Preparation method of black ginseng extract powder rich in rare ginsenosides

Abstract

The present application relates to the technical field of plant extract, and specifically discloses a preparation method of black ginseng extract powder rich in rare ginsenosides, which comprises the following steps: step 1), crushing black ginseng, putting it into water, keeping the temperature at 75-85 DEG C, soaking for 1.5-2.5 h, filtering, discarding the filtrate, and obtaining black ginseng particles; step 2), putting the black ginseng particles and water into a container, passing in carbon dioxide to increase the pressure to 0.15-0.25 MPa, keeping the temperature at 105-125 DEG C, extracting for 0.5-2 h, filtering while hot, and obtaining an extract; and step 3), concentrating and drying the extract, and obtaining black ginseng extract powder rich in rare ginsenosides. The present application has the advantage of improving the purity of rare ginsenosides.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of plant extracts, in particular to a preparation method of black ginseng extract powder rich in rare ginsenosides. BACKGROUND

[0002] Black ginseng is a black or dark brown product processed by repeated steaming and drying of ginseng (Panax ginseng C.A.Mey.). During the processing, ginsenosides are converted into rare ginsenosides (such as rare ginsenoside Rg3), which have the effects of anti-tumor, enhancing immunity, anti-fatigue, controlling weight, anti-aging, beauty, reducing blood sugar, and improving memory.

[0003] The existing method for extracting rare ginsenosides is mainly alcohol extraction, but in the food field, alcohol extraction cannot be used according to GB / T31326-2014 "Plant Beverages", which leads to the use of water extraction for extracting rare ginsenosides in the food field. However, the water solubility of rare ginsenosides is poor, which leads to the dissolution of a large amount of acidic polysaccharides (containing low-carbon sugars), water-soluble polypeptides, amino acids, glycoproteins, pigments and other impurities during water extraction, resulting in low purity of rare ginsenosides in the extract. Therefore, there is still room for improvement. SUMMARY

[0004] In order to improve the purity of rare ginsenosides, the present application provides a preparation method of black ginseng extract powder rich in rare ginsenosides.

[0005] The preparation method of black ginseng extract powder rich in rare ginsenosides provided by the present application adopts the following technical scheme:

[0006] A preparation method of black ginseng extract powder rich in rare ginsenosides, comprising the following steps:

[0007] Step 1), crushing black ginseng, putting it into water, constant temperature 75-85℃, soaking for 1.5-2.5h, filtering, discarding the filtrate, and obtaining black ginseng particles;

[0008] Step 2), putting the black ginseng particles and water into a container, introducing carbon dioxide to increase the pressure to 0.15-0.25MPa, constant temperature 105-125℃, extracting for 0.5-2h, and filtering while hot to obtain an extract;

[0009] Step 3), concentrating and drying the extract to obtain black ginseng extract powder rich in rare ginsenosides.

[0010] By adopting the above technical solution, black ginseng is first soaked in water at 75-85℃, which allows some of the impurities such as acidic polysaccharides (including low-carbon sugars), water-soluble polypeptides, amino acids, glycoproteins, and pigments in the black ginseng to dissolve into the water, thus achieving preliminary impurity removal. Then, during the extraction process, carbon dioxide is introduced to increase the pressure, turning the water into a dilute carbonic acid solution. The black ginseng particles are extracted under special pressure and temperature, which significantly improves the water solubility of rare ginsenosides, making them very easy to dissolve. Combined with a special extraction time, the content of rare ginsenosides in the extracted extract is significantly increased, thereby effectively and significantly improving the purity of rare ginsenosides in the extract. The product quality is better, and because water extraction is used, it complies well with the regulations of food industry laws and regulations, and has a wider range of applications.

[0011] Preferably, in step 2), carbon dioxide is introduced to increase the pressure to 0.2-0.22 MPa, and the extraction is carried out at a constant temperature of 115-122℃ for 1.5-1.8 hours.

[0012] By adopting the above technical solution, specifically selecting a pressure of 0.2-0.22 MPa, a constant temperature of 115-122℃, and an extraction time of 1.5-1.8 h, the content of rare ginsenosides in the extract can be further increased, resulting in higher purity of rare ginsenosides.

[0013] Preferably, in step 2), when carbon dioxide is introduced, the carbon dioxide is introduced into the water, and the air in the container is discharged at the same time as the carbon dioxide is introduced, and then the container is sealed to increase the pressure.

[0014] By adopting the above technical solution, the oxygen content can be reduced by venting the air in the container, thereby reducing oxidation during the high-temperature extraction process and resulting in higher quality rare ginsenosides.

[0015] Preferably, in step 2), the ratio of the mass of black ginseng particles to the mass of water is 1:5-20.

[0016] By adopting the above technical solution and specifically selecting the mass ratio of black ginseng granules to water, the rare ginsenosides in the black ginseng granules are more easily dissolved in water, effectively improving the extraction efficiency and the purity of rare ginsenosides.

[0017] Preferably, in step 3), the extract is cooled before concentration and drying. During cooling, the temperature is reduced to 3-5°C at a rate of 10-11°C / min before concentration and drying.

[0018] By adopting the above technical solution, and rapidly cooling to 3-5℃ at a rate of 10-11℃ / min, the water solubility stability of rare ginsenosides at room temperature can be greatly increased during the rapid cooling process. This allows the extract to dissolve better in water and is less prone to precipitation when left to stand, thus making it more suitable for the food industry and improving the quality of the extract.

[0019] Preferably, after cooling to 3-5℃, the temperature is maintained at 3-5℃ for 4-10 hours.

[0020] By adopting the above technical solution, and by cooling to 3-5℃ and then maintaining the temperature for 4-10 hours, the water solubility of rare ginsenosides at room temperature is increased, making them more suitable for application in the food industry.

[0021] Preferably, in step 1), the particle size of the black ginseng particles is 0.5-1cm.

[0022] By adopting the above technical solution and specifically selecting the particle size of black ginseng granules, rare ginsenosides in black ginseng granules are more easily extracted, thereby improving extraction efficiency.

[0023] Preferably, in step 2), 80-100 mesh filter cloth is used for pressure filtration.

[0024] By adopting the above technical solution and specifically selecting 80-100 mesh filter cloth, the effect of filtering drug residue is better, and the filtration efficiency is higher. Through pressure filtration, the waste of extract can be reduced, resulting in higher economic value.

[0025] In summary, this application has the following beneficial effects:

[0026] 1. This application achieves preliminary impurity removal by first soaking black ginseng in water at 75-85℃, which allows some of the impurities such as acidic polysaccharides (including low-carbon sugars), water-soluble polypeptides, amino acids, glycoproteins, and pigments in the black ginseng to dissolve into the water. Then, during the extraction process, carbon dioxide is introduced to increase the pressure, turning the water into a dilute carbonic acid solution. The black ginseng particles are extracted under special pressure and temperature, which significantly improves the water solubility of rare ginsenosides, making them very easy to dissolve. Combined with a special extraction time, the content of rare ginsenosides in the extracted extract is significantly increased, thereby effectively and significantly improving the purity of rare ginsenosides in the extract. The product quality is better, and because water extraction is used, it complies well with the regulations and laws in the food industry, and has a wider range of applications.

[0027] 2. In this application, it is preferred to select a specific extraction pressure of 0.2-0.22 MPa, a constant temperature of 115-122℃, and an extraction time of 1.5-1.8 h, which can further increase the content of rare ginsenosides in the extract, resulting in higher purity of rare ginsenosides.

[0028] 3. In this application, it is preferred to rapidly cool down to 3-5℃ at a rate of 10-11℃ / min. During the rapid cooling process, the water solubility stability of rare ginsenosides at room temperature can be greatly increased, so that the extract can dissolve better when added to water and is less likely to precipitate when left to stand. This makes it more suitable for the food industry and improves the quality of the extract. Attached Figure Description

[0029] Figures 1-8 The high-performance liquid chromatograms of ginsenoside black ginseng extract powder in Examples 1-8 are shown below.

[0030] Figures 9-16 The high-performance liquid chromatograms of ginsenoside black ginseng extract powders of comparative examples 1-8 are shown in the figure.

[0031] Figures 17-24 These are photographs showing the water solubility stability test results of ginsenoside black ginseng extract powder in Examples 1-8.

[0032] Figures 25-32 Photographs showing the water solubility stability test results of ginsenoside black ginseng extract powders (comparative examples 1-8). Detailed Implementation

[0033] The present application will be further described in detail below with reference to the embodiments.

[0034] Example 1

[0035] A method for preparing black ginseng extract powder rich in rare ginsenosides, the specific steps of which are as follows:

[0036] Step 1): Put 1 kg of black ginseng into a grinder and grind it. Pass it through a 0.5 cm sieve and take the particles that do not pass through the sieve. Then pass it through a 1 cm sieve and take the particles that pass through the sieve. Put them into 4 kg of water and soak them at a constant temperature of 75℃ for 1.5 hours. Filter and discard the filtrate to obtain black ginseng particles with a particle size of 0.5-1 cm.

[0037] Step 2): Add 1 kg of black ginseng granules and 5 kg of deionized water to the reactor. Introduce carbon dioxide into the deionized water to expel air. The carbon dioxide introduce rate is 1 L / min. After the carbon dioxide introduce reaches twice the volume of the reactor, seal the reactor and continue to introduce carbon dioxide to increase the pressure inside the reactor to 0.15 MPa. Heat the reactor to prepare deionized water at 105℃ and extract at a constant temperature of 105℃ for 0.5 h. Discharge the solid-liquid mixture from the reactor into a plate and frame filter press and filter while hot to obtain the extract. The filter cloth specification is 80 mesh and the pressure is 1 MPa.

[0038] Step 3): After the extract is naturally cooled to room temperature, it is concentrated by rotary evaporation at a vacuum of -0.06 MPa and a temperature of 70°C until it becomes a paste. The paste is then air-dried at room temperature to obtain black ginseng extract powder rich in rare ginsenosides.

[0039] Among them, the black ginseng is homemade, and the preparation method of black ginseng is as follows:

[0040] Spread the ginseng evenly on a steaming tray and place it in a continuous steaming-drying integrated equipment. Turn on the steam, control the temperature at 115℃, and steam for 2.5 hours. Release the steam and automatically move the steaming tray to the drying area. Dry at 90℃ for 4 hours. Take it out and repeat the above operation 8 times to obtain black ginseng.

[0041] Example 2

[0042] A method for preparing black ginseng extract powder rich in rare ginsenosides, the specific steps of which are as follows:

[0043] Step 1): Put the black ginseng into a grinder and grind it. Pass it through a 0.5cm sieve and take the particles that do not pass through the sieve. Then pass it through a 1cm sieve and take the particles that pass through the sieve. Put them into 6kg of water, keep the temperature at 78℃, soak for 1.8h, filter, discard the filtrate, and you will get black ginseng particles with a particle size of 0.5-1cm.

[0044] Step 2): Add 1 kg of black ginseng granules and 10 kg of deionized water to the reactor. Introduce carbon dioxide into the deionized water to expel air. The carbon dioxide introduce rate is 1 L / min. After the carbon dioxide introduce reaches twice the volume of the reactor, seal the reactor and continue to introduce carbon dioxide to increase the pressure inside the reactor to 0.2 MPa. Heat the reactor to prepare deionized water at 115℃ and extract at a constant temperature of 115℃ for 1.5 h. Discharge the solid-liquid mixture from the reactor into a plate and frame filter press and filter while hot to obtain the extract. The filter cloth specification is 80 mesh and the pressure is 1 MPa.

[0045] Step 3): After the extract is naturally cooled to room temperature, it is concentrated by rotary evaporation at a vacuum of -0.07 MPa and a temperature of 68°C until it becomes a paste. The paste is then air-dried at room temperature to obtain black ginseng extract powder rich in rare ginsenosides.

[0046] Among them, the black ginseng is homemade, and the preparation method of black ginseng is as follows:

[0047] Spread the ginseng evenly on a steaming tray and place it in a continuous steaming-drying integrated equipment. Turn on the steam, control the temperature at 115℃, and steam for 2.5 hours. Release the steam and automatically move the steaming tray to the drying area. Dry at 90℃ for 4 hours. Take it out and repeat the above operation 8 times to obtain black ginseng.

[0048] Example 3

[0049] A method for preparing black ginseng extract powder rich in rare ginsenosides, the specific steps of which are as follows:

[0050] Step 1): Put the black ginseng into a grinder and grind it. Pass it through a 0.5cm sieve and take the particles that do not pass through the sieve. Then pass it through a 1cm sieve and take the particles that pass through the sieve. Put them into 7kg of water, keep the temperature at 80℃, soak for 2 hours, filter, discard the filtrate, and obtain black ginseng particles with a particle size of 0.5-1cm.

[0051] Step 2): Add 1 kg of black ginseng granules and 12.5 kg of deionized water to the reactor. Introduce carbon dioxide into the deionized water to expel air. The carbon dioxide introduce rate is 1 L / min. After the carbon dioxide introduce reaches twice the volume of the reactor, seal the reactor and continue to introduce carbon dioxide to increase the pressure inside the reactor to 0.21 MPa. Heat the reactor to prepare deionized water at 120°C and extract at a constant temperature of 120°C for 1.65 h. Discharge the solid-liquid mixture from the reactor into a plate and frame filter press and filter while hot to obtain the extract. The filter cloth is 80 mesh and the pressure is 1 MPa.

[0052] Step 3): After the extract is naturally cooled to room temperature, it is concentrated by rotary evaporation at a vacuum of -0.08 MPa and a temperature of 65°C until it becomes a paste. The paste is then air-dried at room temperature to obtain black ginseng extract powder rich in rare ginsenosides.

[0053] Among them, the black ginseng is homemade, and the preparation method of black ginseng is as follows:

[0054] Spread the ginseng evenly on a steaming tray and place it in a continuous steaming-drying integrated equipment. Turn on the steam, control the temperature at 115℃, and steam for 2.5 hours. Release the steam and automatically move the steaming tray to the drying area. Dry at 90℃ for 4 hours. Take it out and repeat the above operation 8 times to obtain black ginseng.

[0055] Example 4

[0056] A method for preparing black ginseng extract powder rich in rare ginsenosides, the specific steps of which are as follows:

[0057] Step 1): Put the black ginseng into a grinder and grind it. Pass it through a 0.5cm sieve and take the particles that do not pass through the sieve. Then pass it through a 1cm sieve and take the particles that pass through the sieve. Put them into 8kg of water, keep the temperature at 82℃, soak for 2.2h, filter, discard the filtrate, and you will get black ginseng particles with a particle size of 0.5-1cm.

[0058] Step 2): Add 1 kg of black ginseng granules and 15 kg of deionized water to the reactor. Introduce carbon dioxide into the deionized water to expel air. The carbon dioxide introduce rate is 1 L / min. After the carbon dioxide introduce reaches twice the volume of the reactor, seal the reactor and continue to introduce carbon dioxide to increase the pressure inside the reactor to 0.22 MPa. Heat the reactor to prepare deionized water at 122℃ and extract at a constant temperature of 122℃ for 1.8 h. Discharge the solid-liquid mixture from the reactor into a plate and frame filter press and filter while hot to obtain the extract. The filter cloth specification is 100 mesh and the pressure is 1 MPa.

[0059] Step 3): After the extract is naturally cooled to room temperature, it is concentrated by rotary evaporation at a vacuum of -0.09 MPa and a temperature of 62°C until it becomes a paste. The paste is then air-dried at room temperature to obtain black ginseng extract powder rich in rare ginsenosides.

[0060] Among them, the black ginseng is homemade, and the preparation method of black ginseng is as follows:

[0061] Spread the ginseng evenly on a steaming tray and place it in a continuous steaming-drying integrated equipment. Turn on the steam, control the temperature at 115℃, and steam for 2.5 hours. Release the steam and automatically move the steaming tray to the drying area. Dry at 90℃ for 4 hours. Take it out and repeat the above operation 8 times to obtain black ginseng.

[0062] Example 5

[0063] A method for preparing black ginseng extract powder rich in rare ginsenosides, the specific steps of which are as follows:

[0064] Step 1): Put the black ginseng into a grinder and grind it. Pass it through a 0.5cm sieve and take the particles that do not pass through the sieve. Then pass it through a 1cm sieve and take the particles that pass through the sieve. Put them into 10kg of water and soak them at a constant temperature of 85℃ for 2.5h. Filter and discard the filtrate to obtain black ginseng particles with a particle size of 0.5-1cm.

[0065] Step 2): Add 1 kg of black ginseng granules and 20 kg of deionized water to the reactor. Introduce carbon dioxide into the deionized water to expel air. The carbon dioxide introduce rate is 1 L / min. After the carbon dioxide introduce reaches twice the volume of the reactor, seal the reactor and continue to introduce carbon dioxide to increase the pressure inside the reactor to 0.25 MPa. Heat the reactor to prepare deionized water at 125°C and extract at a constant temperature of 125°C for 2 hours. Discharge the solid-liquid mixture from the reactor into a plate and frame filter press and filter while hot to obtain the extract. The filter cloth is 100 mesh and the pressure is 1 MPa.

[0066] Step 3): After the extract is naturally cooled to room temperature, it is concentrated by rotary evaporation at a vacuum of -0.09 MPa and a temperature of 60°C until it becomes a paste. The paste is then air-dried at room temperature to obtain black ginseng extract powder rich in rare ginsenosides.

[0067] Among them, the black ginseng is homemade, and the preparation method of black ginseng is as follows:

[0068] Spread the ginseng evenly on a steaming tray and place it in a continuous steaming-drying integrated equipment. Turn on the steam, control the temperature at 115℃, and steam for 2.5 hours. Release the steam and automatically move the steaming tray to the drying area. Dry at 90℃ for 4 hours. Take it out and repeat the above operation 8 times to obtain black ginseng.

[0069] Example 6

[0070] A method for preparing black ginseng extract powder rich in rare ginsenosides, the specific steps of which are as follows:

[0071] Step 1): Put the black ginseng into a grinder and grind it. Pass it through a 0.5cm sieve and take the particles that do not pass through the sieve. Then pass it through a 1cm sieve and take the particles that pass through the sieve. Put them into 7kg of water, keep the temperature at 80℃, soak for 2 hours, filter, discard the filtrate, and obtain black ginseng particles with a particle size of 0.5-1cm.

[0072] Step 2): Add 1 kg of black ginseng granules and 12.5 kg of deionized water to the reactor. Introduce carbon dioxide into the deionized water to expel air. The carbon dioxide introduce rate is 1 L / min. After the carbon dioxide introduce reaches twice the volume of the reactor, seal the reactor and continue to introduce carbon dioxide to increase the pressure inside the reactor to 0.21 MPa. Heat the reactor to prepare deionized water at 120°C and extract at a constant temperature of 120°C for 1.65 h. Discharge the solid-liquid mixture from the reactor into a plate and frame filter press and filter while hot to obtain the extract. The filter cloth is 80 mesh and the pressure is 1 MPa.

[0073] Step 3): The extract is cooled to 3°C at a rate of 10°C / min and kept at 3°C ​​for 4 hours. Then, it is concentrated by rotary evaporation at a vacuum of -0.08 MPa and a temperature of 65°C until it becomes a paste. The paste is then air-dried at room temperature to obtain black ginseng extract powder rich in rare ginsenosides.

[0074] Among them, the black ginseng is homemade, and the preparation method of black ginseng is as follows:

[0075] Spread the ginseng evenly on a steaming tray and place it in a continuous steaming-drying integrated equipment. Turn on the steam, control the temperature at 115℃, and steam for 2.5 hours. Release the steam and automatically move the steaming tray to the drying area. Dry at 90℃ for 4 hours. Take it out and repeat the above operation 8 times to obtain black ginseng.

[0076] Example 7

[0077] A method for preparing black ginseng extract powder rich in rare ginsenosides, the specific steps of which are as follows:

[0078] Step 1): Put the black ginseng into a grinder and grind it. Pass it through a 0.5cm sieve and take the particles that do not pass through the sieve. Then pass it through a 1cm sieve and take the particles that pass through the sieve. Put them into 7kg of water, keep the temperature at 80℃, soak for 2 hours, filter, discard the filtrate, and obtain black ginseng particles with a particle size of 0.5-1cm.

[0079] Step 2): Add 1 kg of black ginseng granules and 12.5 kg of deionized water to the reactor. Introduce carbon dioxide into the deionized water to expel air. The carbon dioxide introduce rate is 1 L / min. After the carbon dioxide introduce reaches twice the volume of the reactor, seal the reactor and continue to introduce carbon dioxide to increase the pressure inside the reactor to 0.21 MPa. Heat the reactor to prepare deionized water at 120°C and extract at a constant temperature of 120°C for 1.65 h. Discharge the solid-liquid mixture from the reactor into a plate and frame filter press and filter while hot to obtain the extract. The filter cloth is 80 mesh and the pressure is 1 MPa.

[0080] Step 3) The extract was cooled to 4℃ at 10.5℃ / min and kept at 4℃ for 6 hours. Then, it was concentrated by rotary evaporation with a vacuum degree of -0.08MPa and a temperature of 65℃. The mixture was concentrated into a paste and then air-dried at room temperature to obtain black ginseng extract powder rich in rare ginsenosides.

[0081] Among them, the black ginseng is homemade, and the preparation method of black ginseng is as follows:

[0082] Spread the ginseng evenly on a steaming tray and place it in a continuous steaming-drying integrated equipment. Turn on the steam, control the temperature at 115℃, and steam for 2.5 hours. Release the steam and automatically move the steaming tray to the drying area. Dry at 90℃ for 4 hours. Take it out and repeat the above operation 8 times to obtain black ginseng.

[0083] Example 8

[0084] A method for preparing black ginseng extract powder rich in rare ginsenosides, the specific steps of which are as follows:

[0085] Step 1): Put the black ginseng into a grinder and grind it. Pass it through a 0.5cm sieve and take the particles that do not pass through the sieve. Then pass it through a 1cm sieve and take the particles that pass through the sieve. Put them into 7kg of water, keep the temperature at 80℃, soak for 2 hours, filter, discard the filtrate, and obtain black ginseng particles with a particle size of 0.5-1cm.

[0086] Step 2): Add 1 kg of black ginseng granules and 12.5 kg of deionized water to the reactor. Introduce carbon dioxide into the deionized water to expel air. The carbon dioxide introduce rate is 1 L / min. After the carbon dioxide introduce reaches twice the volume of the reactor, seal the reactor and continue to introduce carbon dioxide to increase the pressure inside the reactor to 0.21 MPa. Heat the reactor to prepare deionized water at 120°C and extract at a constant temperature of 120°C for 1.65 h. Discharge the solid-liquid mixture from the reactor into a plate and frame filter press and filter while hot to obtain the extract. The filter cloth is 80 mesh and the pressure is 1 MPa.

[0087] Step 3) The extract was cooled to 5℃ at 11℃ / min and kept at 5℃ for 10h. Then, it was concentrated by rotary evaporation with a vacuum degree of -0.08MPa and a temperature of 65℃. The mixture was concentrated into a paste and then air-dried at room temperature to obtain black ginseng extract powder rich in rare ginsenosides.

[0088] Among them, the black ginseng is homemade, and the preparation method of black ginseng is as follows:

[0089] Spread the ginseng evenly on a steaming tray and place it in a continuous steaming-drying integrated equipment. Turn on the steam, control the temperature at 115℃, and steam for 2.5 hours. Release the steam and automatically move the steaming tray to the drying area. Dry at 90℃ for 4 hours. Take it out and repeat the above operation 8 times to obtain black ginseng.

[0090] Comparative Example 1

[0091] A method for preparing black ginseng extract powder rich in rare ginsenosides, which differs from Example 3 only in that:

[0092] Step 2): Add 1 kg of black ginseng granules and 12.5 kg of deionized water to the reactor. Introduce nitrogen into the deionized water to expel air. The nitrogen introduce rate is 1 L / min. After the nitrogen introduce reaches twice the volume of the reactor, seal the reactor and continue to introduce nitrogen to increase the pressure inside the reactor to 0.21 MPa. Heat the reactor to prepare deionized water at 120°C and extract at a constant temperature of 120°C for 1.65 h. Discharge the solid-liquid mixture from the reactor into a plate and frame filter press and filter while hot to obtain the extract. The filter cloth is 80 mesh and the pressure is 1 MPa.

[0093] The remaining steps are the same as in Example 3.

[0094] Comparative Example 2

[0095] A method for preparing black ginseng extract powder rich in rare ginsenosides, which differs from Example 3 only in that:

[0096] Step 2): Add 1 kg of black ginseng granules and 12.5 kg of deionized water to the reactor. Introduce helium into the deionized water to expel air. The helium introduce rate is 1 L / min. After the helium introduce reaches twice the volume of the reactor, seal the reactor and continue to introduce helium to increase the pressure inside the reactor to 0.21 MPa. Heat the reactor to prepare deionized water at 120°C and extract at a constant temperature of 120°C for 1.65 h. Discharge the solid-liquid mixture from the reactor into a plate and frame filter press and filter while hot to obtain the extract. The filter cloth is 80 mesh and the pressure is 1 MPa.

[0097] The remaining steps are the same as in Example 3.

[0098] Comparative Example 3

[0099] A method for preparing black ginseng extract powder rich in rare ginsenosides, which differs from Example 3 only in that:

[0100] Step 2): Add 1 kg of black ginseng granules and 12.5 kg of deionized water to the reactor. Introduce carbon dioxide into the deionized water to expel air. The carbon dioxide introduce rate is 1 L / min. After the carbon dioxide introduce reaches twice the volume of the reactor, seal the reactor and continue to introduce carbon dioxide to increase the pressure inside the reactor to 0.13 MPa. Heat the reactor to prepare deionized water at 120°C and extract at a constant temperature of 120°C for 1.65 h. Discharge the solid-liquid mixture from the reactor into a plate and frame filter press and filter while hot to obtain the extract. The filter cloth is 80 mesh and the pressure is 1 MPa.

[0101] The remaining steps are the same as in Example 3.

[0102] Comparative Example 4

[0103] A method for preparing black ginseng extract powder rich in rare ginsenosides, which differs from Example 3 only in that:

[0104] Step 2): Add 1 kg of black ginseng granules and 12.5 kg of deionized water to the reactor. Introduce carbon dioxide into the deionized water to expel air. The carbon dioxide introduce rate is 1 L / min. After the carbon dioxide introduce reaches twice the volume of the reactor, seal the reactor and continue to introduce carbon dioxide to increase the pressure inside the reactor to 0.27 MPa. Heat the reactor to prepare deionized water at 120°C and extract at a constant temperature of 120°C for 1.65 h. Discharge the solid-liquid mixture from the reactor into a plate and frame filter press and filter while hot to obtain the extract. The filter cloth specification is 80 mesh and the pressure is 1 MPa.

[0105] The remaining steps are the same as in Example 3.

[0106] Comparative Example 5

[0107] A method for preparing black ginseng extract powder rich in rare ginsenosides, which differs from Example 3 only in that:

[0108] Step 2): Add 1 kg of black ginseng granules and 12.5 kg of deionized water to the reactor. Introduce carbon dioxide into the deionized water to expel air. The carbon dioxide introduce rate is 1 L / min. After the carbon dioxide introduce reaches twice the volume of the reactor, seal the reactor and continue to introduce carbon dioxide to increase the pressure inside the reactor to 0.15 MPa. Heat the reactor to prepare deionized water at 102℃ and extract at a constant temperature of 102℃ for 1.65 h. Discharge the solid-liquid mixture from the reactor into a plate and frame filter press and filter while hot to obtain the extract. The filter cloth specification is 80 mesh and the pressure is 1 MPa.

[0109] The remaining steps are the same as in Example 3.

[0110] Comparative Example 6

[0111] A method for preparing black ginseng extract powder rich in rare ginsenosides, which differs from Example 3 only in that:

[0112] Step 2): Add 1 kg of black ginseng granules and 12.5 kg of deionized water to the reactor. Introduce carbon dioxide into the deionized water to expel air. The carbon dioxide introduce rate is 1 L / min. After the carbon dioxide introduce reaches twice the volume of the reactor, seal the reactor and continue to introduce carbon dioxide to increase the pressure inside the reactor to 0.15 MPa. Heat the reactor to prepare deionized water at 128°C and extract at a constant temperature of 128°C for 1.65 h. Discharge the solid-liquid mixture from the reactor into a plate and frame filter press and filter while hot to obtain the extract. The filter cloth is 80 mesh and the pressure is 1 MPa.

[0113] The remaining steps are the same as in Example 3.

[0114] Comparative Example 7

[0115] A method for preparing black ginseng extract powder rich in rare ginsenosides, which differs from Example 3 only in that:

[0116] Step 2): Add 1 kg of black ginseng granules and 12.5 kg of deionized water to the reactor. Introduce carbon dioxide into the deionized water to expel air. The carbon dioxide introduce rate is 1 L / min. After the carbon dioxide introduce reaches twice the volume of the reactor, seal the reactor and continue to introduce carbon dioxide to increase the pressure inside the reactor to 0.15 MPa. Heat the reactor to prepare deionized water at 120°C and extract at a constant temperature of 120°C for 2.5 h. Discharge the solid-liquid mixture from the reactor into a plate and frame filter press and filter while hot to obtain the extract. The filter cloth specification is 80 mesh and the pressure is 1 MPa.

[0117] The remaining steps are the same as in Example 3.

[0118] Comparative Example 8

[0119] A method for preparing black ginseng extract powder rich in rare ginsenosides, which differs from Example 3 only in that:

[0120] Step 2): Add 1 kg of black ginseng granules and 12.5 kg of deionized water to the reactor. Introduce carbon dioxide into the deionized water to expel air. The carbon dioxide introduce rate is 1 L / min. After the carbon dioxide introduce reaches twice the volume of the reactor, seal the reactor and continue to introduce carbon dioxide to increase the pressure inside the reactor to 0.15 MPa. Heat the reactor to prepare deionized water at 120°C and extract at a constant temperature of 120°C for 3 hours. Discharge the solid-liquid mixture from the reactor into a plate and frame filter press and filter while hot to obtain the extract. The filter cloth specification is 80 mesh and the pressure is 1 MPa.

[0121] The remaining steps are the same as in Example 3.

[0122] Experiment 1

[0123] The content of rare ginsenosides in the black ginseng extract powder rich in rare ginsenosides prepared in each example and comparative example was determined according to T / CNHFA 001-2021 "Determination of Rare Ginsenoside Content".

[0124] Experiment 2

[0125] Water solubility stability test of black ginseng extract powder rich in rare ginsenosides: The test steps are as follows:

[0126] Weigh 1g of ginsenoside black ginseng extract powder and add it to 99g of deionized water. Stir at 120r / min for 5min to obtain the test solution. Let it stand and observe every 0.5h. Record the time when precipitation appears in the test solution. If it is longer than 8h, record it as >8h, which proves that the water solubility stability is good. The shorter the precipitation time, the worse the water solubility stability.

[0127] For detailed test results of Experiments 1 and 2, please refer to Figures 1-32 .

[0128] The specific test data for Experiments 1 and 2 are detailed in Table 1.

[0129] Table 1

[0130]

[0131]

[0132] According to the data comparison between the embodiments and comparative examples in Table 1, the content of rare ginsenosides in each embodiment is significantly higher than that in each comparative example. It can be seen that by using dilute carbonic acid solution as a solvent and under the combination of special temperature, pressure and extraction time during the extraction process, rare ginsenosides can be extracted to the maximum extent, and the purity of rare ginsenosides in the black ginseng extract powder rich in rare ginsenosides is relatively high.

[0133] The water solubility stability of the black ginseng extract powder rich in rare ginsenosides in Examples 1-5 is lower than that in Examples 6-8. It can be seen that after heating and extraction, adding a rapid cooling process can improve the water solubility stability of rare ginsenosides, making the black ginseng extract powder rich in rare ginsenosides more suitable for the food industry.

[0134] This specific embodiment is merely an explanation of this application and is not intended to limit it. After reading this specification, those skilled in the art can make modifications to this embodiment without contributing any inventive step, but such modifications are protected by patent law as long as they fall within the scope of the claims of this application.

Claims

1. A method for preparing black ginseng extract powder rich in rare ginsenosides, characterized in that: Includes the following steps: Step 1) Crush the black ginseng, put it into water, keep it at a constant temperature of 75-85℃, soak for 1.5-2.5 hours, filter, discard the filtrate, and obtain black ginseng granules; Step 2): Put the black ginseng granules and water into a container, introduce carbon dioxide to increase the pressure to 0.15-0.25 MPa, extract at a constant temperature of 105-125℃ for 0.5-2 hours, and filter while hot to obtain the extract. Step 3) Concentrate and dry the extract to obtain black ginseng extract powder rich in rare ginsenosides; In step 3), the extract is first cooled and then concentrated and dried. During cooling, the temperature is reduced to 3-5℃ at a rate of 10-11℃ / min, and then concentrated and dried. After cooling to 3-5℃, maintain a constant temperature of 3-5℃ for 4-10 hours.

2. The method for preparing black ginseng extract powder rich in rare ginsenosides according to claim 1, characterized in that: In step 2), carbon dioxide is introduced to increase the pressure to 0.2-0.22 MPa, and the extraction is carried out at a constant temperature of 115-122℃ for 1.5-1.8 hours.

3. The method for preparing black ginseng extract powder rich in rare ginsenosides according to claim 2, characterized in that: In step 2), when carbon dioxide is introduced, it is introduced into the water, and the air in the container is expelled at the same time. Then the container is sealed and the pressure is increased.

4. The method for preparing black ginseng extract powder rich in rare ginsenosides according to claim 1, characterized in that: In step 2), the ratio of the mass of black ginseng granules to the mass of water is 1:5-20.

5. The method for preparing black ginseng extract powder rich in rare ginsenosides according to claim 1, characterized in that: In step 1), the particle size of the black ginseng particles is 0.5-1cm.

6. The method for preparing black ginseng extract powder rich in rare ginsenosides according to claim 1, characterized in that: In step 2), 80-100 mesh filter cloth is used for pressure filtration.

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