A kind of extraction process of Brazilian green propolis

Abstract

The invention discloses a Brazilian green propolis extraction process, which uses Brazilian green propolis as a raw material, extracts and residues after ultrasonic oscillation extraction with an ethanol aqueous solution, takes the residue and performs hydrogen activation treatment to obtain an activated residue, then disperses the activated residue in a magnetic field with the help of polyglycerol ricinoleate and medium-chain triglycerides, freezes under the action of a magnetic field to obtain frozen particles, finally adds the frozen particles to the extract, heats, cools naturally to room temperature, performs high pressure treatment, centrifuges to obtain a supernatant, and sprays to obtain the obtained product. The Brazilian green propolis powder obtained by the invention has good fluidity, is comprehensively rich in nutrients, and has broad market prospects.

Description

Technical Field

[0001] The invention belongs to the technical field of propolis extraction, and particularly relates to a process for extracting Brazilian green propolis. Background Art

[0002] Propolis is a colloidal solid with an aromatic smell. It is made from the gum collected by bees from plant buds and tree trunks, mixed with the secretions of the bees' palatine glands and beeswax. The chemical composition of propolis is extremely complex. It has multiple biological functions such as antioxidant, anti-inflammatory, anti-proliferative, anti-viral, and anti-aging. It is a health product and Chinese herbal medicine with great development value. Brazilian green propolis is one of the propolis products that is very popular among consumers. Since the production area of ​​Brazilian green propolis is located in the Amazon Basin in South America, it has the largest virgin forest in the world and a beautiful and pollution-free natural environment. Therefore, the content of effective ingredients in Brazilian green propolis products is high and the heavy metal pollution is low. The source of propolis is safe and guaranteed.

[0003] Flavonoids are one of the main functional ingredients of propolis, and the characteristic of domestic propolis is that the content of flavonoids is high. Compared with domestic propolis, Brazilian green propolis contains more terpenes, phytoncides, and aspirin C. Among them, isopentenyl phenylpropane and isopentenyl derivatives of p-coumaric acid are unique to Brazilian green propolis, which have strong immune regulation, promote cell regeneration and anti-cancer effects on the human body, and can be used to improve human health and prevent diseases, with broad market prospects.

[0004] Ethanol extraction is a common method for extracting propolis. However, after propolis is extracted and concentrated by ethanol, the extract obtained is very viscous and usually difficult to dry. In addition, the propolis extract contains a large amount of tannin components, such as gum and resin, which makes the extract less polar and easy to stick together, making it difficult to obtain a propolis powder product with good fluidity. Brazilian green propolis extraction also inevitably has this problem.

[0005] In addition, conventional ethanol extraction can easily lead to the loss of active substances in propolis, resulting in poor product quality, which cannot meet people's usage needs and is not conducive to large-scale production and promotion. In particular, the raw material cost of Brazilian green propolis is relatively high. The existing extraction process undoubtedly increases raw material expenses and causes great waste of resources.

[0006] Patent application CN115138099A discloses a method for preparing a propolis extract, comprising the following steps: S1. The propolis raw gel is graded and impurities removed, frozen and crushed, and sieved with a sieve of 80-120 mesh to obtain powdered propolis; S2. According to the mass ratio of powdered propolis: ethanol = 1: 10-15, ethanol with a concentration of 30-45% is added, and it is immersed at room temperature for 6-12 hours, and propolis extract A and a filtrate containing heavy metals are obtained after standing and filtering; S3. The propolis extract A is placed in a spray water washing tank for washing, and the residual ethanol is removed to obtain propolis extract B and a washing liquid; S4. According to the mass ratio of propolis extract B: alkaline aqueous solution = 1: 20-30, an alkaline aqueous solution with a pH value of 10-13.5 is added for microwave treatment, and the propolis extract is allowed to stand, filtered, and dried to obtain the propolis extract. The alkaline aqueous solution used in this patented technology is highly alkaline and has great destructive effect on the active substances in propolis. In addition, the aforementioned drying problem still exists, and drying is difficult, and the fluidity of the final product is poor.

[0007] Patent application CN111346112A discloses a method for extracting Brazilian green propolis by using ethanol at low temperature, comprising the following steps: step 1, taking raw material Brazilian green propolis, freezing it at low temperature for a period of time, and then crushing it at low temperature to 50-80 meshes to obtain a crushed material of Brazilian propolis; step 2, adding alcohol to the crushed material of Brazilian green propolis and soaking it once, filtering it to obtain a filtrate; soaking the filter residue twice, filtering it to obtain a filtrate; combining the two filtrates; step 3, decompressing and distilling the filtrate obtained in step 2, condensing it at low temperature and extracting it, and finally controlling the extraction temperature at below 55°C, recovering ethanol, and obtaining a propolis extract; step 4, dehydrating it at low temperature until the ethanol content is 1-3%; step 5, after the dehydration is completed, releasing the propolis extract with fluidity from the reactor, flowing it into a food-grade PE bag, weighing it, cooling it, fixing it into a shape, and packing it. This patented technology uses Brazilian green propolis as raw material for extraction, but it retains the flavonoids in Brazilian green propolis to the greatest extent, while neglecting the unique nutritional components of Brazilian green propolis, greatly reducing the quality of the product. Summary of the invention

[0008] In view of the shortcomings of the prior art, the purpose of the present invention is to provide a process for extracting Brazilian green propolis, which has good powder fluidity and rich nutritional ingredients.

[0009] In order to achieve the above object, the present invention adopts the following technical solution:

[0010] A Brazilian green propolis extraction process, the specific steps are as follows:

[0011] (1) firstly freeze-harden Brazilian green propolis and then crush it into 80-100 meshes to obtain raw material powder, then subject the raw material powder to ultrasonic oscillation extraction using 75-85% ethanol aqueous solution by volume concentration, centrifuge, and obtain an extract and a residue;

[0012] (2) subjecting the residue to hydrogen activation treatment to obtain an activated residue;

[0013] (3) then ultrasonically dispersing the activated residue in an ethanol aqueous solution with a volume concentration of 75-85% to obtain a premix; then adding polyglycerol ricinoleate to the medium chain triglyceride, stirring and mixing, then adding the premix, uniformly dispersing with ultrasonic oscillation, applying a magnetic field and freezing to obtain frozen particles;

[0014] (4) Finally, the frozen particles are added to the extract, heated, naturally cooled to room temperature, subjected to high pressure treatment, centrifuged to obtain the supernatant, and spray-dried to obtain Brazilian green propolis powder.

[0015] Preferably, in step (1), the freezing hardening process conditions are: treating at -25 to -30°C for 3 to 4 hours.

[0016] Preferably, in step (1), the mass ratio of the raw material powder to the ethanol aqueous solution is 1:8-10.

[0017] Preferably, in step (1), the process conditions of ultrasonic oscillation extraction are: frequency 30 to 40 kHz, and extraction time 20 to 30 minutes.

[0018] Preferably, the specific method of step (2) is: placing the residue in a sealed container, evacuating to a vacuum degree of ≤2Pa, and then introducing hydrogen to a pressure of 1 to 2×10 5 Pa, maintain the pressure for 3 to 4 hours, extract the hydrogen and heat to 60 to 70°C, keep warm for 40 to 50 minutes, and cool naturally to room temperature.

[0019] Preferably, in step (3), the mass ratio of the activated residue, the ethanol aqueous solution, the polyglycerol polyricinoleate, and the medium-chain triglyceride is 1:8-10:1.5-2.5:0.1-0.2.

[0020] Preferably, in step (3), the process conditions of ultrasonic oscillation dispersion are: 30-40 kHz ultrasonic oscillation dispersion for 40-50 minutes.

[0021] Preferably, in step (3), the magnetic field strength is 0.3 to 0.5 T, the freezing temperature is -25 to -30°C, and the processing time is 20 to 22 hours.

[0022] Preferably, in step (4), the process conditions for the heating treatment are: heating to 60-65° C. at a rate of 10-15° C. / min, and stirring at this temperature for 30-40 minutes.

[0023] Preferably, in step (4), the process conditions of high pressure treatment are: 500-600 MPa high pressure treatment for 5-7 minutes.

[0024] Preferably, in step (4), the process conditions for spray drying are: inlet air temperature 60-70°C, outlet air temperature 35-45°C, air volume 100-110m 3 / h, liquid intake 180~200mL / h.

[0025] Compared with the prior art, the present invention has the following beneficial effects:

[0026] The invention uses Brazilian green propolis as a raw material, extracts and residues after ultrasonic oscillation extraction with an ethanol aqueous solution, takes the residue and performs hydrogen activation treatment to obtain an activated residue, then disperses the activated residue in a magnetic field with the help of polyglycerol ricinoleate and medium-chain triglyceride, freezes under the action of a magnetic field to obtain frozen particles, finally adds the frozen particles to the extract, heats, cools naturally to room temperature, performs high pressure treatment, centrifuges to obtain a supernatant, and sprays and dries to obtain Brazilian green propolis powder. The Brazilian green propolis powder obtained by the invention has good fluidity, is comprehensively rich in nutrients, and has broad market prospects.

[0027] The specific analysis is as follows:

[0028] 1. The present invention freezes and hardens Brazilian green propolis and then crushes it into raw material powder with a particle size of 80 to 100 meshes, which is conducive to the release and extraction of nutrients in Brazilian green propolis and improves the extraction effect.

[0029] 2. The raw powder is subjected to ultrasonic oscillation extraction with an ethanol aqueous solution having a volume concentration of 75-85%. Most of the nutrients enter the extract, but some nutrients still remain in the residue. Therefore, the present application continues to extract the residue.

[0030] 3. After the residue is treated with hydrogen activation, on the one hand, the free radicals in the residue are reduced, the antioxidant capacity is improved, and the nutrients are prevented from being destroyed. On the other hand, it has an activation effect on the enzyme components in propolis and promotes the subsequent extraction process.

[0031] 4. Ultrasonic dispersion of the activated residue in an ethanol aqueous solution with a volume concentration of 75-85% to obtain a premix; then polyglycerol ricinoleate is added to the medium-chain triglyceride, stirred and mixed, and then the premix is ​​added, ultrasonic vibration is used to disperse it evenly, and a magnetic field is applied and frozen to obtain frozen particles. In this process, the premix is ​​used as the water phase, and polyglycerol ricinoleate and medium-chain triglyceride constitute the oil phase. After mixing, an emulsion is formed, and freezing is performed under the action of a magnetic field. The activated residue plays a role similar to a crystal nucleus, promoting the formation of a "small ice crystal" structure.

[0032] Frozen particles with a "small ice crystal" structure are added to the extract. During the heating process, the extract penetrates into the frozen particles and slowly melts. The viscosity of the system is low. Combined with the subsequent high-pressure treatment, the nutrients are fully extracted, and the final powder product has good fluidity. DETAILED DESCRIPTION

[0033] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments 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.

[0034] Unless otherwise specified, all commodities in this invention are purchased through market channels.

[0035] Example 1

[0036] A Brazilian green propolis extraction process, the specific steps are as follows:

[0037] (1) firstly freeze-harden Brazilian green propolis and then crush it into 80 meshes to obtain raw material powder, then subject the raw material powder to ultrasonic oscillation extraction using 75% ethanol aqueous solution with a volume concentration of 8 times its weight, and centrifuge to obtain an extract and a residue;

[0038] (2) The residue is then placed in a sealed container and evacuated to a vacuum degree of ≤2 Pa, followed by the introduction of hydrogen gas to a pressure of 1×10 5 Pa, maintain the pressure for 3 hours, evacuate the hydrogen and heat to 60 ° C, keep the temperature for 40 minutes, and cool naturally to room temperature to obtain an activated residue;

[0039] (3) Then, 1 kg of the activated residue is ultrasonically dispersed in 8 kg of 75% ethanol aqueous solution to obtain a premix; then, 1.5 kg of polyglycerol ricinoleate is added to the medium chain triglyceride, stirred and mixed, and then the premix is ​​added, ultrasonically dispersed evenly, and a magnetic field is applied and frozen to obtain frozen particles;

[0040] (4) Finally, the frozen particles obtained in step (3) are added to the extract obtained in step (1), subjected to heating treatment, naturally cooled to room temperature, subjected to high pressure treatment, centrifuged to obtain the supernatant, and spray-dried to obtain Brazilian green propolis powder.

[0041] Wherein, in step (1), the process conditions for freeze hardening are: treatment at -25°C for 3 hours.

[0042] In step (1), the process conditions of ultrasonic oscillation extraction are: frequency 30 kHz, extraction time 20 minutes.

[0043] In step (3), the process conditions of ultrasonic oscillation dispersion are: 30kHz ultrasonic oscillation dispersion for 40 minutes.

[0044] In step (3), the magnetic field strength is 0.3 T, the freezing temperature is -25°C, and the processing time is 20 hours.

[0045] In step (4), the process conditions for the heating treatment are: heating to 60°C at 10°C / min, and stirring at this temperature for 30 minutes.

[0046] In step (4), the process conditions for high pressure treatment are: 500 MPa high pressure treatment for 5 minutes.

[0047] In step (4), the process conditions of spray drying are: inlet air temperature 60°C, outlet air temperature 35°C, air volume 100m 3 / h, liquid intake 180mL / h.

[0048] Example 2

[0049] A Brazilian green propolis extraction process, the specific steps are as follows:

[0050] (1) firstly freeze-harden Brazilian green propolis and then crush it into 100 meshes to obtain raw powder, then subject the raw powder to ultrasonic oscillation extraction using 85% ethanol aqueous solution with a volume concentration of 10 times its weight, and centrifuge to obtain an extract and a residue;

[0051] (2) The residue is then placed in a sealed container and evacuated to a vacuum degree of ≤2Pa, followed by the introduction of hydrogen to a pressure of 2×10 5 Pa, keep the pressure for 4 hours, evacuate the hydrogen and heat to 70 ° C, keep the temperature for 50 minutes, and cool naturally to room temperature to obtain an activated residue;

[0052] (3) Then, 1 kg of the activated residue is ultrasonically dispersed in 10 kg of 85% ethanol aqueous solution to obtain a premix; then, 2.5 kg of polyglycerol polyricinoleate is added to the medium chain triglyceride, stirred and mixed, and then the premix is ​​added, ultrasonically dispersed evenly, and a magnetic field is applied and frozen to obtain frozen particles;

[0053] (4) Finally, the frozen particles obtained in step (3) are added to the extract obtained in step (1), subjected to heating treatment, naturally cooled to room temperature, subjected to high pressure treatment, centrifuged to obtain the supernatant, and spray-dried to obtain Brazilian green propolis powder.

[0054] Wherein, in step (1), the process conditions for freeze hardening are: treatment at -30°C for 4 hours.

[0055] In step (1), the process conditions of ultrasonic oscillation extraction are: frequency 40 kHz, extraction time 30 minutes.

[0056] In step (3), the process conditions of ultrasonic oscillation dispersion are: 40kHz ultrasonic oscillation dispersion for 50 minutes.

[0057] In step (3), the magnetic field strength is 0.5 T, the freezing temperature is -30°C, and the processing time is 22 hours.

[0058] In step (4), the process conditions for the heating treatment are: heating to 65°C at 15°C / min, and stirring at this temperature for 40 minutes.

[0059] In step (4), the process conditions for high pressure treatment are: 600 MPa high pressure treatment for 7 minutes.

[0060] In step (4), the process conditions of spray drying are: inlet air temperature 70°C, outlet air temperature 45°C, air volume 110m 3 / h, liquid intake 200mL / h.

[0061] Example 3

[0062] A Brazilian green propolis extraction process, the specific steps are as follows:

[0063] (1) firstly freeze-harden Brazilian green propolis and then crush it into 80 meshes to obtain raw powder, then subject the raw powder to ultrasonic oscillation extraction using 75% ethanol aqueous solution with a volume concentration of 10 times its weight, and centrifuge to obtain an extract and a residue;

[0064] (2) The residue is then placed in a sealed container and evacuated to a vacuum degree of ≤2Pa, followed by the introduction of hydrogen to a pressure of 2×10 5 Pa, maintain the pressure for 3 hours, evacuate the hydrogen and heat to 70 ° C, keep the temperature for 40 minutes, and cool naturally to room temperature to obtain an activated residue;

[0065] (3) Then, 1 kg of the activated residue is ultrasonically dispersed in 10 kg of 75% ethanol aqueous solution to obtain a premix; then, 2.5 kg of polyglycerol polyricinoleate is added to the medium chain triglyceride, stirred and mixed, and then the premix is ​​added, ultrasonically dispersed evenly, and a magnetic field is applied and frozen to obtain frozen particles;

[0066] (4) Finally, the frozen particles obtained in step (3) are added to the extract obtained in step (1), subjected to heating treatment, naturally cooled to room temperature, subjected to high pressure treatment, centrifuged to obtain the supernatant, and spray-dried to obtain Brazilian green propolis powder.

[0067] Wherein, in step (1), the process conditions for freeze hardening are: treatment at -25°C for 4 hours.

[0068] In step (1), the process conditions of ultrasonic oscillation extraction are: frequency 30 kHz, extraction time 30 minutes.

[0069] In step (3), the process conditions of ultrasonic oscillation dispersion are: 30kHz ultrasonic oscillation dispersion for 50 minutes.

[0070] In step (3), the magnetic field strength is 0.3 T, the freezing temperature is -30°C, and the processing time is 20 hours.

[0071] In step (4), the process conditions for the heating treatment are: heating to 60°C at 15°C / min, and stirring at this temperature for 40 minutes.

[0072] In step (4), the process conditions for high pressure treatment are: 500 MPa high pressure treatment for 7 minutes.

[0073] In step (4), the process conditions of spray drying are: inlet air temperature 60°C, outlet air temperature 45°C, air volume 100m 3 / h, liquid intake 200mL / h.

[0074] Example 4

[0075] A Brazilian green propolis extraction process, the specific steps are as follows:

[0076] (1) firstly freeze-harden Brazilian green propolis and then crush it into 90 meshes to obtain raw material powder, then subject the raw material powder to ultrasonic oscillation extraction using 80% ethanol aqueous solution with a volume concentration of 9 times its weight, and centrifuge to obtain an extract and a residue;

[0077] (2) The residue is then placed in a sealed container and evacuated to a vacuum degree of ≤2 Pa, followed by the introduction of hydrogen to a pressure of 1.5×10 5 Pa, maintain the pressure for 3.5 hours, evacuate the hydrogen and heat to 65 ° C, keep the temperature for 45 minutes, and cool naturally to room temperature to obtain an activated residue;

[0078] (3) Then, 1 kg of the activated residue is ultrasonically dispersed in 9 kg of 80% ethanol aqueous solution to obtain a premix; then, 2 kg of polyglycerol ricinoleate is added to the medium chain triglyceride, stirred and mixed, and then the premix is ​​added, ultrasonically dispersed evenly, and a magnetic field is applied and frozen to obtain frozen particles;

[0079] (4) Finally, the frozen particles obtained in step (3) are added to the extract obtained in step (1), subjected to heating treatment, naturally cooled to room temperature, subjected to high pressure treatment, centrifuged to obtain the supernatant, and spray-dried to obtain Brazilian green propolis powder.

[0080] Wherein, in step (1), the freezing hardening process conditions are: treatment at -28°C for 3.5 hours.

[0081] In step (1), the process conditions of ultrasonic oscillation extraction are: frequency 35 kHz, extraction time 25 minutes.

[0082] In step (3), the process conditions of ultrasonic oscillation dispersion are: 35kHz ultrasonic oscillation dispersion for 45 minutes.

[0083] In step (3), the magnetic field strength is 0.4 T, the freezing temperature is -28°C, and the processing time is 21 hours.

[0084] In step (4), the process conditions for the heating treatment are: heating to 63°C at 12°C / min, and stirring at this temperature for 35 minutes.

[0085] In step (4), the process conditions for high pressure treatment are: 600 MPa high pressure treatment for 6 minutes.

[0086] In step (4), the process conditions of spray drying are: inlet air temperature 65°C, outlet air temperature 40°C, air volume 105m 3 / h, liquid intake 190mL / h.

[0087] Comparative Example 1

[0088] A Brazilian green propolis extraction process, the specific steps are as follows:

[0089] (1) firstly freeze-harden Brazilian green propolis and then crush it into 80 meshes to obtain raw material powder, then subject the raw material powder to ultrasonic oscillation extraction using 75% ethanol aqueous solution with a volume concentration of 8 times its weight, and centrifuge to obtain an extract and a residue;

[0090] (2) Then, 1 kg of the residue is ultrasonically dispersed in 8 kg of 75% ethanol aqueous solution to obtain a premix; 1.5 kg of polyglycerol polyricinoleate is added to the medium chain triglyceride, stirred and mixed, and then the premix is ​​added, ultrasonically dispersed evenly, and a magnetic field is applied and frozen to obtain frozen particles;

[0091] (3) Finally, the frozen particles obtained in step (2) are added to the extract obtained in step (1), subjected to heating treatment, naturally cooled to room temperature, subjected to high pressure treatment, centrifuged to obtain the supernatant, and spray-dried to obtain Brazilian green propolis powder.

[0092] Wherein, in step (1), the process conditions for freeze hardening are: treatment at -25°C for 3 hours.

[0093] In step (1), the process conditions of ultrasonic oscillation extraction are: frequency 30 kHz, extraction time 20 minutes.

[0094] In step (2), the process conditions of ultrasonic oscillation dispersion are: 30kHz ultrasonic oscillation dispersion for 40 minutes.

[0095] In step (2), the magnetic field strength is 0.3 T, the freezing temperature is -25°C, and the processing time is 20 hours.

[0096] In step (3), the process conditions for the heating treatment are: heating to 60°C at 10°C / min, and stirring at this temperature for 30 minutes.

[0097] In step (3), the process conditions for high pressure treatment are: 500 MPa high pressure treatment for 5 minutes.

[0098] In step (3), the process conditions of spray drying are: inlet air temperature 60°C, outlet air temperature 35°C, air volume 100m 3 / h, liquid intake 180mL / h.

[0099] Comparative Example 2

[0100] A Brazilian green propolis extraction process, the specific steps are as follows:

[0101] (1) firstly freeze-harden Brazilian green propolis and then crush it into 80 meshes to obtain raw material powder, then subject the raw material powder to ultrasonic oscillation extraction using 75% ethanol aqueous solution with a volume concentration of 8 times its weight, and centrifuge to obtain an extract and a residue;

[0102] (2) The residue is then placed in a sealed container and evacuated to a vacuum degree of ≤2 Pa, followed by the introduction of hydrogen gas to a pressure of 1×10 5 Pa, maintain the pressure for 3 hours, evacuate the hydrogen and heat to 60 ° C, keep the temperature for 40 minutes, and cool naturally to room temperature to obtain an activated residue;

[0103] (3) Finally, the activated residue obtained in step (2) is added to the extract obtained in step (1), subjected to heating treatment, naturally cooled to room temperature, subjected to high pressure treatment, centrifuged to obtain the supernatant, and spray-dried to obtain Brazilian green propolis powder.

[0104] Wherein, in step (1), the process conditions for freeze hardening are: treatment at -25°C for 3 hours.

[0105] In step (1), the process conditions of ultrasonic oscillation extraction are: frequency 30 kHz, extraction time 20 minutes.

[0106] In step (3), the process conditions for the heating treatment are: heating to 60°C at 10°C / min, and stirring at this temperature for 30 minutes.

[0107] In step (3), the process conditions for high pressure treatment are: 500 MPa high pressure treatment for 5 minutes.

[0108] In step (3), the process conditions of spray drying are: inlet air temperature 60°C, outlet air temperature 35°C, air volume 100m 3 / h, liquid intake 180mL / h.

[0109] The performance of the Brazilian green propolis powder obtained in Examples 1 to 4 and Comparative Examples 1 and 2 was tested respectively, and the specific method is as follows:

[0110] 1. Powder fluidity

[0111] With reference to GB / T 11986-89 "Measurement of the angle of repose of surfactant powders and particles", the angle of repose was measured using the JT6098 angle of repose tester (Shanghai Jinte Testing Equipment Co., Ltd.). The angle of repose is the maximum angle formed between the free slope of a certain amount of powder layer and the horizontal plane.

[0112] The test results are shown in Table 1.

[0113] Table 1. Powder flowability test results

[0114] Angle of repose(°) Example 1 35.2 Example 2 35.3 Example 3 34.8 Example 4 34.3 Comparative Example 1 45.7 Comparative Example 2 48.9

[0115] 2. Nutritional testing

[0116] With reference to "Study on the Determination Method of Total Flavonoids in Health Foods" (Yu Cun et al., Chinese Journal of Health Inspection, Vol. 12, No. 4, August 2002, pp. 401-402), the total flavonoid content in the Brazilian green propolis powder obtained in Examples 1 to 4 of the present application and Comparative Examples 1 and 2 was detected.

[0117] The contents of chlorogenic acid and aspirin C in the Brazilian green propolis powder obtained in Examples 1 to 4 and Comparative Examples 1 and 2 of the present application were detected by referring to the method described in Example 1 of Patent CN105929074B "A method for controlling the quality of Brazilian green propolis".

[0118] The test results are shown in Table 2.

[0119] Table 2. Nutritional composition test results

[0120] Total flavonoids (%) Chlorogenic acid (mg / 100g) Acepyrine C (mg / 100g) Example 1 25.2 425 403 Example 2 25.3 427 404 Example 3 25.6 430 409 Example 4 26.2 437 416 Comparative Example 1 20.3 417 397 Comparative Example 2 19.5 410 390

[0121] It can be seen from Table 1 and Table 2 that the Brazilian green propolis powder obtained in Examples 1 to 4 has good fluidity, high contents of total flavonoids, chlorogenic acid and aspirin C, and is comprehensive and rich in nutrition.

[0122] In Comparative Example 1, the hydrogen activation treatment was omitted, and in Comparative Example 2, the freezing step of the activated residue was omitted. The fluidity of the obtained Brazilian green propolis powder was significantly deteriorated and the nutrient content was reduced, indicating that the synergistic effects of the residue activation treatment and the freezing treatment under magnetic field conditions helped to improve the extraction effect and the powder fluidity.

[0123] The present invention illustrates the technical concept of the present invention through the above-mentioned embodiments, but the present invention is not limited to the above-mentioned embodiments, that is, it does not mean that the present invention must rely on the above-mentioned embodiments to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of individual raw materials of the product of the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

Claims

1. A process for extracting Brazilian green propolis, characterized in that: The specific steps are as follows: (1) First, the Brazilian green propolis is frozen and hardened, and then crushed into 80-100 meshes to obtain a raw material powder, and then the raw material powder is subjected to ultrasonic oscillation extraction using an ethanol aqueous solution with a volume concentration of 75-85%, and centrifuged to obtain an extract and a residue; (2) subjecting the residue to hydrogen activation treatment to obtain an activated residue; (3) Then, the activated residue is ultrasonically dispersed in an ethanol aqueous solution with a volume concentration of 75-85% to obtain a premix; then, polyglycerol ricinoleate is added to the medium chain triglyceride, stirred and mixed, and then the premix is ​​added, ultrasonically dispersed evenly, and a magnetic field is applied and frozen to obtain frozen particles; (4) Finally, the frozen particles are added to the extract, heated, naturally cooled to room temperature, subjected to high pressure treatment, centrifuged to obtain the supernatant, and spray dried to obtain Brazilian green propolis powder; In step (1), the freezing and hardening process conditions are: -25 to -30 ° C for 3 to 4 hours; The specific method of step (2) is: placing the residue in a sealed container, evacuating to a vacuum degree of ≤2Pa, and then introducing hydrogen to a pressure of 1 to 2×10 5 Pa, maintain the pressure for 3 to 4 hours, extract the hydrogen and heat to 60 to 70 ° C, keep warm for 40 to 50 minutes, and cool naturally to room temperature; In step (3), the mass ratio of the activated residue, the ethanol aqueous solution, the polyglycerol polyricinoleate, and the medium chain triglyceride is 1:8-10:1.5-2.5:0.1-0.2; In step (3), the process conditions of ultrasonic oscillation dispersion are: 30-40kHz ultrasonic oscillation dispersion for 40-50 minutes; In step (3), the magnetic field strength is 0.3 to 0.5 T, the freezing temperature is -25 to -30°C, and the processing time is 20 to 22 hours.

2. The extraction process of Brazilian green propolis according to claim 1, characterized in that: In step (1), the mass ratio of the raw material powder to the ethanol aqueous solution is 1:8-10.

3. The extraction process of Brazilian green propolis according to claim 1, characterized in that: In step (1), the process conditions of ultrasonic oscillation extraction are: frequency 30 to 40 kHz, and extraction time 20 to 30 minutes.

4. The extraction process of Brazilian green propolis according to claim 1, characterized in that: In step (4), the process conditions of the heating treatment are: heating to 60-65°C at 10-15°C / min, and stirring at this temperature for 30-40 minutes; The process conditions of high pressure treatment are: 500-600Mpa high pressure treatment for 5-7 minutes.

5. The extraction process of Brazilian green propolis according to claim 1, characterized in that: In step (4), the process conditions for spray drying are: inlet air temperature 60-70°C, outlet air temperature 35-45°C, air volume 100-110m 3 / h, liquid intake 180~200mL / h.