Osmanthus fragrans extract and extraction method thereof

Abstract

The invention provides a sweet osmanthus extract and an extraction method thereof. The extraction method comprises the following steps: S1, dehydrating and crushing fresh sweet-scented osmanthus to obtain sweet-scented osmanthus powder; s2, mixing the osmanthus fragrans powder with the enzymatic hydrolysate, and carrying out primary microwave extraction; carrying out secondary microwave extraction to obtain an enzymolysis mixture; and S3, carrying out instantaneous pressurization extraction on the ethanol solution and the enzymolysis mixture to obtain a mixed extract, filtering the mixed extract to obtain filtrate, carrying out rotary evaporation concentration to remove ethanol, and carrying out concentration to obtain the osmanthus fragrans extract. In the process of extracting the osmanthus fragrans extract, the compound enzyme is combined with proper microwave and instantaneous pressurization process conditions, so that plant cell walls of osmanthus fragrans can be effectively broken, active ingredients in osmanthus fragrans can be quickly dissolved out, and the extraction yield of the osmanthus fragrans extract is effectively improved. Moreover, in the extraction process, the damage to active ingredients can be reduced, the activity and stability of the extract are ensured, the content of substances such as flavone in the sweet-scented osmanthus extract is increased, and the quality of a product extracted from the sweet-scented osmanthus extract is effectively ensured.

Description

Technical Field

[0001] The invention relates to the technical field of osmanthus extraction, in particular to an osmanthus extract and an extraction method thereof. Background Art

[0002] Osmanthus (Osmanthus.fiagrans Lour.) is one of the ten traditional famous flowers in China. It is an evergreen woody plant belonging to the genus Osmanthus of the family Oleaceae. It is also known as Osmanthus, Rock Osmanthus, and Osmanthus fragrans. Osmanthus is a plant with both medicinal and edible properties. It has the effects of warming the lungs and resolving phlegm, promoting the production of body fluids, eliminating odor, and moistening the intestines and relieving constipation. Osmanthus petals are rich in nutrients such as flavonoids, amino acids, and minerals. They are usually used to make osmanthus cakes, osmanthus tea, osmanthus wine, etc. In addition, osmanthus extracts are also used in the development of daily necessities, skin care products, perfumes, and other products. These products are deeply loved by consumers, further improving the deep processing value of osmanthus.

[0003] Deep processing of sweet osmanthus mainly involves further extracting sweet osmanthus essential oil and sweet osmanthus extract. Sweet osmanthus extract can be used in beverages, candies, alcohol and tobacco, daily chemicals, cosmetics, etc., and is widely used and in great demand. At present, the traditional solvent extraction method mainly using petroleum ether as solvent is the main method in the extraction process of sweet osmanthus extract, and the process is relatively backward, so that the extraction yield of sweet osmanthus extract is low and the product quality is also low. Although other extraction methods occur, the extraction effect is still unsatisfactory. Along with the continuous increase of the market price of sweet osmanthus, improving the extraction efficiency and product quality of sweet osmanthus extract has become an important problem urgently to be solved in the deep processing industry of sweet osmanthus. Summary of the invention

[0004] In view of this, the present invention provides an osmanthus extract and an extraction method thereof.

[0005] The technical solution of the present invention is achieved in this way:

[0006] A method for extracting osmanthus extract comprises the following steps:

[0007] S1, dehydrating fresh osmanthus by vacuum freeze drying, and crushing to obtain osmanthus powder;

[0008] S2, after mixing the osmanthus powder with the enzymatic hydrolyzate, perform a microwave extraction for 25 to 30 minutes at a temperature of 30 to 45° C. and a power of 200 to 250 W; then perform a second microwave extraction for 12 to 15 minutes at a temperature of 30 to 45° C. and a power of 500 to 600 W to obtain an enzymatic hydrolyzate mixture;

[0009] S3. Adding ethanol solution to the enzymatic hydrolysis mixture for instantaneous pressure extraction to obtain a mixed extract, filtering the mixed extract to obtain the filtrate, and concentrating the filtrate by rotary evaporation to remove ethanol, and concentrating to obtain osmanthus extract.

[0010] Furthermore, the particle size of the osmanthus powder is 50 to 60 meshes.

[0011] Furthermore, the material-liquid ratio of the osmanthus powder to the enzymatic hydrolysis liquid is 1:7-10 g / mL.

[0012] Furthermore, the enzymatic hydrolysate comprises β-glucosidase, xylanase, pectinase and water in a mass ratio of 5-8:0.8-1.4:1-2:120-150.

[0013] Furthermore, the volume ratio of the ethanol solution to the enzymatic hydrolysis mixture is 1 to 1.8:1; and the mass concentration of the ethanol solution is 90% to 95%.

[0014] Furthermore, the instantaneous pressurization process is as follows: increasing the pressure to 30-40 MPa within 0.1-0.5 s, maintaining the pressure for 8-10 s, then reducing the pressure to normal pressure at a rate of 15-18 MPa / min, maintaining the pressure for 3-5 min, increasing the pressure to 50-55 MPa within 0.1-0.5 s, maintaining the pressure for 5-6 s, then reducing the pressure to normal pressure at a rate of 20-22 MPa / min.

[0015] Furthermore, the present invention realizes instantaneous pressurization by compressing air with a high-pressure pump.

[0016] Furthermore, the specific gravity of the osmanthus extract is 1.1 to 1.3.

[0017] The osmanthus extract is prepared by the extraction method of the invention.

[0018] Compared with the prior art, the present invention has the following beneficial effects:

[0019] The present invention, in the process of extracting osmanthus extract, can effectively break the plant cell wall of osmanthus by combining the composite enzyme with suitable microwave and instantaneous pressurization process conditions to extract, so that the active components in osmanthus are quickly dissolved out, thereby effectively improving the extraction yield of osmanthus extract. In addition, the present invention is carried out at low temperature during the extraction process, which can also reduce the destruction of the active components in osmanthus, ensure the activity and stability of the extract, improve the content of flavonoids and other substances in osmanthus extract, and the osmanthus fragrance is rich and pure, effectively ensuring the product quality extracted from osmanthus extract.

[0020] The present invention adopts microwaves of different frequencies in combination with a reasonably matched enzymolysis solution to effectively shorten the enzymolysis time; and after microwave extraction, an ethanol solution is added for instantaneous pressurization treatment, which can more fully break the cell wall, thereby dissolving more active ingredients and effectively improving the extraction efficiency. DETAILED DESCRIPTION

[0021] In order to better understand the technical content of the present invention, specific embodiments are provided below to further illustrate the present invention.

[0022] Unless otherwise specified, the experimental methods used in the embodiments of the present invention are all conventional methods.

[0023] Unless otherwise specified, the materials, reagents, etc. used in the embodiments of the present invention can be obtained from commercial sources.

[0024] The β-glucosidase of the present invention was purchased from Wuhan Shuer Biotechnology Co., Ltd., and the enzyme activity was 30,000 U / g.

[0025] The xylanase of the present invention was purchased from Hubei Haijia Biotechnology Co., Ltd., and the enzyme activity was 50,000 U / g.

[0026] The pectinase of the present invention was purchased from Nanning Pangbo Bioengineering Co., Ltd., and the enzyme activity was 30,000 U / g.

[0027] The sweet osmanthus variety used in the embodiment of the present invention is silver osmanthus produced in Xianning City, Hubei Province, China.

[0028] Example 1

[0029] The method for extracting the sweet osmanthus extract of the present embodiment comprises the following steps:

[0030] S1, dehydrating fresh osmanthus by vacuum freeze drying, crushing into 50 meshes, and obtaining osmanthus powder;

[0031] S2, the enzymatic hydrolysate is prepared by mixing β-glucosidase, xylanase, pectinase and water in a mass ratio of 8:0.8:1.5:140; according to the g / mL ratio of osmanthus powder to enzymatic hydrolysate of 1:7, the osmanthus powder and the enzymatic hydrolysate are mixed and subjected to a microwave extraction for 25 minutes at a temperature of 40°C and a power of 250W; then, a second microwave extraction is carried out for 12 minutes at a temperature of 40°C and a power of 600W to obtain an enzymatic hydrolysate mixture;

[0032] S3. Take an ethanol solution with a mass concentration of 95% and an enzymatic hydrolysis mixture at a volume ratio of 1.5:1, add the ethanol solution to the enzymatic hydrolysis mixture for instantaneous pressure extraction, the instantaneous pressure process is: increase the pressure to 40MPa within 0.1-0.5s, maintain the pressure for 7s, then reduce the pressure to normal pressure at a rate of 15MPa / min, maintain the pressure for 3min, increase the pressure to 55MPa within 0.1-0.5s, maintain the pressure for 5s, then reduce the pressure to normal pressure at a rate of 20MPa / min, to obtain a mixed extract, filter the mixed extract to obtain the filtrate, concentrate it by rotary evaporation to remove ethanol, and concentrate to obtain an osmanthus extract with a specific gravity of 1.2.

[0033] Example 2

[0034] The method for extracting the sweet osmanthus extract of the present embodiment comprises the following steps:

[0035] S1, dehydrating fresh osmanthus by vacuum freeze drying, and crushing into 60 meshes to obtain osmanthus powder;

[0036] S2, the enzymatic hydrolysate is prepared by mixing β-glucosidase, xylanase, pectinase and water in a mass ratio of 5:1.2:2:150; the osmanthus powder and the enzymatic hydrolysate are mixed according to a solid-liquid ratio of g / mL of 1:8, and the osmanthus powder and the enzymatic hydrolysate are subjected to a microwave extraction at a temperature of 45°C and a power of 200W for 30min; and then a second microwave extraction is carried out at a temperature of 45°C and a power of 500W for 15min to obtain an enzymatic hydrolysate mixture;

[0037] S3. Take an ethanol solution with a mass concentration of 90% and an enzymatic hydrolysis mixture in a volume ratio of 1:1, add the ethanol solution to the enzymatic hydrolysis mixture for instantaneous pressure extraction, the instantaneous pressure process is: increase the pressure to 30MPa within 0.1-0.5s, maintain the pressure for 9s, then reduce the pressure to normal pressure at a rate of 18MPa / min, maintain the pressure for 4min, increase the pressure to 50MPa within 0.1-0.5s, maintain the pressure for 6s, then reduce the pressure to normal pressure at a rate of 22MPa / min, to obtain a mixed extract, filter the mixed extract to obtain the filtrate, concentrate it by rotary evaporation to remove ethanol, and concentrate to obtain an osmanthus extract with a specific gravity of 1.2.

[0038] Example 3

[0039] The method for extracting the sweet osmanthus extract of the present embodiment comprises the following steps:

[0040] S1, dehydrating fresh osmanthus by vacuum freeze drying, and crushing into 60 meshes to obtain osmanthus powder;

[0041] S2, the enzymatic hydrolysate is prepared by mixing β-glucosidase, xylanase, pectinase and water in a mass ratio of 7:1:1:130; according to the material-liquid ratio of osmanthus powder to enzymatic hydrolysate g / mL of 1:9, the osmanthus powder and the enzymatic hydrolysate are mixed and subjected to a microwave extraction for 27 minutes at a temperature of 30°C and a power of 250W; then a second microwave extraction is carried out for 14 minutes at a temperature of 30°C and a power of 550W to obtain an enzymatic hydrolysate mixture;

[0042] S3. Take an ethanol solution with a mass concentration of 93% and an enzymatic hydrolysis mixture at a volume ratio of 1.8:1, add the ethanol solution to the enzymatic hydrolysis mixture for instantaneous pressure extraction, the instantaneous pressure process is: increase the pressure to 35MPa within 0.1-0.5s, maintain the pressure for 8s, then reduce the pressure to normal pressure at a rate of 16MPa / min, maintain the pressure for 5min, increase the pressure to 50MPa within 0.1-0.5s, maintain the pressure for 5s, then reduce the pressure to normal pressure at a rate of 21MPa / min, to obtain a mixed extract, filter the mixed extract to obtain the filtrate, concentrate it by rotary evaporation to remove ethanol, and concentrate it to obtain an osmanthus extract with a specific gravity of 1.2.

[0043] Comparative Example 1

[0044] The difference between this comparative example and Example 1 is that the raw material ratio of the enzymatic hydrolyzate is changed, and the rest is consistent with Example 1.

[0045] The enzymatic hydrolysate of this comparative example comprises β-glucosidase, xylanase, pectinase and water in a mass ratio of 0.3:3:7:140.

[0046] Comparative Example 2

[0047] The difference between this comparative example and Example 1 is that the conditions of microwave extraction are changed, and the rest are the same as Example 1.

[0048] The extraction method of the osmanthus extract of this comparative example comprises the following steps:

[0049] S1, dehydrating fresh osmanthus by vacuum freeze drying, crushing into 50 meshes, and obtaining osmanthus powder;

[0050] S2, the enzymatic hydrolysate is prepared by mixing β-glucosidase, xylanase, pectinase and water in a mass ratio of 8:0.8:1.5:140; according to the g / mL ratio of osmanthus powder to enzymatic hydrolysate of 1:7, the osmanthus powder and the enzymatic hydrolysate are mixed and microwave extracted for 35 minutes at a temperature of 40°C and a power of 400W to obtain an enzymatic hydrolysate mixture;

[0051] S3. Take an ethanol solution with a mass concentration of 95% and an enzymatic hydrolysis mixture at a volume ratio of 1.5:1, add the ethanol solution to the enzymatic hydrolysis mixture for instantaneous pressure extraction, the instantaneous pressure process is: increase the pressure to 40MPa within 0.1-0.5s, maintain the pressure for 10s, then reduce the pressure to normal pressure at a rate of 15MPa / min, maintain it for 3min, increase the pressure to 55MPa within 0.1-0.5s, maintain the pressure for 5s, then reduce the pressure to normal pressure at a rate of 20MPa / min, to obtain a mixed extract, filter the mixed extract to obtain the filtrate, concentrate it by rotary evaporation to remove ethanol, and concentrate it to obtain an osmanthus extract with a specific gravity of 1.2.

[0052] Comparative Example 3

[0053] The difference between this comparative example and Example 1 is that it is not subjected to microwave extraction treatment, and the rest is consistent with Example 1.

[0054] The extraction method of the osmanthus extract of this comparative example comprises the following steps:

[0055] S1, dehydrating fresh osmanthus by vacuum freeze drying, crushing into 50 meshes, and obtaining osmanthus powder;

[0056] S2, the enzymatic hydrolysate is prepared by mixing β-glucosidase, xylanase, pectinase and water in a mass ratio of 8:0.8:1.5:140; the osmanthus powder and the enzymatic hydrolysate are mixed according to a material-liquid ratio of g / mL of 1:7, and the osmanthus powder and the enzymatic hydrolysate are enzymolyzed at a temperature of 40°C for 35 minutes to obtain an enzymatic hydrolysate mixture;

[0057] S3. Take an ethanol solution with a mass concentration of 95% and an enzymatic hydrolysis mixture at a volume ratio of 1.5:1, add the ethanol solution to the enzymatic hydrolysis mixture for instantaneous pressure extraction, the instantaneous pressure process is: increase the pressure to 40MPa within 0.1-0.5s, maintain the pressure for 7s, then reduce the pressure to normal pressure at a rate of 15MPa / min, maintain the pressure for 3min, increase the pressure to 55MPa within 0.1-0.5s, maintain the pressure for 5s, then reduce the pressure to normal pressure at a rate of 20MPa / min, to obtain a mixed extract, filter the mixed extract to obtain the filtrate, concentrate it by rotary evaporation to remove ethanol, and concentrate to obtain an osmanthus extract with a specific gravity of 1.2.

[0058] Comparative Example 4

[0059] The difference between this comparative example and Example 1 is that instantaneous pressurization is replaced by ultrahigh pressure treatment, and the rest is consistent with Example 1.

[0060] The extraction method of the osmanthus extract of this comparative example comprises the following steps:

[0061] S1, dehydrating fresh osmanthus by vacuum freeze drying, crushing into 50 meshes, and obtaining osmanthus powder;

[0062] S2, the enzymatic hydrolysate is prepared by mixing β-glucosidase, xylanase, pectinase and water in a mass ratio of 8:0.8:1.5:140; according to the g / mL ratio of osmanthus powder to enzymatic hydrolysate of 1:7, the osmanthus powder and the enzymatic hydrolysate are mixed and subjected to a microwave extraction for 25 minutes at a temperature of 40°C and a power of 250W; then, a second microwave extraction is carried out for 12 minutes at a temperature of 40°C and a power of 600W to obtain an enzymatic hydrolysate mixture;

[0063] S3. Take a 95% ethanol solution and an enzymatic hydrolysis mixture in a volume ratio of 1.5:1 and put them into an L2-600 / 2 ultrahigh pressure equipment for treatment. Set the extraction pressure to 300 MPa and maintain the pressure for 3 minutes to obtain a mixed extract. Filter the mixed extract to obtain the filtrate, concentrate it by rotary evaporation to remove ethanol, and concentrate to obtain an osmanthus extract with a specific gravity of 1.2.

[0064] The osmanthus extracts prepared in the above Examples 1-3 and Comparative Examples 1-4 were vacuum dried at 40° C. to a constant weight to obtain dried osmanthus extracts, and then the extraction yield of the dried osmanthus extracts was calculated using the following calculation formula:

[0065] C=M1 / M 0 ×100%,

[0066] Where: C is the extraction rate, %; M 1 is the mass of osmanthus extract after drying, g; M 0 is the mass of osmanthus powder, g.

[0067] The results are shown in Table 1 below:

[0068] Table 1 Extraction yield of osmanthus extract

[0069] Extraction yield / % Example 1 5.36 Example 2 5.25 Example 3 5.21 Comparative Example 1 4.93 Comparative Example 2 4.85 Comparative Example 3 4.27 Comparative Example 4 5.03

[0070] The above results show that the extraction method of Examples 1-3 of the present invention can improve the extraction yield of osmanthus extract. Compared with Example 1, Comparative Example 1 affects the enzymatic hydrolysis effect due to the inappropriate ratio of the raw materials of the enzymatic hydrolysis solution; compared with Example 1, Comparative Example 2 changes the microwave extraction process, Comparative Example 3 does not use microwave synergistic treatment during the extraction process, and Comparative Example 4 replaces the instantaneous pressurized extraction with ultra-high pressure treatment. Due to unreasonable extraction process conditions, the cell wall in osmanthus is not completely broken, and the active ingredients cannot be better dissolved, thereby reducing the extraction yield of osmanthus extract.

[0071] The sodium nitrite-aluminum nitrate colorimetric method was used to determine the mass content of total flavonoids in the osmanthus extracts extracted in Examples 1-3 of the present invention and Comparative Examples 1-4, and a standard working curve was prepared using rutin as a standard sample during the test. The test results are shown in Table 2 below.

[0072] Table 2 Total flavonoids content in osmanthus extract

[0073]

[0074]

[0075] The above results show that in the preparation process, Examples 1-3 of the present invention can effectively dissolve the active ingredients in osmanthus through a more reasonable enzymatic solution and the coordinated microwave and instantaneous pressurization, improve the extraction efficiency, and especially improve the content of total flavonoids. Examples 1-4 respectively change the raw material ratio of the enzymatic solution, change the conditions of microwave extraction, do not use microwave extraction treatment, and replace instantaneous pressurization extraction with ultra-high pressure treatment, resulting in less dissolution of active ingredients and large losses during the extraction process, and reduced extraction efficiency.

[0076] In addition, the osmanthus extracts of Examples 1-3 and Comparative Examples 1-4 dried to constant weight were subjected to a sensory evaluation, and it was found that the osmanthus extracts extracted in Examples 1-3 of the present invention were brown-yellow pastes with natural osmanthus aroma, and the aroma was rich and odorless. The sensory evaluation of the osmanthus extract prepared in Comparative Example 1 was not significantly different from that of Example 1, but compared with Example 1, the osmanthus extracts prepared in Comparative Examples 2-4 had a lighter aroma.

[0077] In summary, the extraction method of the present invention improves the extraction yield of osmanthus extract while also effectively ensuring the product quality of the osmanthus extract.

[0078] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for extracting osmanthus extract, characterized in that: The following steps are involved: S1, dehydrating fresh osmanthus by vacuum freeze drying, and crushing to obtain osmanthus powder; S2, after mixing the osmanthus powder with the enzymatic hydrolyzate, perform a microwave extraction for 25 to 30 minutes at a temperature of 30 to 45° C. and a power of 200 to 250 W; then perform a second microwave extraction for 12 to 15 minutes at a temperature of 30 to 45° C. and a power of 500 to 600 W to obtain an enzymatic hydrolyzate mixture; S3. Adding ethanol solution to the enzymatic hydrolysis mixture for instantaneous pressure extraction to obtain a mixed extract, filtering the mixed extract to obtain the filtrate, and concentrating the filtrate by rotary evaporation to remove ethanol, and concentrating to obtain osmanthus extract.

2. The method for extracting osmanthus extract according to claim 1, characterized in that: The particle size of the osmanthus powder is 50 to 60 meshes.

3. The method for extracting osmanthus extract according to claim 1, characterized in that: The material-liquid ratio of the osmanthus powder to the enzymatic hydrolysis liquid is 1:7-10 g / mL.

4. The method for extracting osmanthus extract according to claim 1, characterized in that: The enzymatic hydrolysate comprises beta-glucosidase, xylanase, pectinase and water in a mass ratio of 5-8:0.8-1.4:1-2:120-150.

5. The method for extracting osmanthus extract according to claim 1, characterized in that: The volume ratio of the ethanol solution to the enzymatic hydrolysis mixture is 1-1.8:1; the mass concentration of the ethanol solution is 90%-95%.

6. The method for extracting osmanthus extract according to claim 1, characterized in that: The instantaneous pressurization process is as follows: the pressure is increased to 30-40 MPa within 0.1-0.5 s, the pressure is maintained for 8-10 s, and then the pressure is reduced to normal pressure at a rate of 15-18 MPa / min, and the pressure is maintained for 3-5 min, and then the pressure is increased to 50-55 MPa within 0.1-0.5 s, and the pressure is maintained for 5-6 s, and then the pressure is reduced to normal pressure at a rate of 20-22 MPa / min.

7. The method for extracting osmanthus extract according to claim 1, characterized in that: The specific gravity of the osmanthus extract is 1.1 to 1.

3.

8. Osmanthus fragrans extract obtained by the extraction method according to any one of claims 1 to 7.

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