Preparation method of Sini Tang preparation and Sini Tang preparation

Abstract

The present invention relates to the technical field of traditional Chinese medicine preparations, and discloses a preparation method of a Sini Tang preparation and a Sini Tang preparation. In the preparation method provided by the present invention, by subjecting the water extraction mixed solution to a primary heat concentration treatment, and subjecting the alcohol precipitation filtrate to a secondary heat concentration treatment, and adding a mixing and co-heating step after adding a flavoring agent solution, the medicinal solution can be prompted to reach a dynamic equilibrium in terms of thermodynamics and kinetics, thereby significantly improving the stability and clarity of Sini Tang.

Description

Technical Field

[0001] The present invention relates to the technical field of traditional Chinese medicine preparations, and in particular to a preparation method of a Sini Decoction preparation and the Sini Decoction preparation. Background Art

[0002] The functions and indications of Sini Decoction are yang deficiency and collapse, spontaneous cold sweats, cold limbs, diarrhea, and weak pulse. Because of its remarkable effect of restoring yang, warming the interior and dispelling cold, it is known as the best prescription for restoring yang and rescuing from adverse conditions. It is often used in modern clinical practice to treat coronary heart disease, angina pectoris, heart failure, myocardial infarction and other diseases, and has good therapeutic effects.

[0003] Sini Decoction is made of three herbs: Radix Aconiti Lateralis Preparata, dried ginger and licorice root. The preparation process involves distillation of dried ginger, boiling and extraction of the three herbs, and precipitation with alcohol and water. However, in the process of realizing the present invention, the inventors found that the finished Sini Decoction prepared in the related art is prone to excessive precipitation and poor clarity of the medicine solution after being exposed to oxygen, heated, or left for a long time. Summary of the invention

[0004] In view of this, the present invention provides a preparation method of Sini Decoction preparation and Sini Decoction preparation, so as to solve the problem that the Sini Decoction finished product prepared in the related art is prone to excessive precipitation and poor clarity of the medicinal solution after being exposed to oxygen, heated, left for a long time, etc.

[0005] In a first aspect, the present invention provides a method for preparing a Sini Decoction preparation, comprising the following steps:

[0006] Take the water extraction mixture of Radix Aconiti Lateralis Preparata, dried ginger and licorice root, and heat and concentrate it once to obtain the first solution;

[0007] Take the first solution, perform alcohol precipitation and let it stand, and perform solid-liquid separation to obtain a second solution;

[0008] The second solution is taken, subjected to secondary heating and concentration and water precipitation, and subjected to secondary solid-liquid separation to obtain a third solution;

[0009] Take the third solution, add the flavoring agent solution, mix and heat, and perform three solid-liquid separations to obtain a fourth solution;

[0010] Take the fourth solution, add the preservative solution and the dried ginger volatile oil extract, and make up to volume.

[0011] The inventors have found that since Chinese medicinal materials contain high-molecular substances such as starch, gum, pectin, mucus, protein, tannin, resin, pigment, etc., the prepared Sini Decoction finished product often contains some unstable components, and the conventional water extraction and alcohol precipitation method can only remove most of the high-molecular impurities in the liquid medicine. Other substances such as alkaloids, salts, glycosides, organic acids and their salts, amino acids, saponins, anthraquinones, flavonoids, inorganic salts, tannins, pigments, resins, gum, pectin, proteins, polysaccharides, etc. will affect the stability and clarity of the Sini Decoction finished product. In particular, when the Sini Decoction finished product is in contact with oxygen, heated or left for a long time, it is more likely to have problems of excessive precipitation and poor clarity of the liquid medicine.

[0012] In the above-mentioned preparation method provided by the present invention, by subjecting the water extraction mixture to a first heat concentration treatment, and subjecting the alcohol precipitation filtrate to a second heat concentration treatment, and adding a mixing and co-heating step after adding the flavoring agent solution, the medicinal solution can be prompted to reach a dynamic equilibrium in terms of thermodynamics and kinetics, thereby significantly improving the stability and clarity of Sini Decoction.

[0013] In an optional embodiment, the conditions of the primary heat concentration include: vacuum degree of -0.08MPa to 0MPa, temperature of 60°C to 100°C, and concentration to 30% to 50% of the target volume of the finished product;

[0014] Optionally, the time for the first heat concentration is 3 hours to 12 hours.

[0015] In an optional embodiment, before the first solution is subjected to alcohol precipitation and allowed to stand, the step of cooling the first solution to below 40° C. is also included;

[0016] Optionally, the conditions for the alcohol precipitation include: the amount of the alcohol solvent is 3 to 4 times the volume of the first solution, and the standing time is 24 to 96 hours;

[0017] Optionally, the temperature difference between the alcohol solvent and the first solution does not exceed 30°C;

[0018] Optionally, the concentration of alcohol in the alcohol solvent is 80% to 97%;

[0019] Optionally, the primary solid-liquid separation includes clarification plate filtration and membrane filtration, the pore size of the clarification plate is 0.2 μm to 6 μm, and the pore size of the membrane is 0.1 μm to 0.45 μm.

[0020] In an optional embodiment, the conditions for the secondary heat concentration include: vacuum degree of -0.08MPa to 0MPa, temperature of 60°C to 100°C, and concentration to 10% to 30% of the target volume of the finished product;

[0021] Optionally, the time for the secondary heating and concentration is 1 h to 8 h.

[0022] In an optional embodiment, before the water precipitation, the step of cooling the second heated concentrated solution to below 40° C. is also included;

[0023] Optionally, the conditions for the water sedimentation to stand still include: the amount of water used is 2 to 5 times the volume of the second heated concentrated solution of the second solution, and the standing time is 24 to 96 hours;

[0024] Optionally, the temperature difference between water and the second heated concentrate of the second solution does not exceed 30°C;

[0025] Optionally, the secondary solid-liquid separation includes clarification plate filtration and membrane filtration, the pore size of the clarification plate is 0.2 μm to 6 μm, and the pore size of the membrane is 0.1 μm to 0.45 μm.

[0026] In an optional embodiment, the concentration of the flavoring solution is 0.70 g / mL to 0.90 g / mL, and the amount of the flavoring solution is 0.5 to 0.6 times the volume of the third solution;

[0027] Optionally, the flavoring agent includes at least one of sucrose, sorbitol and aspartame;

[0028] Optionally, the temperature of the mixed co-heating is 60°C to 100°C, and the time is 20min to 60min;

[0029] Optionally, the three solid-liquid separations include clarification plate filtration and membrane filtration, the pore size of the clarification plate is 0.2 μm to 6 μm, and the pore size of the membrane is 0.1 μm to 0.45 μm.

[0030] In an optional embodiment, the concentration of the preservative solution is 0.012 g / mL to 0.12 g / mL, and the amount of the preservative solution is 0.022 to 0.028 times the volume of the fourth solution;

[0031] Optionally, the preservative includes at least one of sodium benzoate, potassium sorbate, methylparaben and ethylparaben.

[0032] In an optional embodiment, the Sini Decoction comprises the following raw materials in parts by weight:

[0033] 300 parts by weight of Radix Aconiti Lateralis Preparata, 200 parts by weight of dried ginger, and 300 parts by weight of roasted liquorice root.

[0034] In the above-mentioned preparation method provided by the present invention, by controlling the temperature difference between the drug solution and the alcohol solvent and the water solvent to not exceed 30°C, standardizing the standing time timing standard, and using a clarification plate (fine filter paperboard) and a filter membrane for multiple filtrations, it is possible to prevent the effective components from being precipitated while further ensuring that the impurity components are fully settled and removed.

[0035] The preparation method provided by the present invention has the advantages of wide raw material sources, low cost, no need for special equipment, etc., is suitable for large-scale preparation, and is conducive to industrial production; the content (not less than 0.55 mg / mL), pH, identification and other indicators of the prepared Sini Decoction all meet the pharmacopoeia standards, and no precipitation occurs when stored for at least 6 months under the conditions of 40°C±2°C and 75%±5%; the product functions and indications are yang deficiency, spontaneous cold sweat, limb coldness, diarrhea, weak pulse, etc., and has the advantages of good economic benefits, wide application, significant efficacy, etc.

[0036] In a second aspect, the present invention also provides a Sini Decoction preparation prepared by the above-described method. BRIEF DESCRIPTION OF THE DRAWINGS

[0037] In order to more clearly illustrate the specific implementation methods of the present invention or the technical solutions in the prior art, the drawings required for use in the specific implementation methods or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are some implementation methods of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0038] Figure 1 This is a picture of the finished product of Sini Decoction prepared in Example 1 of Experimental Example 1 of the present invention after 6 months of stability inspection under high temperature and high humidity conditions. DETAILED DESCRIPTION

[0039] The following examples are provided for a better understanding of the present invention, but are not intended to limit the best mode of implementation, nor to limit the content and protection scope of the present invention. Any product identical or similar to the present invention obtained by anyone under the inspiration of the present invention or by combining the features of the present invention with other prior arts shall fall within the protection scope of the present invention.

[0040] If no specific experimental steps or conditions are specified in the examples, the conventional experimental steps or conditions described in the literature in the field can be used. If no manufacturer is specified for the reagents or instruments used, they are all conventional reagent products that can be obtained commercially.

[0041] In order to solve the problems existing in the above-mentioned related art, according to a first aspect of the present invention, a method for preparing a Sini Decoction preparation is provided, comprising the following steps:

[0042] Take the water extraction mixture of Radix Aconiti Lateralis Preparata, dried ginger and licorice root, and heat and concentrate it once to obtain the first solution;

[0043] Take the first solution, perform alcohol precipitation and let it stand, and perform solid-liquid separation to obtain a second solution;

[0044] The second solution is taken, subjected to secondary heating and concentration and water precipitation, and subjected to secondary solid-liquid separation to obtain a third solution;

[0045] Take the third solution, add the flavoring agent solution, mix and heat, and perform three solid-liquid separations to obtain a fourth solution;

[0046] Take the fourth solution, add the preservative solution and the dried ginger volatile oil extract, and make up to volume.

[0047] The inventors have found that since Chinese medicinal materials contain high-molecular substances such as starch, gum, pectin, mucus, protein, tannin, resin, pigment, etc., the prepared Sini Decoction finished product often contains some unstable components, and the conventional water extraction and alcohol precipitation method can only remove most of the high-molecular impurities in the liquid medicine. Other substances such as alkaloids, salts, glycosides, organic acids and their salts, amino acids, saponins, anthraquinones, flavonoids, inorganic salts, tannins, pigments, resins, gum, pectin, proteins, polysaccharides, etc. will affect the stability and clarity of the Sini Decoction finished product. In particular, when the Sini Decoction finished product is in contact with oxygen, heated or left for a long time, it is more likely to have problems of excessive precipitation and poor clarity of the liquid medicine.

[0048] In the above-mentioned preparation method provided by the present invention, by subjecting the water extraction mixture to a first heat concentration treatment, and subjecting the alcohol precipitation filtrate to a second heat concentration treatment, and adding a mixing and co-heating step after adding the flavoring agent solution, the medicinal solution can be prompted to reach a dynamic equilibrium in terms of thermodynamics and kinetics, thereby significantly improving the stability and clarity of Sini Decoction.

[0049] The preparation process of the water extraction mixture and the dried ginger volatile oil extract may include (the multiple refers to the number of milliliters of water added per gram of Chinese medicinal materials):

[0050] The Radix Aconiti Lateralis and Radix Glycyrrhizae are decocted in water twice, the first time for 2 hours (7-10 times the amount of water) and the second time for 1.5 hours (4-8 times the amount of water), the decoctions are combined and filtered; the volatile oil is extracted from the dried ginger by steam distillation, and the volatile oil and the distilled aqueous solution are reserved; the ginger residue is decocted in water for another hour (4-8 times the amount), the decoction is combined with the above-mentioned distilled aqueous solution, filtered, and then combined with the decoctions of Radix Aconiti Lateralis and Radix Glycyrrhizae to obtain a water-extracted mixed solution.

[0051] In an optional embodiment, the conditions of the primary heat concentration include: vacuum degree of -0.08MPa to 0MPa, temperature of 60°C to 100°C, and concentration to 30% to 50% of the target volume of the finished product, for example, 40%;

[0052] Optionally, the time for the first heat concentration is 3 h to 12 h, for example 10 h.

[0053] In an optional embodiment, before the first solution is subjected to alcohol precipitation and allowed to stand, the step of cooling the first solution to below 40° C. is also included;

[0054] Optionally, the conditions for the alcohol precipitation include: the amount of the alcohol solvent is 3 to 4 times the volume of the first solution, and the standing time is 24 hours to 96 hours; for example, the amount of the alcohol solvent is 3 times the volume of the first solution, the standing time is 24 hours, and the standing can be refrigerated standing;

[0055] Optionally, the temperature difference between the alcohol solvent and the first solution does not exceed 30°C;

[0056] Optionally, the concentration of alcohol in the alcohol solvent is 80% to 97%;

[0057] Optionally, the primary solid-liquid separation includes clarification plate filtration and membrane filtration, the pore size of the clarification plate is 0.2 μm to 6 μm, and the pore size of the membrane is 0.1 μm to 0.45 μm.

[0058] In an optional embodiment, the conditions of the secondary heat concentration include: vacuum degree of -0.08MPa to 0MPa, temperature of 60°C to 100°C, and concentration to 10% to 30% of the target volume of the finished product, for example, 15%;

[0059] Optionally, the time for the secondary heating and concentration is 1 h to 8 h, for example 6 h.

[0060] In an optional embodiment, before the water precipitation, the step of cooling the second heated concentrated solution to below 40° C. is also included;

[0061] Optionally, the conditions for the water sedimentation include: the amount of water used is 2 to 5 times the volume of the second heated concentrated solution of the second solution, and the standing time is 24 hours to 96 hours; illustratively, the standing is refrigerated standing, and the standing time is 24 hours;

[0062] Optionally, the temperature difference between water and the second heated concentrate of the second solution does not exceed 30°C;

[0063] Optionally, the secondary solid-liquid separation includes clarification plate filtration and membrane filtration, the pore size of the clarification plate is 0.2 μm to 6 μm, and the pore size of the membrane is 0.1 μm to 0.45 μm.

[0064] In an optional embodiment, the concentration of the flavoring solution is 0.70 g / mL to 0.90 g / mL, and the amount of the flavoring solution is 0.5 to 0.6 times the volume of the third solution;

[0065] Optionally, the flavoring agent includes at least one of sucrose, sorbitol and aspartame;

[0066] Optionally, the temperature of the mixed co-heating is 60°C to 100°C, and the time is 20min to 60min;

[0067] Optionally, the three solid-liquid separations include clarification plate filtration and membrane filtration, the pore size of the clarification plate is 0.2 μm to 6 μm, and the pore size of the membrane is 0.1 μm to 0.45 μm.

[0068] In an optional embodiment, the concentration of the preservative solution is 0.012 g / mL to 0.12 g / mL, and the amount of the preservative solution is 0.022 to 0.028 times the volume of the fourth solution;

[0069] Optionally, the preservative includes at least one of sodium benzoate, potassium sorbate, methylparaben and ethylparaben.

[0070] In an optional embodiment, the Sini Decoction comprises the following raw materials in parts by weight:

[0071] 300 parts by weight of Radix Aconiti Lateralis Preparata, 200 parts by weight of dried ginger, and 300 parts by weight of roasted liquorice root.

[0072] In the above-mentioned preparation method provided by the present invention, by controlling the temperature difference between the drug solution and the alcohol solvent and the water solvent to not exceed 30°C, standardizing the standing time timing standard, and using a clarification plate (fine filter paperboard) and a filter membrane for multiple filtrations, it is possible to prevent the effective components from being precipitated while further ensuring that the impurity components are fully settled and removed.

[0073] The preparation method provided by the present invention has the advantages of wide raw material sources, low cost, no need for special equipment, etc., is suitable for large-scale preparation, and is conducive to industrial production; the content (not less than 0.55 mg / mL), pH, identification and other indicators of the prepared Sini Decoction all meet the pharmacopoeia standards, and no precipitation occurs when stored for at least 6 months under the conditions of 40°C±2°C and 75%±5%; the product functions and indications are yang deficiency, spontaneous cold sweat, limb coldness, diarrhea, weak pulse, etc., and has the advantages of good economic benefits, wide application, significant efficacy, etc.

[0074] In a second aspect, the present invention also provides a Sini Decoction preparation prepared by the above-described method.

[0075] The present invention is further described in detail below in conjunction with specific embodiments. These embodiments should not be construed as limiting the scope of protection claimed by the present invention.

[0076] Example 1

[0077] In this embodiment, 1000 mL of Sini Decoction was prepared using 300 g of Radix Aconiti Lateralis Preparata, 200 g of dried ginger, 300 g of Radix Glycyrrhizae Preparata, 255 g of sucrose, and 3 g of sodium benzoate. The specific preparation method is as follows:

[0078] (1) Boil and extract with Radix Aconiti Lateralis Preparata and Radix Licorice

[0079] According to the weight of the Sini Decoction recipe, 300g of Radix Aconiti Lateralis and 300g of Radix Glycyrrhizae were weighed respectively; the Radix Aconiti Lateralis and Radix Glycyrrhizae were mixed, 4800mL of water (8 times the amount) was added and boiled for 2 hours, and the decoction was filtered through an 80-mesh stainless steel sieve; 3600mL of water (6 times the amount) was added to the filter residue and boiled for 1.5 hours, and the decoction was filtered through an 80-mesh stainless steel sieve; the filtrates filtered through the stainless steel sieves twice were combined to obtain the decoction extract of Radix Aconiti Lateralis and Radix Glycyrrhizae.

[0080] (2) Distillation and boiling of dried ginger

[0081] Weigh 200 g of dried ginger, suspend it on an 80-mesh stainless steel steamer, and perform steam distillation in a sealed stainless steel barrel containing 2000 mL of water to extract 50 mL of volatile oil. The volatile oil and the distilled aqueous solution are set aside; add 1200 mL of water (6 times the amount) to the ginger residue and boil for 1 hour. The decoction is combined with the above-mentioned distilled aqueous solution, and filtered through an 80-mesh stainless steel sieve to obtain the dried ginger water extract.

[0082] (3) The water extraction mixture is heated and concentrated once

[0083] The decoction extracts of Radix Aconiti Lateralis and Radix Glycyrrhizae and the water extract of dried ginger are combined to obtain a water extract mixture, which is heated and concentrated for 10 hours (vacuum degree: -0.08MPa~0MPa, temperature: 60℃~100℃) to 40% of the target volume of the finished product (volume: about 400mL) to obtain the first solution.

[0084] (4) Alcohol precipitation

[0085] The first solution was cooled to below 40°C, 1200 mL of 95% ethanol was added (the temperature difference between the first solution and 95% ethanol was not more than 30°C), stirred for 15 min, and refrigerated for 24 hours; after standing, the obtained solution was filtered through a clarification plate (1.5-3 μm) + a polypropylene filter membrane (0.45 μm) to obtain a second solution.

[0086] (5) Water sink

[0087] The second solution was concentrated by secondary heating for 6 h (vacuum degree: -0.08 MPa ~ 0 MPa, temperature 60 ° C ~ 100 ° C), concentrated to 20% of the target volume of the finished product (volume of about 200 mL), cooled to below 40 ° C, added with purified water to 600 mL (the amount of purified water added is 2 times the volume of the secondary heated concentrated solution, and the temperature difference does not exceed 30 ° C), refrigerated for 24 hours, and the obtained drug solution was filtered through a clarification plate (1.5-3 μm) + polypropylene filter membrane (0.45 μm) to obtain a third solution.

[0088] (6) Preparation of monosaccharide syrup (flavoring agent solution)

[0089] Take 135mL of purified water, heat to 60℃±5℃, add 255g of sucrose, add purified water to 300mL, stir while adding, continue heating to 100℃ and start timing, heat for 5min to obtain monosaccharide syrup, filter the monosaccharide syrup through a 200-mesh stainless steel sieve while hot, and cool to 50-60℃.

[0090] (7) Preparation

[0091] The third solution is heated to 50-60°C, 300 mL of monosaccharide syrup is added while stirring, and heating is continued to 100°C and timing is started. Mix and heat for 20 minutes, cool, and filter through a clarification plate (1.5-3 μm) + a polypropylene filter membrane (0.45 μm) until clear to obtain a fourth solution;

[0092] Take the fourth solution, add 25 mL of sodium benzoate solution (containing 3 g of sodium benzoate), then add 50 mL of dried ginger volatile oil extract, add water to make the volume to 1000 mL, stir well, filter through a 0.45 μm polypropylene filter membrane and wait for potting.

[0093] (8) Filling and sterilization

[0094] The above-mentioned drug solution was filled into a 10 mL soda-lime glass tube oral liquid bottle (the oral liquid bottle was equipped with an easy-to-puncture aluminum cap and a silicone stopper) and sterilized (sterilization conditions: 100° C., 30 min).

[0095] Example 2

[0096] Sini Decoction was prepared according to the method of Example 1, except that in step (1) of this embodiment, Radix Aconiti Lateralis Preparata and Radix Glycyrrhizae Radix were mixed, 4200 mL of water (7 times the amount) was added and boiled for 2 hours, and the decoction was filtered through an 80-mesh stainless steel sieve; 3000 mL of water (5 times the amount) was added to the filter residue and boiled for 1.5 hours.

[0097] Example 3

[0098] Sini Decoction was prepared according to the method of Example 1, except that in step (1) of this embodiment, Radix Aconiti Lateralis Preparata and Radix Glycyrrhizae Radix were mixed, 6000 mL of water (10 times the amount) was added and boiled for 2 hours, and the decoction was filtered through an 80-mesh stainless steel sieve; 4800 mL of water (8 times the amount) was added to the filter residue and boiled for 1.5 hours.

[0099] Example 4

[0100] Sini Decoction was prepared according to the method of Example 1, except that in step (2) of this embodiment, 1600 mL of water (8 times the amount) was added to the ginger residue and boiled for 1 hour, and the decoction was combined with the above-mentioned distilled aqueous solution and filtered through an 80-mesh stainless steel sieve to obtain a dry ginger water extract.

[0101] Example 5

[0102] Sini Decoction was prepared according to the method of Example 1, except that in step (3) of this example, the water extraction mixture was subjected to a heat concentration for 12 hours.

[0103] Example 6

[0104] Sini Decoction was prepared according to the method of Example 1, except that in step (5) of this example, the second solution was heated and concentrated for a second time for 8 hours.

[0105] Example 7

[0106] Sini Decoction was prepared according to the method of Example 1, except that in step (7) of this example, after adding monosaccharide syrup to the third solution, the mixing and heating time was 60 minutes.

[0107] Comparative Example 1

[0108] Sini Decoction was prepared according to the method of Example 1, except that in step (3) of this comparative example, the water extraction mixture was concentrated under reduced pressure at room temperature to obtain the first solution; and in step (5), the second solution was decompressed at room temperature and then allowed to stand in water.

[0109] Comparative Example 2

[0110] Sini Decoction was prepared according to the method of Example 1, except that in step (3) of this comparative example, the water extraction mixture was concentrated under reduced pressure at room temperature to obtain the first solution.

[0111] Comparative Example 3

[0112] Sini Decoction was prepared according to the method of Example 1, except that in step (5) of this comparative example, the second solution was concentrated under reduced pressure at room temperature and then allowed to stand in water.

[0113] Comparative Example 4

[0114] Sini Decoction was prepared according to the method of Example 1, except that in step (7) of this comparative example, monosaccharide syrup, sodium benzoate solution and dried ginger volatile oil extract were added in sequence and fixed to volume, that is, after the monosaccharide syrup was added in step (7), mixing and heating were not performed.

[0115] Comparative Example 5

[0116] Sini Decoction was prepared according to the method of Example 1, except that in step (7) of this comparative example, after adding monosaccharide syrup to the third solution and mixing and heating, sodium benzoate solution and dried ginger volatile oil extract were directly added to the solution without solid-liquid separation and the volume was fixed.

[0117] Experimental Example 1

[0118] The Sini Decoction prepared in Examples 1-7 and Comparative Examples 1-5 were stored at room temperature and high temperature and humidity (temperature 40°C ± 2°C, humidity 75% ± 5%), respectively, and stability was investigated for 6 months. The time when precipitation of the medicinal solution occurred was observed and recorded during the storage process. The results are shown in Table 1.

[0119] Table 1 The time when each Sini Decoction solution precipitates

[0120] Sini Decoction Precipitation time due to high temperature and high humidity, days Precipitation time at room temperature, days Example 1 No precipitation No precipitation Example 2 No precipitation No precipitation Example 3 No precipitation No precipitation Example 4 No precipitation No precipitation Example 5 No precipitation No precipitation Example 6 No precipitation No precipitation Example 7 No precipitation No precipitation Comparative Example 1 1 14 Comparative Example 2 10 125 Comparative Example 3 10 130 Comparative Example 4 12 140 Comparative Example 5 10 40

[0121] As can be seen from Table 1, the preparation method of Sini Decoction provided by the present invention, by adopting a multi-place heating and concentration method to treat the decoction extract of the three herbs involved in the process route and the alcohol precipitation filtrate, and increasing the heating of the medicine liquid after the monosaccharide syrup, can promote the medicine liquid after the three herbs are fully compatible to reach a dynamic equilibrium in thermodynamics and kinetics, significantly improve the clarity and stability of the medicine liquid, and thus effectively alleviate the problem of precipitation of the medicine liquid after long-term storage.

[0122] The finished product of Sini Decoction prepared in Example 1 after 6 months of stability test under high temperature and high humidity conditions is shown in FIG. Figure 1 shown.

[0123] Experimental Example 2

[0124] This experimental example is used to verify the effect of the preparation method of the present invention on the content of the index component (glycyrrhizic acid) of the finished product of Sini Decoction.

[0125] Take the Sini Decoction prepared in Examples 1-7 and Comparative Examples 1-5 respectively, and detect the glycyrrhizic acid content in each medicinal solution according to the following method:

[0126] (1) Chromatographic conditions and system suitability test

[0127] Octadecylsilane bonded silica gel is used as filler; methanol-0.2 mol / L ammonium acetate solution-glacial acetic acid (67:33:1) is used as mobile phase; the detection wavelength is 250nm. The theoretical plate number calculated based on the glycyrrhizic acid peak should be no less than 2000.

[0128] (2) Preparation of reference solution

[0129] Take an appropriate amount of ammonium glycyrrhizinate reference substance, weigh it accurately, and add the mobile phase to make a reference substance solution containing 0.4 mg per 1 mL (equivalent to 0.3918 mg glycyrrhizic acid per 1 mL).

[0130] (3) Preparation of test solution

[0131] Accurately measure 10 mL of the product, place it in a 50 mL volumetric flask, add mobile phase to the scale, shake well, filter, and obtain the test solution.

[0132] (4) Determination method

[0133] Accurately pipette 10 μl of reference solution and test solution respectively, inject into liquid chromatograph, and measure. 42 H 62 O 16 ) shall not be less than 0.50 mg. The test results are shown in Table 2.

[0134] Table 2 Glycyrrhizic acid content in various Sini decoctions

[0135]

[0136]

[0137] It can be seen from Table 2 that the preparation method of Sini Decoction of the present invention will not affect the content of the index components in Sini Decoction.

[0138] Obviously, the above embodiments are merely examples for the purpose of clear explanation, and are not intended to limit the implementation methods. For those skilled in the art, other different forms of changes or modifications can be made based on the above description. It is not necessary and impossible to list all the implementation methods here. The obvious changes or modifications derived therefrom are still within the scope of protection of the invention.

Claims

1. A method for preparing a Sini Decoction preparation, characterized in that: In parts by weight, the Sini Decoction comprises the following raw materials: 300 parts by weight of Radix Aconiti Lateralis Preparata, 200 parts by weight of dried ginger, and 300 parts by weight of Radix Glycyrrhizae Preparata; the preparation method comprises the following steps: A water-extracted mixed solution of Radix Aconiti Lateralis, dried ginger and licorice root is heated and concentrated once to obtain a first solution; wherein the preparation method of the water-extracted mixed solution comprises: boiling Radix Aconiti Lateralis and licorice root with water twice, adding 7-10 times of water for the first time and 4-8 times of water for the second time, combining the decoctions and filtering; extracting volatile oil from dried ginger by steam distillation, and reserving the volatile oil and the distilled aqueous solution separately; boiling ginger residue with 4-8 times of water again, combining the decoction with the distilled aqueous solution, filtering, and then combining with the decoctions of Radix Aconiti Lateralis and licorice root to obtain a water-extracted mixed solution; The conditions of the primary heat concentration include: vacuum degree of -0.08MPa to 0MPa, temperature of 60°C to 100°C, concentration to 30% to 50% of the target volume of the finished product; the time of the primary heat concentration is 3h to 12h; Take the first solution, perform alcohol precipitation and let it stand, and perform solid-liquid separation to obtain a second solution; The second solution is taken, subjected to secondary heat concentration and water precipitation, and subjected to secondary solid-liquid separation to obtain a third solution; the conditions for the secondary heat concentration include: a vacuum degree of -0.08MPa to 0MPa, a temperature of 60°C to 100°C, and concentration to 10% to 30% of the target volume of the finished product; the time for the secondary heat concentration is 1h to 8h; Take the third solution, add the flavoring agent solution, mix and heat, and perform three solid-liquid separations to obtain a fourth solution; Take the fourth solution, add the preservative solution and the dried ginger volatile oil extract, and fix the volume; wherein the dried ginger volatile oil extract is the volatile oil extracted from dried ginger by steam distillation.

2. The preparation method according to claim 1, characterized in that: Before the first solution is subjected to alcohol precipitation and allowed to stand, the method further includes cooling the first solution to a temperature below 40°C.

3. The preparation method according to claim 2, characterized in that: The conditions for the alcohol precipitation include: the amount of the alcohol solvent is 3 to 4 times the volume of the first solution, and the standing time is 24 hours to 96 hours.

4. The preparation method according to claim 3, characterized in that: The temperature difference between the alcohol solvent and the first solution does not exceed 30°C.

5. The preparation method according to claim 4, characterized in that: The concentration of alcohol in the alcohol solvent is 80% to 97%.

6. The preparation method according to claim 5, characterized in that: The primary solid-liquid separation includes clarification plate filtration and membrane filtration, the pore size of the clarification plate is 0.2 μm to 6 μm, and the pore size of the membrane is 0.1 μm to 0.45 μm.

7. The preparation method according to claim 1, characterized in that: Before the water settling step, the method further includes cooling the second heated concentrated solution to below 40°C.

8. The preparation method according to claim 7, characterized in that: The conditions for the water sediment to stand still include: the amount of water used is 2 to 5 times the volume of the second heated concentrated solution of the second solution, and the standing time is 24 hours to 96 hours.

9. The preparation method according to claim 8, characterized in that: The temperature difference between water and the second heated concentrate of the second solution does not exceed 30°C.

10. The preparation method according to claim 9, characterized in that: The secondary solid-liquid separation includes clarification plate filtration and membrane filtration, the pore size of the clarification plate is 0.2 μm to 6 μm, and the pore size of the membrane is 0.1 μm to 0.45 μm.

11. The preparation method according to any one of claims 1 to 10, characterized in that: The concentration of the flavoring agent solution is 0.70 g / mL to 0.90 g / mL, and the amount of the flavoring agent solution used is 0.5 to 0.6 times the volume of the third solution.

12. The preparation method according to claim 11, characterized in that: The flavoring agent includes at least one of sucrose, sorbitol and aspartame.

13. The preparation method according to claim 12, characterized in that: The temperature of the mixed co-heating is 60° C. to 100° C., and the time is 20 min to 60 min.

14. The preparation method according to claim 13, characterized in that: The three solid-liquid separations include clarification plate filtration and membrane filtration, the pore size of the clarification plate is 0.2 μm to 6 μm, and the pore size of the membrane is 0.1 μm to 0.45 μm.

15. The preparation method according to any one of claims 1 to 10, characterized in that: The concentration of the preservative solution is 0.012 g / mL to 0.12 g / mL, and the amount of the preservative solution used is 0.022 to 0.028 times the volume of the fourth solution.

16. The preparation method according to claim 15, characterized in that: The preservative includes at least one of sodium benzoate, potassium sorbate, methylparaben and ethylparaben.

17. The Sini Decoction preparation prepared by the method according to any one of claims 1 to 16.

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