Preparation method of areca flower oral liquid

Abstract

The invention relates to the technical field of oral liquid preparation, and discloses a preparation method of betelnutpalm male flower oral liquid, which comprises the following steps: selecting betelnutpalm male flower medicinal materials in an initial flowering period, and removing non-medicinal parts, foreign matters, mildewed medicinal materials and worm-damaged medicinal materials to obtain the selected betelnutpalm male flower medicinal materials; cutting the cleaned and selected areca flower medicinal material to obtain a cut medicinal material; carrying out coarse crushing on the cut medicinal materials; carrying out freezing treatment on the coarsely crushed medicinal material, and carrying out superfine grinding until the particle size is 1-10 [mu] m, so as to obtain a pre-treated medicinal material of the flos arecae; carrying out low-temperature dipping extraction on the pre-treated medicinal material of the areca flowers to obtain an areca flower extracting solution; pumping the areca flower extracting solution into a single-effect concentrator for concentration; adding activated carbon for decoloring to obtain clear and transparent decolored filtrate; concentrating the decolorized filtrate into a fluid extract, adding sodium benzoate, refrigerating and filtering; and adding the fluid extract refrigerated filtrate and the refined honey into a preparation tank, adding water, stirring, filtering, sub-packaging and sterilizing to obtain the areca flower oral liquid.

Description

Technical Field

[0001] The present invention relates to the technical field of oral liquid preparation, and particularly relates to a preparation method of areca flower oral liquid. Background Art

[0002] Areca flower is the dried inflorescence of the palm plant Areca catechu L. Areca flower oral liquid is an oral liquid prepared from areca flower, and has the effects of strengthening the spleen and regulating qi, resolving phlegm and relieving cough.

[0003] CN1124586A discloses areca flower oral liquid, and CN102224932A discloses areca flower extract and oral liquid, but both lack how to improve the content of active ingredients in areca flower oral liquid; CN115006479A discloses an areca flower oral liquid and its preparation method, which extracts areca flower medicinal materials by ethanol impregnation, and adopts two-stage microwave composite enzymatic hydrolysis and dilution enzymatic hydrolysis, which cooperate with each other to avoid reducing the content of active ingredients in the oral liquid and improve the clarity and stability of the oral liquid. However, enzymes have specific requirements for environmental conditions such as temperature, pH, and moisture, which limit the application of enzymatic hydrolysis extraction under certain process conditions. Moreover, adopting two-stage composite enzymatic hydrolysis and dilution enzymatic hydrolysis may produce more enzymatic hydrolysis products, increasing the complexity and cost of post-treatment. Summary of the Invention

[0004] In view of the above problems existing in the prior art, the present application provides a preparation method of areca flower oral liquid.

[0005] To solve the above problems, the present invention provides the following technical solutions:

[0006] The present application provides a preparation method of areca flower oral liquid, comprising the following steps:

[0007] S1. Select areca flower medicinal materials at the early flowering stage, remove non-medicinal parts, foreign matters, mildewed and insect-infested medicinal materials, and obtain the selected areca flower medicinal materials;

[0008] S2. Cut the selected areca flower medicinal materials to obtain cut medicinal materials;

[0009] S3. Coarsely crush the cut medicinal materials to obtain coarsely crushed medicinal materials with a coarsely crushed particle size of less than 5 mm;

[0010] S4. Freeze-treat the coarsely crushed medicinal materials and ultrafinely crush them to a particle size of 1-10 μm to obtain pre-treated areca flower medicinal materials;

[0011] S5. Perform low-temperature maceration extraction on the pre-treated betel nut flower medicinal materials to obtain a betel nut flower extract; the solution used for maceration extraction is a composite extract, and the composite extract is a mixture of ethanol, ether, and chloroform. The ethanol is an ethanol solution with a volume concentration of 60-70%, and the ethanol solution contains a phosphate buffer solution.

[0012] S6. Pump the betel nut flower extract into a single-effect concentrator for concentration.

[0013] S7. Add activated carbon for decolorization according to a dosage ratio of 200L:1kg to obtain a clear and transparent decolorized filtrate.

[0014] S8. Concentrate the decolorized filtrate into a fluid extract, add sodium benzoate, refrigerate, and filter.

[0015] S9. Put the refrigerated filtrate of the fluid extract and refined honey into a preparation tank, add water, stir, filter, subpackage, and sterilize to obtain betel nut flower oral liquid.

[0016] In one embodiment of the present application, the moisture content of the cleaned betel nut flower medicinal materials does not exceed 3 wt.%.

[0017] In one embodiment of the present application, no less than 90% of the cut medicinal materials have a length less than 8 cm.

[0018] In one embodiment of the present application, the temperature of the freezing treatment is -20 to -40 °C, and the time of the freezing treatment is 10 to 30 min.

[0019] In one embodiment of the present application, the volume ratio of ethanol, ether, and chloroform in the composite extract is 1:0.2-0.3:0.2-0.3.

[0020] In one embodiment of the present application, the temperature of the low-temperature maceration extraction is 4 to 10 °C.

[0021] In one embodiment of the present application, the maceration extraction includes two extractions. The first maceration extraction is: add the composite extract according to a material-liquid mass ratio of 1:6-8, macerate and extract for 45-50 h, filter, and pump the maceration liquid into a storage tank; the second maceration extraction is: add the composite extract according to a material-liquid mass ratio of 1:5-7, macerate and extract for 20-30 h, filter, and pump the maceration liquid into a storage tank to obtain the betel nut flower extract.

[0022] In one embodiment of the present application, each 1 mL of the fluid extract contains 0.24-0.36 mg of ether-soluble alkaloids calculated as arecoline.

[0023] In one embodiment of the present application, each 1 mL of the betel nut flower oral liquid contains 0.1-0.2 mg of ether-soluble alkaloids calculated as arecoline.

[0024] In one embodiment of the present application, the concentration temperature in the evaporation chamber of the single-effect concentrator is 40 - 90 °C, the vacuum temperature is 0.02 - 0.095 Mpa, and the steam pressure < 0.1 Mpa.

[0025] In one embodiment of the present application, the concentration time of the areca flower extract is 20 - 40 min.

[0026] In one embodiment of the present application, the refrigeration temperature is 4 - 10 °C.

[0027] In one embodiment of the present application, the prepared areca flower oral liquid contains 233 g of areca flower, 3.5 g of activated carbon, 3 g of sodium benzoate, and 100 g of honey per 1000 mL.

[0028] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0029] (1) For the preparation method of the areca flower oral liquid provided in the present application, the tissue structure of the frozen areca flower becomes fragile and is easier to be crushed, which helps to improve the release of the active ingredients in the areca flower, thereby improving the extraction efficiency. At the same time, since the powder particle size after cryogenic ultrafine grinding is uniform and fine, it can be better dispersed in the impregnation extract, reducing the precipitation of large particle substances, and thus improving the clarity of the solution.

[0030] (2) For the preparation method of the areca flower oral liquid provided in the present application, by adopting a composite extract and using a phosphate buffer solution with less influence by temperature, combined with low-temperature impregnation extraction to protect the stability of bioactive ingredients, some reactions during the extraction process are reduced, enhancing the extraction efficiency and clarity. Specific Embodiments

[0031] Next, the technical solutions in the embodiments of the present application will be clearly and completely described in conjunction with the embodiments of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all of the embodiments.

[0032] The "range" disclosed in the present application is defined in the form of a lower limit and an upper limit. A given range is defined by selecting a lower limit and an upper limit, and the selected lower limit and upper limit define the boundary of a specific range. The range defined in this way can include the end values or not include the end values, and can be combined arbitrarily, that is, any lower limit can be combined with any upper limit to form a range.

[0033] Unless otherwise specified, when the present invention relates to the percentage between liquids, the percentage is volume / volume percentage; when the present invention relates to the percentage between a liquid and a solid, the percentage is volume / weight percentage; when the present invention relates to the percentage between a solid and a liquid, the percentage is weight / volume percentage; the rest are weight / weight percentages.

[0034] The materials, reagents, etc. used in the following examples can be obtained from commercial sources without special instructions.

[0035] Example 1

[0036] This application provides a preparation method of areca flower oral liquid, which includes the following steps:

[0037] S1. Select areca flower medicinal materials at the early flowering stage, remove non-medicinal parts, foreign matters, mildewed and insect-infested medicinal materials, and obtain the selected areca flower medicinal materials with a moisture content not exceeding 3 wt.%.

[0038] S2. Cut the selected areca flower medicinal materials to obtain cut medicinal materials; no less than 90% of the cut medicinal materials have a length less than 8 cm.

[0039] S3. Check whether the pulverizer is normal, install the sieve mesh, run it without load for 1 - 2 min to ensure no abnormal situation, and coarsely crush the cut medicinal materials to obtain coarsely crushed medicinal materials with a coarsely crushed particle size less than 5 mm.

[0040] S4. Freeze the coarsely crushed medicinal materials at -30°C for 20 min and ultrafinely crush them to a particle size of 1 - 10 μm to obtain pre-treated areca flower medicinal materials.

[0041] S5. Before the feeding operation, confirm that the bottom valve of the percolation tank is closed well, lay a 100-mesh filter cloth at the bottom, and then slowly put 233 g of pre-treated areca flower medicinal materials into the percolation extraction tank for low-temperature impregnation extraction at 4°C. The impregnation extraction includes two extractions. The first impregnation extraction is: add a compound extraction solution according to a material-liquid mass ratio of 1:7, impregnate for 48 h, filter through a 100-mesh sieve, and pump the impregnation liquid into the storage tank; the second impregnation extraction is: add a compound extraction solution according to a material-liquid mass ratio of 1:6, impregnate for 24 h, filter through a 100-mesh sieve, and pump the impregnation liquid into the storage tank. Combine the two impregnation liquids to obtain areca flower extraction liquid. The compound extraction solution is a mixed solution of ethanol, ether, and chloroform with a volume ratio of 1:0.25:0.25; the ethanol is an ethanol solution with a volume concentration of 65%, and the ethanol solution contains a phosphate buffer solution.

[0042] S6. Pump the areca flower extraction liquid into a single-effect concentrator for concentration until it is concentrated to about 700 mL; the evaporation chamber concentration temperature of the single-effect concentrator is 40 - 90°C, the vacuum temperature is 0.02 - 0.095 Mpa, the steam pressure < 0.1 Mpa, and the concentration time of the areca flower extraction liquid is 30 min.

[0043] S7. Pump the concentrated liquid into the feed liquid temporary storage tank, add 3.5 g of activated carbon for decolorization to obtain a clear and transparent decolorized and filtered liquid;

[0044] S8. Concentrate the decolorized and filtered liquid into a fluid extract, add 3 g of sodium benzoate, refrigerate at 4 - 10°C for 24 h, and filter with a 300 - mesh filter cloth;

[0045] S9. Separately, take 100 g of honey, dissolve it in 400 mL of water, boil it, filter it to obtain refined honey. Add the refrigerated and filtered fluid extract and the refined honey into a preparation tank, add water to 1000 mL, stir, filter, dispense into vials at 10 mL / vial, then set the sterilization parameters: sterilization temperature 115°C, sterilization time 30 min, and perform sterilization to obtain the areca flower oral liquid.

[0046] Comparative Example 1

[0047] This application provides a preparation method of areca flower oral liquid, which includes the following steps:

[0048] S1. Select areca flower medicinal materials in the full - bloom period, remove non - medicinal parts, foreign matters, mildewed and insect - eaten medicinal materials to obtain the selected areca flower medicinal materials with a moisture content not exceeding 3 wt.%.

[0049] S2. Cut the selected areca flower medicinal materials to obtain the cut medicinal materials; not less than 90% of the cut medicinal materials have a length less than 8 cm.

[0050] S3. Check whether the pulverizer is normal, install the sieve mesh, run it without load for 1 - 2 min to ensure no abnormal situation, and coarsely crush the cut medicinal materials to obtain coarsely crushed medicinal materials with a particle size less than 5 mm.

[0051] S4. Freeze - treat the coarsely crushed medicinal materials at - 30°C for 20 min and ultrafinely pulverize them to a particle size of 1 - 10 μm to obtain the pretreated areca flower medicinal materials.

[0052] S5. Before the feeding operation, confirm that the bottom valve of the percolation tank is closed well, lay a 100 - mesh filter cloth at the bottom, and then slowly put 233 g of the pretreated areca flower medicinal materials into the percolation extraction tank for low - temperature impregnation extraction at 4°C. The impregnation extraction includes two extractions. The first impregnation extraction: add a compound extraction solution according to the mass ratio of material to liquid of 1:7, impregnate for 48 h, filter through a 100 - mesh filter, and pump the impregnation liquid into the storage tank; the second impregnation extraction: add a compound extraction solution according to the mass ratio of material to liquid of 1:6, impregnate for 24 h, filter through a 100 - mesh filter, and pump the impregnation liquid into the storage tank. Combine the two impregnation liquids to obtain the areca flower extraction solution. The compound extraction solution is a mixed solution of ethanol, ether and chloroform, and their volume ratio is 1:0.25:0.25; the ethanol is an ethanol solution with a volume concentration of 65%, and the ethanol solution contains a phosphate buffer solution.

[0053] S6. Pump the areca flower extract into a single-effect concentrator for concentration until it reaches about 700 mL. The concentration temperature in the evaporation chamber of the single-effect concentrator is 40 - 90 °C, the vacuum temperature is 0.02 - 0.095 Mpa, the steam pressure < 0.1 Mpa, and the concentration time of the areca flower extract is 30 min.

[0054] S7. Pump the concentrated liquid into a feed liquid temporary storage tank, add 3.5 g of activated carbon for decolorization to obtain a clear and transparent decolorized and filtered liquid.

[0055] S8. Concentrate the decolorized and filtered liquid into a fluid extract, add 3 g of sodium benzoate, refrigerate at 4 - 10 °C for 24 h, and filter with a 300-mesh filter cloth.

[0056] S9. Take another 100 g of honey, dissolve it in 400 mL of water, boil it, filter it to obtain refined honey. Add the refrigerated and filtered fluid extract and the refined honey into a preparation tank, add water to 1000 mL, stir, filter, divide it into portions of 10 mL per vial, then set the sterilization parameters, with a sterilization temperature of 115 °C and a sterilization time of 30 min for sterilization to obtain areca flower oral liquid.

[0057] Comparative Example 2

[0058] This application provides a preparation method of areca flower oral liquid, including the following steps:

[0059] S1. Select areca flower medicinal materials at the late flowering stage, remove non-medicinal parts, foreign matters, mildewed and insect-infested medicinal materials to obtain the selected areca flower medicinal materials with a moisture content not exceeding 3 wt.%.

[0060] S2. Cut the selected areca flower medicinal materials to obtain cut medicinal materials. No less than 90% of the cut medicinal materials have a length less than 8 cm.

[0061] S3. Check whether the crusher is normal, install the sieve mesh, run it without load for 1 - 2 min to ensure no abnormal situation, and coarsely crush the cut medicinal materials to obtain coarsely crushed medicinal materials with a coarsely crushed particle size less than 5 mm.

[0062] S4. Freeze the coarsely crushed medicinal materials at -30 °C for 20 min and ultrafinely crush them to a particle size of 1 - 10 μm to obtain pre-treated areca flower medicinal materials.

[0063] S5. Before the feeding operation, confirm that the bottom valve of the percolation tank is closed properly, lay a 100-mesh filter cloth at the bottom, and then slowly put 233 g of the pretreated Areca flower medicinal materials into the percolation extraction tank for low-temperature impregnation extraction at 4 °C. The impregnation extraction includes two extractions. The first impregnation extraction is: add a compound extraction solution according to the mass ratio of material to liquid of 1:7, impregnate and extract for 48 h, filter through a 100-mesh filter, and pump the impregnation solution into the storage tank; the second impregnation extraction is: add a compound extraction solution according to the mass ratio of material to liquid of 1:6, impregnate and extract for 24 h, filter through a 100-mesh filter, and pump the impregnation solution into the storage tank. Combine the two impregnation solutions to obtain the Areca flower extraction solution. The compound extraction solution is a mixed solution of ethanol, ether and chloroform, and its volume ratio is 1:0.25:0.25; the ethanol is an ethanol solution with a volume concentration of 65%, and the ethanol solution contains a phosphate buffer solution.

[0064] S6. Pump the Areca flower extraction solution into a single-effect concentrator for concentration until it is concentrated to about 700 mL; the concentration temperature in the evaporation chamber of the single-effect concentrator is 40 - 90 °C, the vacuum temperature is 0.02 - 0.095 Mpa, the steam pressure < 0.1 Mpa, and the concentration time of the Areca flower extraction solution is 30 min.

[0065] S7. Pump the concentrated solution into the feed liquid storage tank, add 3.5 g of activated carbon for decolorization to obtain a clear and transparent decolorized filtrate;

[0066] S8. Concentrate the decolorized filtrate into a fluid extract, add 3 g of sodium benzoate, refrigerate at 4 - 10 °C for 24 h, and filter with a 300-mesh filter cloth;

[0067] S9. Take another 100 g of honey, dissolve it in 400 mL of water, boil it, filter it to obtain refined honey. Put the refrigerated filtrate of the fluid extract and the refined honey into a preparation tank, add water to 1000 mL, stir, filter, sub-pack into 10 mL per vial, then set the sterilization parameters, the sterilization temperature is 115 °C, the sterilization time is 30 min, and perform sterilization to obtain the Areca flower oral liquid.

[0068] Comparative Example 3

[0069] The present application provides a preparation method of an Areca flower oral liquid, which includes the following steps:

[0070] S1. Select Areca flower medicinal materials at the early flowering stage, remove non-medicinal parts, foreign matters, mildewed and insect-infested medicinal materials to obtain the selected Areca flower medicinal materials, with the moisture content not exceeding 3 wt.%.

[0071] S2. Cut the selected Areca flower medicinal materials to obtain the cut medicinal materials; no less than 90% of the length of the cut medicinal materials is less than 8 cm.

[0072] S3. Check whether the crusher is normal, install the sieve mesh, and run it without load for 1 - 2 minutes to ensure no abnormal situation. Coarsely crush the cut medicinal materials to obtain coarsely crushed medicinal materials with a coarsely crushed particle size of less than 5 mm.

[0073] S4. Before the feeding operation, confirm that the bottom valve of the percolation tank is closed properly, lay a 100 - mesh filter cloth at the bottom, and then slowly put 233 g of the pre - treated medicinal materials of betel nut flower into the percolation extraction tank for low - temperature impregnation extraction at 4°C. The impregnation extraction includes two extractions. The first impregnation extraction is: add a compound extraction solution according to the mass ratio of material to liquid of 1:7, impregnate for 48 h, filter through a 100 - mesh filter, and pump the impregnation liquid into the storage tank; the second impregnation extraction is: add a compound extraction solution according to the mass ratio of material to liquid of 1:6, impregnate for 24 h, filter through a 100 - mesh filter, and pump the impregnation liquid into the storage tank. Combine the two impregnation liquids to obtain the betel nut flower extraction solution. The compound extraction solution is a mixed solution of ethanol, ether and chloroform, and its volume ratio is 1:0.25:0.25; the ethanol is an ethanol solution with a volume concentration of 65%, and the ethanol solution contains a phosphate buffer solution.

[0074] S5. Pump the betel nut flower extraction solution into a single - effect concentrator for concentration until it is concentrated to about 700 mL; the evaporation chamber concentration temperature of the single - effect concentrator is 40 - 90°C, the vacuum temperature is 0.02 - 0.095 Mpa, the steam pressure < 0.1 Mpa, and the concentration time of the betel nut flower extraction solution is 30 min.

[0075] S6. Pump the concentrated liquid into the liquid storage tank, add 3.5 g of activated carbon for decolorization to obtain a clear and transparent decolorized and filtered liquid;

[0076] S7. Concentrate the decolorized and filtered liquid into a fluid extract, add 3 g of sodium benzoate, refrigerate at 4 - 10°C for 24 h, and filter with a 300 - mesh filter cloth;

[0077] S8. Take another 100 g of honey, dissolve it in 400 mL of water, boil it, filter it to obtain refined honey. Put the refrigerated and filtered fluid extract and refined honey into a preparation tank, add water to 1000 mL, stir, filter, dispense into 10 - mL vials, then set the sterilization parameters, the sterilization temperature is 115°C, the sterilization time is 30 min, and perform sterilization to obtain betel nut flower oral liquid.

[0078] Comparative Example 4

[0079] This application provides a preparation method of betel nut flower oral liquid, including the following steps:

[0080] S1. Select betel nut flower medicinal materials at the early flowering stage, remove non - medicinal parts, foreign matters, mildewed and insect - eaten medicinal materials to obtain the selected betel nut flower medicinal materials with a moisture content not exceeding 3 wt.%.

[0081] S2. Cut the selected betel nut flower medicinal materials to obtain cut medicinal materials; no less than 90% of the cut medicinal materials have a length less than 8 cm.

[0082] S3. Check whether the crusher is normal, install the sieve mesh, and run it without load for 1 - 2 min to ensure no abnormal situation. Coarsely crush the cut medicinal materials to obtain coarsely crushed medicinal materials with a coarsely crushed particle size less than 5 mm.

[0083] S4. Freeze the coarsely crushed medicinal materials at -30°C for 20 min and then ultrafinely crush them to a particle size of 1 - 10 μm to obtain pre-treated betel nut flower medicinal materials.

[0084] S5. Before the feeding operation, confirm that the bottom valve of the percolation tank is closed well, lay a 100-mesh filter cloth at the bottom, and then slowly put 233 g of the pre-treated betel nut flower medicinal materials into the percolation extraction tank for low-temperature impregnation extraction at 4°C. The impregnation extraction includes two extractions. The first impregnation extraction is: add an ethanol solution with a volume concentration of 65% (the ethanol solution is prepared with a phosphate buffer solution) according to a material-liquid mass ratio of 1:7, impregnate and extract for 48 h, filter through a 100-mesh sieve, and pump the impregnation liquid into the storage tank; the second impregnation extraction is: add an ethanol solution with a volume concentration of 65% (the ethanol solution is prepared with a phosphate buffer solution) according to a material-liquid mass ratio of 1:6, impregnate and extract for 24 h, filter through a 100-mesh sieve, and pump the impregnation liquid into the storage tank. Combine the two impregnation liquids to obtain the betel nut flower extraction liquid.

[0085] S6. Pump the betel nut flower extraction liquid into a single-effect concentrator for concentration until it is about 700 mL; the concentration temperature in the evaporation chamber of the single-effect concentrator is 40 - 90°C, the vacuum temperature is 0.02 - 0.095 Mpa, the steam pressure < 0.1 Mpa, and the concentration time of the betel nut flower extraction liquid is 30 min.

[0086] S7. Pump the concentrated liquid into the feed liquid storage tank, add 3.5 g of activated carbon for decolorization to obtain a clear and transparent decolorized and filtered liquid;

[0087] S8. Concentrate the decolorized and filtered liquid into a fluid extract, add 3 g of sodium benzoate, refrigerate at 4 - 10°C for 24 h, and filter with a 300-mesh filter cloth;

[0088] S9. Take another 100 g of honey, dissolve it in 400 mL of water, boil it, filter it to obtain refined honey. Put the refrigerated and filtered fluid extract and the refined honey into a preparation tank, add water to 1000 mL, stir, filter, dispense into 10 mL per vial, then set the sterilization parameters, with a sterilization temperature of 115°C and a sterilization time of 30 min for sterilization to obtain the betel nut flower oral liquid.

[0089] Comparative Example 5

[0090] This application provides a preparation method of betel nut flower oral liquid, including the following steps:

[0091] S1. Select betel nut flower medicinal materials at the early flowering stage, remove non-medicinal parts, foreign matters, mildewed and insect-infested medicinal materials to obtain the cleaned betel nut flower medicinal materials with moisture not exceeding 3 wt.%.

[0092] S2. Cut the cleaned betel nut flower medicinal materials to obtain the cut medicinal materials; no less than 90% of the cut medicinal materials have a length less than 8 cm.

[0093] S3. Check whether the crusher is normal, install the sieve mesh, run it without load for 1 - 2 min to ensure no abnormal situation, and coarsely crush the cut medicinal materials to obtain the coarsely crushed medicinal materials with a coarsely crushed particle size less than 5 mm.

[0094] S4. Freeze the coarsely crushed medicinal materials at -30 °C for 20 min and ultrafinely crush them to a particle size of 1 - 10 μm to obtain the pre-treated betel nut flower medicinal materials.

[0095] S5. Before the feeding operation, confirm that the bottom valve of the percolation tank is closed well, lay a 100-mesh filter cloth at the bottom, and then slowly put 233 g of the pre-treated betel nut flower medicinal materials into the percolation extraction tank for low-temperature impregnation extraction at 4 °C. The impregnation extraction includes two extractions. The first impregnation extraction is: add a compound extraction solution according to the mass ratio of material to liquid of 1:7, impregnate for 48 h, filter through a 100-mesh sieve, and pump the impregnation liquid into the storage tank; the second impregnation extraction is: add a compound extraction solution according to the mass ratio of material to liquid of 1:6, impregnate for 24 h, filter through a 100-mesh sieve, and pump the impregnation liquid into the storage tank. Combine the two impregnation liquids to obtain the betel nut flower extraction solution. The compound extraction solution is a mixed solution of ethanol, ether and chloroform, and its volume ratio is 1:0.25:0.25; the ethanol is an ethanol solution with a volume concentration of 65%, and the ethanol solution contains a sodium carbonate - sodium bicarbonate buffer solution.

[0096] S6. Pump the betel nut flower extraction solution into a single-effect concentrator for concentration to about 700 mL; the evaporation chamber concentration temperature of the single-effect concentrator is 40 - 90 °C, the vacuum temperature is 0.02 - 0.095 Mpa, the steam pressure < 0.1 Mpa, and the concentration time of the betel nut flower extraction solution is 30 min.

[0097] S7. Add 3.5 g of activated carbon to the concentrated solution for decolorization to obtain a clear and transparent decolorized filtrate;

[0098] S8. Concentrate the decolorized filtrate into a fluid extract, add 3 g of sodium benzoate, refrigerate at 4 - 10 °C for 24 h, and filter with a 300-mesh filter cloth;

[0099] S9. Take another 100 g of honey, dissolve it in 400 mL of water, boil it, filter it to obtain refined honey. Add the refrigerated filtrate of the fluidextract and the refined honey into a preparation tank, add water to make up to 1000 mL, stir, filter, fill into vials at 10 mL / vial, then set the sterilization parameters: sterilization temperature 115°C, sterilization time 30 min, and perform sterilization to obtain the areca flower oral liquid.

[0100] Comparative Example 6

[0101] This application provides a preparation method of areca flower oral liquid, including the following steps:

[0102] S1. Select areca flower medicinal materials at the early flowering stage, remove non-medicinal parts, foreign matters, mildewed and insect-infested medicinal materials to obtain the selected areca flower medicinal materials with moisture not exceeding 3 wt.%.

[0103] S2. Cut the selected areca flower medicinal materials to obtain cut medicinal materials; no less than 90% of the cut medicinal materials have a length less than 8 cm.

[0104] S3. Check whether the crusher is normal, install the sieve mesh, run it without load for 1 - 2 min to ensure no abnormal situation, and coarsely crush the cut medicinal materials to obtain coarsely crushed medicinal materials with a coarsely crushed particle size less than 5 mm.

[0105] S4. Freeze the coarsely crushed medicinal materials at -30°C for 20 min and ultrafinely crush them to a particle size of 1 - 10 μm to obtain the pre-treated areca flower medicinal materials.

[0106] S5. Before the feeding operation, confirm that the bottom valve of the percolation tank is closed well, lay a 100-mesh filter cloth at the bottom, and then slowly put 233 g of the pre-treated areca flower medicinal materials into the percolation extraction tank for impregnation extraction at room temperature. The impregnation extraction includes two extractions. The first impregnation extraction is: add a compound extraction solution according to the mass ratio of material to liquid of 1:7, impregnate for 48 h, filter through a 100-mesh sieve, and pump the impregnation solution into the storage tank; the second impregnation extraction is: add a compound extraction solution according to the mass ratio of material to liquid of 1:6, impregnate for 24 h, filter through a 100-mesh sieve, and pump the impregnation solution into the storage tank. Combine the two impregnation solutions to obtain the areca flower extraction solution. The compound extraction solution is a mixed solution of ethanol, ether and chloroform, and their volume ratio is 1:0.25:0.25; the ethanol is an ethanol solution with a volume concentration of 65%, and the ethanol solution contains a phosphate buffer solution.

[0107] S6. Pump the areca flower extraction solution into a single-effect concentrator for concentration until it is concentrated to about 700 mL; the evaporation chamber concentration temperature of the single-effect concentrator is 40 - 90°C, the vacuum temperature is 0.02 - 0.095 Mpa, the steam pressure < 0.1 Mpa, and the concentration time of the areca flower extraction solution is 30 min.

[0108] S7. Add 3.5 g of activated carbon to the concentrated solution for decolorization to obtain a clear and transparent decolorized filtrate.

[0109] S8. Concentrate the decolorized filtrate into a fluid extract, add 3 g of sodium benzoate, refrigerate at 4 - 10 °C for 24 h, and filter with a 300 - mesh filter cloth.

[0110] S9. Take another 100 g of honey, dissolve it in 400 mL of water, boil, filter to obtain refined honey. Add the refrigerated filtrate of the fluid extract and the refined honey into a preparation tank, add water to 1000 mL, stir, filter, dispense into 10 - mL vials, then set the sterilization parameters: sterilization temperature 115 °C, sterilization time 30 min, and perform sterilization to obtain betel flower oral liquid.

[0111] Before preparing the betel flower oral liquid in the above examples and comparative examples, it is necessary to conduct cleaning validation on the percolation tank, impregnating solution storage tank, single - effect concentrator, and preparation tank.

[0112] Determine the alkaloid content and clarity of the betel flower oral liquid prepared in the above examples and comparative examples, and the results are shown in Table 1.

[0113] Determination of clarity: Use spectrophotometry to measure the transmittance of the betel flower oral liquid. The clarity is expressed by the transmittance. The greater the transmittance, the higher the clarity. Using distilled water as the blank, measure the absorbance value at 590 - 610 nm.

[0114] Determination of alkaloid content: Take 10 mL of the betel flower oral liquid, add 80 mL of ether, shake well, add 4 mL of ammonia reagent, shake for 10 min, add 10 g of anhydrous sodium sulfate, shake for 10 min, let stand, separate and remove the ether. Wash the residue with ether 3 times, 10 mL each time. Combine the ether washing solutions, add 0.5 g of talc powder, shake for 10 min, let stand, separate and remove the ether layer. Wash the aqueous layer with a small amount of ether 2 times. Combine the ether washing solutions and the ether layer, evaporate the ether solution at low temperature to about 20 mL, add 20 mL of 0.01 M sulfuric acid titrant, shake for 10 min, let stand, separate and remove the ether layer. Extract the ether layer with water by shaking 3 times, 5 mL each time. Combine the washing solutions and the acid solution, add 2 - 3 drops of methyl red indicator, and titrate with 0.01 M standard sodium hydroxide titrant. Perform parallel determination 3 times. Among them, the alkaloid is ether - soluble alkaloid, and the ether - soluble alkaloid is calculated as arecoline (C8H 13 NO2).

[0115] Table 1

[0116] <![CDATA[Alkaloid / mg·mL -1 > Transmittance / % Example 1 0.176 70.2％ Comparative Example 1 0.171 70.6％ Comparative Example 2 0.155 70.5％ Comparative Example 3 0.158 69.2％ Comparative Example 4 0.161 69.9％ Comparative Example 5 0.163 70.0％ Comparative Example 6 0.170 69.5％

[0117] As shown in Table 1, compared with Comparative Example 1 and Comparative Example 2, when areca flowers at different flowering stages are used in the preparation process of areca flower oral liquid, the synthesis and accumulation of alkaloids also decrease; compared with Comparative Example 3, the tissue structure of areca flowers becomes fragile after freezing and is easier to be pulverized, which helps to improve the release of active ingredients in areca flowers, thereby improving the extraction efficiency. At the same time, since the particle size of the powder after cryogenic ultrafine pulverization is uniform and fine, it is beneficial to better disperse in the impregnation extract and reduce the precipitation of large particle substances, thereby improving the clarity of the solution. Compared with Comparative Example 4 and Comparative Example 5, the efficiency of extracting alkaloids with a composite extract is higher, and the stability of sodium carbonate - sodium bicarbonate is more affected by temperature than that of phosphate buffer solution. Compared with Comparative Example 6, low-temperature impregnation extraction can protect the stability of bioactive ingredients, reduce some reactions during the extraction process, and thus enhance the extraction efficiency and clarity.

[0118] The present application has been described in detail above in combination with specific embodiments and exemplary embodiments, but these descriptions should not be construed as limiting the present application. Those skilled in the art understand that without departing from the spirit and scope of the present application, various equivalent substitutions, modifications or improvements can be made to the technical solutions and their implementation manners of the present application, and all of these fall within the scope of the present application.

Claims

1. A method for preparing betel nut flower oral liquid, characterized in that: The following steps are involved: S1. Select the betel nut flower medicinal materials in the early flowering stage, remove the non-medicinal parts, foreign matter, moldy and insect-infested medicinal materials, and obtain the cleaned betel nut flower medicinal materials; S2, cutting the cleaned and selected Areca nut flower medicinal material to obtain cut medicinal material; S3, coarsely chopping the cut medicinal materials to obtain coarsely chopping medicinal materials with a coarse granularity of less than 5 mm; S4, freezing the roughly crushed medicinal materials, and ultrafine grinding them to a particle size of 1 to 10 μm to obtain betel nut flower pre-treated medicinal materials; S5, performing low-temperature immersion extraction on the pre-treated betel nut flower medicinal material to obtain a betel nut flower extract; the solution used for the immersion extraction is a composite extract, which is a mixture of ethanol, ether and chloroform, the ethanol is an ethanol solution with a volume concentration of 60-70%, and the ethanol solution contains a phosphate buffer solution; S6, pumping the betel nut flower extract into a single-effect concentrator for concentration; S7, adding activated carbon at a dosage ratio of 200L:1kg for decolorization to obtain a clear and transparent decolorized filtrate; S8, concentrating the decolorized filtrate into a fluid extract, adding sodium benzoate, refrigerating, and filtering; S9. Add the refrigerated filtrate of the fluid extract and refined honey into a preparation tank, add water, stir, filter, package, and sterilize to obtain the betel nut flower oral liquid.

2. The method for preparing the betel nut flower oral liquid according to claim 1, characterized in that: The moisture content of the cleaned betel nut flower medicinal material does not exceed 3wt.%.

3. The method for preparing the betel nut flower oral liquid according to claim 1, characterized in that: The length of the cut medicinal materials is less than 8 cm for no less than 90%.

4. The method for preparing the betel nut flower oral liquid according to claim 1, characterized in that: The temperature of the freezing treatment is -20 to -40°C, and the time of the freezing treatment is 10 to 30 minutes.

5. The method for preparing the betel nut flower oral liquid according to claim 1, characterized in that: The volume ratio of ethanol, ether and chloroform in the composite extract is 1:0.2-0.3:0.2-0.

3.

6. The method for preparing the betel nut flower oral liquid according to claim 1, characterized in that: The temperature of the low-temperature immersion extraction is 4 to 10° C.; the immersion extraction includes two extractions, the first immersion extraction is: adding the composite extract according to the mass ratio of the material to the liquid of 1:6 to 8, immersion extraction for 45 to 50 hours, filtering, and pumping the immersion liquid into a storage tank; the second immersion extraction is: adding the composite extract according to the mass ratio of the material to the liquid of 1:5 to 7, immersion extraction for 20 to 30 hours, filtering, and pumping the immersion liquid into a storage tank to obtain the betel nut flower extract.

7. The method for preparing the betel nut flower oral liquid according to claim 1, characterized in that: The fluid extract contains 0.24-0.36 mg of ether-soluble alkaloids in terms of arecoline per 1 mL.

8. The method for preparing the betel nut flower oral liquid according to claim 1, characterized in that: The betel nut flower oral liquid contains 0.1 to 0.2 mg of ether-soluble alkaloids in terms of arecoline per 1 mL.

9. The method for preparing the betel nut flower oral liquid according to claim 1, characterized in that: The concentration temperature of the evaporation chamber of the single-effect concentrator is 40-90° C., the vacuum temperature is 0.02-0.095 MPa, and the steam pressure is less than 0.1 MPa.

10. The method for preparing the betel nut flower oral liquid according to claim 1, characterized in that: The prepared betel nut flower oral liquid contains 233g of betel nut flower, 3.5g of activated carbon, 3g of sodium benzoate and 100g of honey in every 1000mL.