 450 L / h, and / or the feed temperature is 40°C to 50°C, and / or the vacuum degree is -0.05 MPa to -0.07 MPa, and / or the steam flow rate is 20 kg / hr to 28 kg / hr.
[0016] Preferably, in step (2), the plant slurry is extracted using a rotating cone distillation tower of model SCC10000 or model SCC1000.
[0017] Preferably, in the first extraction and the second extraction, the rotating speed of the rotating cone distillation tower is 400-500 rpm.
[0018] Further preferably, in step (2), the rotating speed of the rotating cone distillation tower is 460-480 rpm.
[0019] Preferably, in step (3), the reverse osmosis method comprises the following steps: placing the preliminary plant aroma extract obtained in step (2) in a reverse osmosis device, concentrating it using a reverse osmosis membrane element to obtain an intercepted liquid, until the volume of the intercepted liquid is concentrated to 1 / 15 to 1 / 5 of the preliminary plant aroma extract, stopping the concentration, and obtaining the plant aroma extract. The reverse osmosis method separates different substances through reverse osmosis membrane elements of different pore sizes at room temperature and without vacuum, thereby achieving the effect of separation and concentration. After the above-mentioned concentration treatment, the aroma concentration of the obtained plant aroma extract is equivalent to 5 to 15 times that of the preliminary plant aroma extract, and the water content is 1 / 15 to 1 / 5 of the water content when feeding.
[0020] Further preferably, the concentration is stopped until the volume of the intercepted liquid is concentrated to 1 / 11 to 1 / 8 of the preliminary plant aroma extract.
[0021] More preferably, the concentration is stopped until the volume of the intercepted liquid is concentrated to 1 / 10 of the preliminary plant aroma extract.
[0022] Preferably, the reverse osmosis permeate used in the reverse osmosis method is pure water.
[0023] Preferably, the pore size of the reverse osmosis membrane element is 10D to 50D.
[0024] Preferably, the working pressure of the reverse osmosis equipment is 2Mpa to 6Mpa.
[0025] Preferably, step (1) further comprises, after obtaining the plant slurry, enzymatically hydrolyzing the plant slurry.
[0026] Preferably, the temperature of the enzymolysis is 40° C. to 45° C., and the time of the enzymolysis is 1 hour to 1.5 hours.
[0027] Preferably, the enzymatic hydrolysis uses at least one of pectinase, cellulase and β-glucosidase.
[0028] Preferably, the enzyme used in the enzymolysis is food grade.
[0029] Preferably, the enzymatic activity of the pectinase is 100,000 U / g to 200,000 U / g.
[0030] Preferably, the added amount of the pectinase is 0.005% to 0.100% by weight of the plant slurry.
[0031] Preferably, the enzymatic activity of the cellulase is 100,000 U / g to 200,000 U / g.
[0032] Preferably, the added amount of the cellulase accounts for 0.005% to 0.20% of the weight of the plant slurry.
[0033] Preferably, the enzymatic activity of the β-glucosidase is 100 U / g to 1000 U / g.
[0034] Preferably, the added amount of the β-glucosidase accounts for 0.005% to 0.100% of the weight of the plant slurry.
[0035] Preferably, in step (1), the plant is a fruit, and the fruit includes at least one of mango, strawberry, apple and grape.
[0036] Further preferably, in step (1), the plant is mango. When extracting the mango aroma extract, enzymolysis is required. When other plants are selected, enzymolysis can be selectively performed. During the enzymolysis process, pectin, cell walls and glycosidic bonds are enzymolyzed; pectin decomposition is beneficial to reducing the viscosity of mango pulp and reducing the resistance to the release of aroma inside mango pulp; cell wall disintegration is beneficial to the full release of free aroma substances, bonded aroma substances and aroma precursor substances in the cell, promoting the synthesis of aroma, and maximizing the aroma content; the cleavage of glycosidic bonds is beneficial to converting bonded aroma substances into free aroma substances, increasing the actual volatile aroma concentration.
[0037] A second aspect of the present invention provides an application of a method for extracting a plant aroma extract.
[0038] A method for extracting a plant aroma extract and its application in the field of food, medicine or electronic cigarette preparation.
[0039] Compared with the prior art, the beneficial effects of the present invention are as follows:
[0040] After the plants are pulped, the present invention first uses a rotating cone distillation tower to extract the plant pulp to obtain a preliminary plant aroma extract, and then uses a reverse osmosis method to concentrate the preliminary plant aroma extract to finally obtain a plant aroma extract. The method provided by the present invention can realize the rapid separation of aroma components and avoid the destruction of the aroma components. More aroma components are retained, and the reverse osmosis method is used to intercept substances other than water molecules in the solution, thereby removing most of the water in the extract, thereby increasing the concentration of the aroma components of the aroma extract and reducing the water content. In addition, the method of the present invention is simple and easy to operate, has low equipment requirements, and is conducive to expanding the application scenarios of plant aroma extracts. BRIEF DESCRIPTION OF THE DRAWINGS
[0041] Figure 1 is the gas chromatography-mass spectrometry (GC / MS) graph of mango puree;
[0042] Figure 2 The gas chromatography-mass spectrometry (GC / MS) diagram of the concentrated mango aroma extract extracted in Example 1 of the present invention;
[0043] Figure 3 This is a gas chromatography-mass spectrometry (GC / MS) graph of the mango aroma extract extracted in Comparative Example 3. DETAILED DESCRIPTION
[0044] In order to make the technical scheme of the present invention more clearly understood by those skilled in the art, the following embodiments are listed for illustration. It should be pointed out that the following embodiments do not limit the protection scope of the present invention.
[0045] Unless otherwise specified, the raw materials, reagents or devices used in the following examples can be obtained from conventional commercial sources or by existing known methods.
[0046] The water content analysis method of the present invention is as follows:
[0047] The moisture content of the analyte was detected by a fully automatic Karl Fischer moisture analyzer, and the detection accuracy of the device was 0.01%.
[0048] Example 1
[0049] A method for extracting a mango aroma extract comprises the following steps:
[0050] (1) Pretreatment: 600 kg of fresh ripe mangoes were washed, the skin was disinfected, the core and skin were removed, and the mangoes were cut into pieces and pulped at 0°C in an oxygen-free environment to obtain about 300 kg of mango pulp for later use.
[0051] (2) Composite enzymatic hydrolysis: add 15 g pectinase (enzyme activity of 200,000 U / g), 15 g cellulase (enzyme activity of 200,000 U / g), and 15 g β-glucosidase (enzyme activity of 1000 U / g) to 300 kg mango pulp, stir well, raise the temperature of the mango pulp to 40°C and maintain it for enzymatic hydrolysis for 1 hour.
[0052] (3) Extraction (separation of aroma and pulp):
[0053] About 300kg of mango pulp after enzymolysis was poured into the feed tank of the rotating cone distillation tower, and the feed rate was adjusted to 400L / h, the feed temperature was 50°C, the vacuum degree was -0.07MPa, the steam flow rate was 28kg / hr, and the speed was 460 rpm. Continuous distillation was started to obtain about 21kg of preliminary mango aroma extract and about 302kg of deodorized mango pulp. The preliminary mango aroma extract was quantitatively analyzed by headspace solid phase microextraction (HS-SPME) technology combined with gas chromatography-mass spectrometry (GC / MS), and the content of its characteristic compound terpinene was detected to be 1.2mg / kg. The water content of the mango aroma primary extract was analyzed, and the water content was measured to be 99.99%.
[0054] (4) Concentration (enrichment and concentration by reverse osmosis):
[0055] Add 21kg of mango aroma primary extract to the reverse osmosis equipment, seal the feed tank, select a reverse osmosis membrane with a membrane element pore size of 20D, start the machine, adjust the working pressure to 4.0Mpa, obtain the intercepted liquid, and stop working until the volume of the intercepted liquid in the feed tank is concentrated to 2.1kg to obtain a concentrated mango aroma extract. The headspace solid phase microextraction (HS-SPME) technology combined with gas chromatography-mass spectrometry (GC / MS) was used to quantitatively analyze the above-mentioned concentrated mango aroma extract, and the content of its characteristic compound terpinene was detected to be 13.4mg / kg. The aroma concentration of the concentrated mango aroma extract is equivalent to 11 times that of the preliminary mango aroma extract. The water content of the concentrated mango aroma extract was analyzed, and the result showed that the water content was 99.90%.
[0056] Example 2
[0057] A method for extracting a strawberry aroma extract comprises the following steps:
[0058] (1) Pretreatment: 600 kg of fresh ripe strawberries were washed, the skins were disinfected, cut into pieces and pulped at 0°C in an oxygen-free environment to obtain about 600 kg of fresh strawberry pulp for later use.
[0059] (2) Composite enzymatic hydrolysis: Add 15 g pectinase (enzyme activity of 200,000 U / g), 15 g cellulase (enzyme activity of 200,000 U / g), and 15 g β-glucosidase (enzyme activity of 1000 U / g) to 600 kg of strawberry pulp, stir thoroughly, raise the temperature of the strawberry pulp to 40°C and maintain it for 1 hour.
[0060] (3) Extraction (separation of aroma and pulp):
[0061] Pour about 600kg of strawberry pulp after enzymatic hydrolysis into the feed tank of the rotating cone distillation tower, adjust the feed rate to 400L / h, the feed temperature to 50°C, the vacuum degree to -0.07MPa, the steam flow rate to 28kg / hr, and the rotation speed to 460 rpm. Start continuous distillation to obtain about 42kg of preliminary strawberry aroma extract and about 606kg of deodorized strawberry pulp. The preliminary strawberry aroma extract was quantitatively analyzed by headspace solid phase microextraction (HS-SPME) technology combined with gas chromatography-mass spectrometry (GC / MS), and the content of its characteristic compound methyl butyrate was detected to be 103.3mg / kg.
[0062] (4) Concentration (enrichment and concentration of strawberry aroma extract):
[0063] 42kg of preliminary strawberry aroma extract was added to the reverse osmosis equipment, the feed tank was sealed, a reverse osmosis membrane with a membrane element pore size of 20D was selected, the machine was turned on, the working pressure was adjusted to 4.0Mpa, and the intercepted liquid was obtained until the volume of the intercepted liquid in the feed tank was concentrated to 4.2kg, and the operation was stopped to obtain a concentrated strawberry aroma extract. The above-mentioned concentrated strawberry aroma extract was quantitatively analyzed by headspace solid phase microextraction (HS-SPME) technology combined with gas chromatography-mass spectrometry (GC / MS), and the content of its characteristic compound methyl butyrate was detected to be 1.01g / kg. The aroma concentration of the concentrated strawberry aroma extract at this time is equivalent to ten times that of the preliminary strawberry aroma extract.
[0064] Example 3
[0065] This embodiment provides a method for extracting plant aroma extracts. The difference from Embodiment 1 is that the feed rate in step (3) is adjusted to 500 L / h, and other conditions remain unchanged.
[0066] The extraction step obtained about 16.8 kg of preliminary mango aroma extract and about 301 kg of deodorized mango pulp. The preliminary mango aroma extract was quantitatively analyzed by headspace solid phase microextraction (HS-SPME) technology combined with gas chromatography-mass spectrometry (GC / MS), and the content of its characteristic compound terpinene was detected to be 1.0 mg / kg. The water content of the mango aroma preliminary extract was analyzed, and the water content was measured to be 99.99%.
[0067] Concentration step, to obtain 1.68kg concentrated mango aroma extract. Using headspace solid phase microextraction (HS-SPME) technology combined with gas chromatography-mass spectrometry (GC / MS), the above-mentioned concentrated mango aroma extract was quantitatively analyzed, and the content of its characteristic compound terpinene was detected to be 11.4mg / kg. The aroma concentration of the concentrated mango aroma extract at this time is equivalent to 11 times that of the preliminary mango aroma extract (the content of terpinene in the preliminary mango aroma extract is 1.0mg / kg, and the content of terpinene in the concentrated mango aroma extract is 11.4mg / kg, which is equivalent to 11 times that of the former). The concentrated mango aroma extract was analyzed for water content, and the result showed that the water content was 99.92%.
[0068] Example 4
[0069] This embodiment provides a method for extracting plant aroma extracts. The difference from Embodiment 2 is that the steam flow rate in step (3) is adjusted to 35 kg / hr, and other conditions remain unchanged.
[0070] The extraction step obtained about 52.5 kg of preliminary strawberry aroma extract and about 607 kg of de-fragrant strawberry pulp. The preliminary strawberry aroma extract was quantitatively analyzed by headspace solid phase microextraction (HS-SPME) technology combined with gas chromatography-mass spectrometry (GC / MS), and the content of its characteristic compound methyl butyrate was detected to be 95.5 mg / kg.
[0071] The concentration step obtained 5.25 kg of concentrated strawberry aroma extract. The concentrated strawberry aroma extract was quantitatively analyzed by headspace solid phase microextraction (HS-SPME) combined with gas chromatography-mass spectrometry (GC / MS), and the content of its characteristic compound methyl butyrate was detected to be 972.1 mg / kg. The aroma concentration of the concentrated strawberry aroma extract at this time is equivalent to 10 times that of the preliminary strawberry aroma extract.
[0072] Example 5 (without enzymolysis)
[0073] This embodiment provides a method for extracting a mango aroma extract. The difference from Embodiment 1 is that the mango is directly extracted without composite enzymatic hydrolysis after pre-treatment, and other process conditions remain unchanged. The specific steps are as follows:
[0074] (1) Pretreatment: 600 kg of fresh ripe mangoes were washed, the skin was disinfected, the core and skin were removed, and the mangoes were cut into pieces and pulped at 0°C in an oxygen-free environment to obtain about 300 kg of mango pulp for later use.
[0075] (2) Extraction (separation of aroma and pulp):
[0076] About 300 kg of mango pulp was poured into the feed tank of the rotating cone distillation tower, and the feed rate was adjusted to 400 L / h, the feed temperature was 50 ° C, the vacuum degree was -0.07 MPa, the steam flow rate was 28 kg / hr, and the rotation speed was 460 rpm. Continuous distillation was started to obtain about 20.1 kg of preliminary mango aroma extract and about 301.8 kg of deodorized mango pulp. The preliminary mango aroma extract was quantitatively analyzed by headspace solid phase microextraction (HS-SPME) technology combined with gas chromatography-mass spectrometry (GC / MS), and the content of its characteristic compound terpinene was detected to be 0.66 mg / kg. The water content of the mango aroma primary extract was analyzed, and the result showed that the water content was 99.99%.
[0077] (3) Concentration (enrichment and concentration by reverse osmosis):
[0078] Add 20.1kg of mango aroma primary extract to the reverse osmosis equipment, seal the feed tank, select a reverse osmosis membrane with a membrane element pore size of 20D, start the machine, adjust the working pressure to 4.0Mpa, obtain the intercepted liquid, and stop working until the volume of the intercepted liquid in the feed tank is concentrated to 2.1kg to obtain a concentrated mango aroma extract. The headspace solid phase microextraction (HS-SPME) technology combined with gas chromatography-mass spectrometry (GC / MS) was used to quantitatively analyze the above-mentioned concentrated mango aroma extract, and the content of its characteristic compound terpinene was detected to be 7.4mg / kg. The aroma concentration of the concentrated mango aroma extract is equivalent to 10 times that of the preliminary mango aroma extract. The water content of the concentrated mango aroma extract was analyzed, and the result showed that the water content was 99.98%.
[0079] Since no enzymatic hydrolysis was performed in Example 5, the cell wall was not completely broken, so the aroma was not released sufficiently in the subsequent aroma extraction process. Although SCC extraction was performed, the terpinene content was only 7.4 mg / kg, which was lower than that in Example 1, indicating that the composite enzymatic hydrolysis had a significant effect on increasing the content of aroma components in the extract.
[0080] Example 6
[0081] This embodiment provides a method for extracting a mango aroma extract, which is different from that of Embodiment 1 in that the extraction process conditions are different. The specific steps are as follows:
[0082] (1) Pretreatment: 600 kg of fresh ripe mangoes were washed, the skin was disinfected, the core and skin were removed, and the mangoes were cut into pieces and pulped at 0°C in an oxygen-free environment to obtain about 300 kg of mango pulp for later use.
[0083] (2) Composite enzymatic hydrolysis: add 15 g pectinase (enzyme activity of 200,000 U / g), 15 g cellulase (enzyme activity of 200,000 U / g), and 15 g β-glucosidase (enzyme activity of 1000 U / g) to 300 kg mango pulp, stir well, raise the temperature of the mango pulp to 40°C and maintain it for enzymatic hydrolysis for 1 hour.
[0084] (3) Extraction (separation of aroma and pulp):
[0085] Pour about 300kg of mango pulp after enzymolysis into the feed tank of the rotating cone distillation tower, adjust the feed rate to 800L / h, the feed temperature to 30°C, the vacuum degree to -0.01MPa, the steam flow rate to 15kg / hr, and the rotation speed to 460 rpm. Start continuous distillation to obtain about 11.25kg of preliminary mango aroma extract and about 304kg of deodorized mango pulp. The preliminary mango aroma extract was quantitatively analyzed by headspace solid phase microextraction (HS-SPME) technology combined with gas chromatography-mass spectrometry (GC / MS), and the content of its characteristic compound terpinene was detected to be 0.72mg / kg. The water content of the mango aroma primary extract was analyzed, and the water content was measured to be 99.99%.
[0086] (4) Concentration (enrichment and concentration by reverse osmosis):
[0087] Add 11.25kg of mango aroma primary extract to the reverse osmosis equipment, seal the feed tank, select a reverse osmosis membrane with a membrane element pore size of 20D, start the machine, adjust the working pressure to 4.0Mpa, obtain the intercepted liquid, and stop working until the volume of the intercepted liquid in the feed tank is concentrated to 1.13kg to obtain a concentrated mango aroma extract. The headspace solid phase microextraction (HS-SPME) technology combined with gas chromatography-mass spectrometry (GC / MS) was used to quantitatively analyze the above-mentioned concentrated mango aroma extract, and the content of its characteristic compound terpinene was detected to be 7.34mg / kg. The aroma concentration of the concentrated mango aroma extract is equivalent to 10 times that of the preliminary mango aroma extract. The water content of the concentrated mango aroma extract was analyzed, and the result showed that the water content was 99.97%.
[0088] Since the feed rate, feed temperature, vacuum degree and steam flow rate of the rotating cone distillation tower are adjusted in Example 6, the terpinolene content of the concentrated mango aroma extract in Example 6 is lower than that in Example 1, and the water content is higher than that in Example 1.
[0089] Comparative Example 1 (without reverse osmosis)
[0090] A method for extracting a plant aroma extract comprises the following steps:
[0091] (1) Pretreatment: 600 kg of fresh ripe mangoes were washed, the skin was disinfected, the core and skin were removed, and the mangoes were cut into pieces and pulped at 0°C in an oxygen-free environment to obtain about 300 kg of mango pulp for later use.
[0092] (2) Composite enzymatic hydrolysis: Add 15 g pectinase, 15 g cellulase and 15 g β-glucosidase to 300 kg mango pulp, stir thoroughly, raise the temperature of the mango pulp to 40°C and maintain it for 1 hour.
[0093] (3) Extraction (separation of aroma and pulp):
[0094] Pour about 300kg of mango pulp after enzymatic hydrolysis into the feed tank of the rotating cone distillation tower, adjust the feed rate to 400L / h, the feed temperature to 50°C, the vacuum degree to -0.07MPa, the steam flow rate to 28kg / hr, and the rotation speed to 460 rpm. Start continuous distillation to obtain about 21kg of mango aroma extract and about 302kg of deodorized mango pulp. The mango aroma extract was quantitatively analyzed by headspace solid phase microextraction (HS-SPME) technology combined with gas chromatography-mass spectrometry (GC / MS), and the content of its characteristic compound terpinene was detected to be 1.2mg / kg.
[0095] Comparative Example 2 (using evaporation concentration method, also known as vacuum concentration method)
[0096] A method for extracting a plant aroma extract comprises the following steps:
[0097] Fresh mangoes were peeled and pitted, and the obtained pulp was pulped and filtered through a 100-mesh filter cloth to obtain mango pulp. The mango pulp was hydrolyzed with pectinase for 30 minutes, and then filtered through a 100-mesh filter cloth to obtain 14.3°Brix mango juice (No. 1), which was then vacuum concentrated to obtain five concentrated samples of different concentrations of 27°Brix (No. 2), 37°Brix (No. 3), 47°Brix (No. 4), and 53°Brix (No. 5). The above five mango juice samples were respectively subjected to detection and analysis of mango aroma components.
[0098] The aroma components in mango juices No. 1-5 were analyzed by headspace solid phase microextraction (HS-SPME) combined with gas chromatography-mass spectrometry (GC / MS). The results showed that compared with mango juice No. 1, under vacuum concentration conditions, the types of aroma components in mango juice No. 2-5 decreased, and the content of each component also decreased. Moreover, the higher the sugar content of concentrated mango juice, the more the aroma substance content decreased. Among them, the main characteristic aroma component of mango juice, terpinolene, gradually decreased with the continuous increase of mango juice concentration, from 1.951×10 -5 % (No. 1) decreased to 0.032×10 -5% (No. 5), a decrease of 98.35%. This is because during the vacuum concentration process, the vacuum is continuously drawn, resulting in the removal of trace aroma components, and the amount that can be condensed is very small.
[0099] Comparative Example 3 (using propylene glycol extraction)
[0100] Take 100g of mango pulp prepared in Example 1, add 500g of propylene glycol, fully stir and extract in a juicer for 3 minutes, then centrifuge the mixture of mango pulp and propylene glycol at 10000 rpm and 15°C for 15 minutes, and the supernatant is the mango aroma extract of the propylene glycol extraction method. The mango aroma extract was analyzed by headspace solid phase microextraction (HS-SPME) technology combined with gas chromatography-mass spectrometry (GC / MS).
[0101] The components in the mango puree, the concentrated mango aroma extract obtained in Example 1, and the mango aroma extract obtained in Comparative Example 3 were detected by headspace solid phase microextraction (HS-SPME) technology combined with gas chromatography-mass spectrometry (GC / MS). The results are shown in Table 1 below.
[0102] Table 1 Comparison of components in the extracts obtained from mango puree, Example 1, and Comparative Example 3
[0103] Component No. Mango Puree Example 1 Comparative Example 3 1 oxygen oxygen oxygen 2 N-Acetyl-DL-Alanine N-Acetyl-DL-Alanine 3 Methyl sulfide Methyl sulfide Methyl sulfide 4 Ethyl acetate Ethyl acetate 5 Glycol Acid Glycol Acid 6 Ethanol Ethanol 7 α-Pinene 8 Ethyl butyrate 9 Isoamyl acetate Isoamyl acetate 10 3-Carene 11 Myrcene 12 Terpinene 13 Limonene 14 Propylene glycol 15 Hexyl acetate Hexyl acetate 16 Terpinolene Terpinolene 17 Allyl hexanoate Allyl hexanoate
[0104] The test results of the components in the mango puree, the concentrated mango aroma extract obtained in Example 1, and the mango aroma extract obtained in Comparative Example 3 are as follows: Figure 1-3 As shown in the figure, and summarized in Table 1, it can be seen from the table that the method used in Example 1 of the present invention can extract and retain most of the main aroma components in mango puree, and its aroma type composition is closer to mango puree. However, the aroma components obtained by the comparative example 3 using the traditional propylene glycol extraction technology are few in variety and the aroma components are seriously missing. The above results show that the extraction method provided by the present invention can better extract mango aroma, and the extracted aroma components are more complete.
[0105] In summary, in Example 1 of the present invention, the mango aroma is initially extracted from the mango slurry by using a rotating cone distillation tower, and then membrane concentration is performed by reverse osmosis, which not only improves the concentration of the mango aroma extract (the concentration of terpinene in the initial extraction is increased from 1.2 mg / kg to 13.4 mg / kg), but also reduces the water content of the mango aroma extract (the water content in the initial extraction is reduced from 99.99% to 99.90%), and the aroma components are more complete. Examples 2-4 can all achieve the same effect as Example 1, and the extraction method of the present invention is simple and efficient, and the membrane concentration equipment has low cost.
Claims
1. A method for extracting a plant aroma extract, characterized in that: The steps include: (1) Pretreatment: pulping the plants to obtain plant pulp; (2) Extraction: extracting the plant slurry obtained in step (1) using a rotating cone distillation tower to obtain a preliminary plant aroma extract; (3) Concentration: The preliminary plant aroma extract obtained in step (2) is concentrated by reverse osmosis to obtain the plant aroma extract.
2. The extraction method according to claim 1, characterized in that In step (2), the plant slurry obtained in step (1) is extracted using a rotating cone distillation tower at a feed rate of 400 L / h to 600 L / h, and / or a feed temperature of 40° C. to 80° C., and / or a vacuum degree of -0.03 MPa to -0.07 MPa, and / or a steam flow rate of 20 kg / hr to 50 kg / hr.
3. The extraction method according to claim 2, characterized in that In step (2), the plant slurry obtained in step (1) is extracted using a rotating cone distillation tower at a feed rate of 400 L / h to 500 L / h, and / or a feed temperature of 40° C. to 60° C., and / or a vacuum degree of -0.04 MPa to -0.07 MPa, and / or a steam flow rate of 20 kg / hr to 30 kg / hr.
4. The extraction method according to claim 1, characterized in that In step (2), the plant slurry is extracted using a rotating cone distillation tower of model SCC1000.
5. The extraction method according to claim 1, characterized in that In step (3), the reverse osmosis method comprises the following steps: placing the preliminary plant aroma extract obtained in step (2) in a reverse osmosis device, and concentrating it using a reverse osmosis membrane element to obtain an intercepted liquid, until the volume of the intercepted liquid is concentrated to 1 / 15 to 1 / 5 of the preliminary plant aroma extract, and then stopping the concentration to obtain the plant aroma extract.
6. The extraction method according to claim 5, characterized in that The concentration is stopped until the volume of the intercepted liquid is concentrated to 1 / 11 to 1 / 8 of the preliminary plant aroma extract.
7. The extraction method according to claim 5, characterized in that The pore size of the reverse osmosis membrane element is 10D to 50D.
8. The extraction method according to claim 1, characterized in that Step (1) also includes, after obtaining the plant slurry, enzymatically hydrolyzing the plant slurry.
9. The extraction method according to claim 1, characterized in that In step (1), the plant is a fruit, and the fruit includes at least one of mango, strawberry, apple, and grape.
10. Application of the method for extracting the plant aroma extract according to any one of claims 1 to 9 in the field of food, medicine or electronic cigarette preparation.