Production process, product and application of safflower Xiaoyao tablet

Abstract

The invention provides a production process, a product and application of a safflower Xiaoyao tablet, and belongs to the technical field of traditional Chinese medicine preparations. The production process of the safflower Xiaoyao tablet provided by the invention comprises the following steps: S1, extracting volatile oil from radix angelicae sinensis, rhizoma atractylodis macrocephalae and herba menthae to obtain a volatile oil mixture and medicine residues; s2, mixing the medicine residues obtained in the step S1 with radix paeoniae alba, poria cocos, flos carthami, spina gleditsiae, bupleurum chinense and liquorice, adding water, decocting, filtering, and concentrating filtrate to obtain thick paste; and S3, drying and crushing the thick paste obtained in the step S2, mixing with auxiliary materials, granulating, mixing with the volatile oil mixture obtained in the step S1, sealing, tabletting and coating to obtain the safflower Xiaoyao tablet. Wherein in the step S2, the filtration comprises screen filtration and ceramic membrane filtration, and the filtrate concentration comprises membrane concentration and vacuum concentration. By improving the procedures of filtering and concentrating the filtrate, the energy consumption is obviously reduced, and the production cost is reduced while the preparation requirements are met.

Description

Technical Field

[0001] The present invention belongs to the field of traditional Chinese medicine preparations, and relates to a production process, product and application of Honghua Xiaoyao tablets. Background Art

[0002] Honghua Xiaoyao tablets are a compound traditional Chinese medicine preparation, which are prepared from traditional Chinese medicine raw materials including Angelica sinensis, Paeonia lactiflora, Atractylodes macrocephala, Poria cocos, Carthamus tinctorius, Gleditsia sinensis spine, Bupleurum chinense DC. var. glabrum, Mentha haplocalyx Briq. and Glycyrrhiza uralensis Fisch. Honghua Xiaoyao tablets are a liver-soothing and qi-regulating medicine, and have the effects of soothing the liver, regulating qi and activating blood circulation. They are mainly used to treat symptoms such as chest and hypochondrium distending pain, dizziness, anorexia, irregular menstruation, breast distending pain and facial chloasma caused by liver qi stagnation.

[0003] Chinese Patent Application CN109394852A provides a granulation process for Honghua Xiaoyao tablets. The dry extract powder of Honghua Xiaoyao tablets and corn starch are premixed for 5 - 15 minutes, made into soft materials with 60% ethanol, made into wet granules with a 14 - 18 mesh sieve, the granulated granules, volatile oil and magnesium stearate are added to a two-dimensional mixer and mixed evenly for 25 - 35 minutes, sent for inspection, pressed into tablets and coated. The present invention can reduce the two processes of drying and granulation, reduce costs, and the content of Paeonia lactiflora in Honghua Xiaoyao tablets is more than 50% higher than that after drying, ensuring that the effective prescription is not lost and ensuring the clinical efficacy.

[0004] Chinese Patent Application CN109682918A provides a quality detection method for Honghua Xiaoyao tablets. This method newly adopts thin-layer chromatography to identify Poria cocos, and uses high-performance liquid chromatography to determine the content of liquiritin. This quality control method is more effective for product quality control, and the precision, sensitivity and stability of the method are all relatively high.

[0005] Chinese Patent Application CN102204967A provides a preparation method for Honghua Xiaoyao tablets, which successively includes the following steps: ① Using the method of steam distillation to extract the volatile oils of three traditional Chinese medicines, namely Angelica sinensis, Atractylodes macrocephala and Mentha haplocalyx Briq.; ② The medicinal residues after extracting the volatile oils are used together with Paeonia lactiflora, Poria cocos, Carthamus tinctorius, Gleditsia sinensis spine, Bupleurum chinense DC. var. glabrum and Glycyrrhiza uralensis Fisch. as solvents, and ultrasonic extraction is used to obtain water extracts; ③ The extracted volatile oils are included with β-cyclodextrin to obtain volatile oil β-cyclodextrin inclusion compounds; ④ The water extracts obtained in step ② and the volatile oil β-cyclodextrin inclusion compounds obtained in step ③ are added with starch, granulated and pressed into tablets, and film-coated to obtain the product. This method can quickly dissolve the effective components in the medicinal materials cells without destroying the chemical structure of the effective components, and has a high extraction rate. In the method of adding volatile oils, the β-cyclodextrin inclusion technology is adopted, which effectively increases the retention index of traditional Chinese medicine volatile components in the preparation.

[0006] However, the existing technologies have not yet provided a production process for Honghua Xiaoyao tablets that can reduce production energy consumption and costs without affecting product quality. Summary of the Invention

[0007] In view of this, aiming at the problem that the prior art cannot provide a production process of Honghua Xiaoyao Tablets that can reduce production energy consumption and costs without affecting product quality, the purpose of the present invention is to provide a production process, product and application of Honghua Xiaoyao Tablets.

[0008] To achieve the above-mentioned invention purpose, on the one hand, the present invention provides a production process of Honghua Xiaoyao Tablets, including the following steps:

[0009] S1. Extract volatile oil from Angelica sinensis, Atractylodes macrocephala and Mentha haplocalyx to obtain a volatile oil mixture and medicinal residues; S2. Mix the medicinal residues obtained in step S1 with Paeonia lactiflora, Poria cocos, Carthamus tinctorius, Gleditsia sinensis Lam., Bupleurum chinense DC. and Glycyrrhiza uralensis Fisch., decoct with water, filter, and concentrate the filtrate to obtain a thick paste; S3. Dry and pulverize the thick paste obtained in step S2, mix with auxiliary materials, granulate, mix with the volatile oil mixture obtained in step S1, seal, press tablets, and coat the tablets to obtain Honghua Xiaoyao Tablets; wherein, in step S2, the filtration includes screen filtration and ceramic membrane filtration, and the concentration of the filtrate includes membrane concentration and vacuum concentration.

[0010] Preferably, in step S2, the screen filtration uses a filter with a screen mesh of 80 - 120 meshes. More preferably, and as an example of the present invention, in step S2, the screen filtration uses a filter with a 100 - mesh screen.

[0011] Preferably, in step S2, the vacuum concentration uses a double - effect energy - saving concentrator. More preferably, and as an example of the present invention, in step S2, the vacuum concentration uses an EJZN - 2500 double - effect energy - saving concentrator.

[0012] Preferably, in step S2, the ceramic membrane filtration uses a ceramic membrane filter with a pore size of 5 - 200 nm, and the membrane concentration uses a reverse osmosis organic membrane concentrator or a nanofiltration organic membrane concentrator.

[0013] More preferably, in step S2, the ceramic membrane filtration uses a ceramic membrane filter with a pore size of 5 nm, 15 nm, 100 nm or 200 nm.

[0014] Still more preferably, and as an example of the present invention, in step S2, the ceramic membrane filtration uses a ceramic membrane filter with a pore size of 100 nm.

[0015] Preferably, in step S2, the material of the ceramic membrane filter used in the ceramic membrane filtration is alumina.

[0016] Preferably, in step S2, the membrane concentration uses a reverse osmosis organic membrane concentrator or a nanofiltration organic membrane concentrator.

[0017] More preferably, and as an example of the present invention, in step S2, the membrane concentration uses a reverse osmosis organic membrane concentrator.

[0018] Preferably, in step S2, the material of the membrane concentrator used for membrane concentration is polyamide.

[0019] Preferably, in step S2, the concentration of the filtrate includes the following steps: the filtrate is concentrated by membrane to 5%-30% of the original volume, and then concentrated under reduced pressure at 75-85 °C to a relative density of 1.37-1.43.

[0020] More preferably, and as an example of the present invention, the concentration of the filtrate includes the following steps: the filtrate is concentrated by membrane to 10%-30% of the original volume, and then concentrated under reduced pressure at 80 °C to a relative density of 1.37-1.43.

[0021] Preferably, in step S2, the excipients include fillers and lubricants. The fillers are selected from one or more of dextrin, starch, lactose, lactose monohydrate, and sucrose. The lubricants are selected from one or more of magnesium stearate, talc, colloidal silicon dioxide, and polyvinyl alcohol.

[0022] More preferably, and as an example of the present invention, in step S2, the excipients include fillers and lubricants. The filler is starch, and the lubricant is magnesium stearate.

[0023] Preferably, in step S2, the granulation is carried out using an aqueous ethanol solution of 90%-99%.

[0024] More preferably, and as an example of the present invention, in step S2, the granulation is carried out using an aqueous ethanol solution of 95%.

[0025] Preferably, the mass ratio of Angelica sinensis, Atractylodes macrocephala, and Mentha haplocalyx in step S1 to Paeonia lactiflora, Poria cocos, Carthamus tinctorius, Gleditsia sinensis, Bupleurum chinense, and Glycyrrhiza uralensis in step S2 is 20-32:20-32:2-6:20-32:20-32:3-7:6-10:20-32:15-24.

[0026] More preferably, and as an example of the present invention, the mass ratio of Angelica sinensis, Atractylodes macrocephala, and Mentha haplocalyx in step S1 to Paeonia lactiflora, Poria cocos, Carthamus tinctorius, Gleditsia sinensis, Bupleurum chinense, and Glycyrrhiza uralensis in step S2 is 26:26:4:26:26:5:8:26:19.5.

[0027] On the other hand, the present invention provides a Safflower Xiaoyao Tablet produced by the production process described in the above claims.

[0028] On yet another aspect, the present invention provides the application of the above production process in the production of Safflower Xiaoyao Tablets.

[0029] Compared with the prior art, the present invention has the following beneficial effects:

[0030] Based on the existing production process of Honghua Xiaoyao Tablets, through the process improvement of the filtration and concentration steps, on the premise that there is no obvious difference in the product quality provided by the existing process, the filtration effect is effectively improved, and the energy consumption and cost of the entire production process of Honghua Xiaoyao Tablets are reduced. Detailed implementation manners

[0031] Terms and declarations of the present invention:

[0032] 1. Articles "a", "an" and "the": Include plural objects unless otherwise explicitly limited to one (kind) of object.

[0033] 2. Numerical ranges: Unless otherwise explicitly indicated, all ranges or ratios disclosed herein will be understood to include any and all sub-ranges or sub-ratios contained therein. For example, the stated range or ratio of 1 to 30 should be considered to include between the minimum value of 1 and the maximum value of 30, and any sub-range or sub-ratio, integer, decimal, or sub-range or sub-ratio composed of integers or decimals including the endpoints.

[0034] The following non-limiting examples can enable those of ordinary skill in the art to more comprehensively understand the present invention, but do not limit the present invention in any way. The following content is merely an exemplary illustration of the scope claimed by the present invention. Those skilled in the art can make various changes and modifications to the invention of the present invention based on the disclosed content, and it should also fall within the scope claimed by the present invention.

[0035] The present invention will be further described below by way of specific examples. All chemical reagents used in the examples of the present invention are obtained through conventional commercial channels unless otherwise specified. Unless otherwise specified, the contents described below are mass contents. Unless otherwise specified, it is understood to be carried out at room temperature.

[0036] Example 1

[0037] An optimized production process of Honghua Xiaoyao Tablets.

[0038] 260 parts by mass of Angelica sinensis, 260 parts by mass of Paeonia lactiflora, 260 parts by mass of Atractylodes macrocephala, 260 parts by mass of Poria cocos, 50 parts by mass of Carthamus tinctorius, 80 parts by mass of Gleditsia sinensis spine, 260 parts by mass of Bupleurum chinense DC. var. glabrum, 40 parts by mass of Mentha haplocalyx Briq., 195 parts by mass of Glycyrrhiza uralensis Fisch. For the above nine herbs, except for Angelica sinensis, Atractylodes macrocephala, and Mentha haplocalyx Briq., the volatile oil is extracted by steam distillation, and the volatile oil is reserved. The medicinal residues and the other six herbs such as Paeonia lactiflora are decocted with water twice, each time for 2 hours. Filter in batches: first filter through a double filter with a 100-mesh sieve of Φ230×750 DN50, and then filter through a ceramic membrane filter of JSMST-MF100-23-2 with a flow rate of 2000 kg / h (ceramic membrane with a pore size of 100 nm). Combine the filtrates and concentrate to a thick paste with a relative density of 1.37 - 1.43 (50 °C). The specific concentration process is to concentrate with a JSMST-RO-8040-12 reverse osmosis organic membrane concentrator at a flow rate of 2000 kg / h to 10% of the original volume, and then concentrate with an EJZN-2500 double-effect energy-saving concentrator at a flow rate of 2500 kg / h.

[0039] Dry, pulverize, add appropriate amounts of starch and magnesium stearate, mix evenly, make granules with 95% ethanol, spray in the above-mentioned volatile oil, seal for 12 hours, press tablets (when each 1 part by mass is 1 g, 1000 tablets can be pressed), and coat with a film coating to obtain the product.

[0040] Example 2

[0041] Compared with Example 1, the 100-nm ceramic membrane is changed to a 5-nm ceramic membrane, and the rest are the same.

[0042] Example 3

[0043] Compared with Example 1, the 100-nm ceramic membrane is changed to a 15-nm ceramic membrane, and the rest are the same.

[0044] Example 4

[0045] Compared with Example 1, the 100-nm ceramic membrane is changed to a 200-nm ceramic membrane, and the rest are the same.

[0046] Example 5

[0047] Compared with Example 1, the reverse osmosis organic membrane is changed to a nanofiltration organic membrane, and the rest are the same.

[0048] Example 6

[0049] Compared with Example 1, the organic membrane is concentrated to 30% of the original volume, and the rest are the same.

[0050] Example 7

[0051] Compared with Example 1, the organic membrane is concentrated to 5% of the original volume, and the rest are the same.

[0052] Comparative Example 1

[0053] A production process of Honghua Xiaoyao Tablets. Compared with Example 1, ceramic membrane filtration and membrane concentration are omitted, and the rest are the same.

[0054] 260 parts by mass of Angelica sinensis, 260 parts by mass of Paeonia lactiflora, 260 parts by mass of Atractylodes macrocephala, 260 parts by mass of Poria cocos, 50 parts by mass of Carthamus tinctorius, 80 parts by mass of Gleditsia sinensis spine, 260 parts by mass of Bupleurum chinense var. glabrum, 40 parts by mass of Mentha haplocalyx, 195 parts by mass of Glycyrrhiza uralensis. For the above nine herbs, except for Angelica sinensis, Atractylodes macrocephala, and Mentha haplocalyx, volatile oils are extracted by steam distillation, and the volatile oils are reserved. The medicinal residues and the other six herbs such as Paeonia lactiflora are decocted with water twice, each time for 2 hours.

[0055] Filter through a double - layer filter with a 100 - mesh sieve of Φ230×750 DN50. Combine the filtrates and concentrate to a thick paste with a relative density of 1.37 - 1.43 (50 °C). The concentration process is carried out with an EJZN - 2500 double - effect energy - saving concentrator at 2500 kg / h.

[0056] Dry, pulverize, add appropriate amounts of starch and magnesium stearate, mix evenly, make into granules with 95% ethanol, spray in the above - mentioned volatile oils, seal for 12 hours, press tablets (when each 1 part by mass is 1 g, 1000 tablets can be pressed), and coat with a film - coating to obtain the product.

[0057] Comparative Example 2

[0058] Prepare Honghua Xiaoyao Tablets by referring to the preparation method provided in Example 1 of Patent CN117045711A.

[0059] Comparative Example 3

[0060] A production process of Honghua Xiaoyao Tablets. Compared with Example 1, membrane concentration is omitted, and the rest are the same.

[0061] 260 parts by mass of Angelica sinensis, 260 parts by mass of Paeonia lactiflora, 260 parts by mass of Atractylodes macrocephala, 260 parts by mass of Poria cocos, 50 parts by mass of Carthamus tinctorius, 80 parts by mass of Gleditsia sinensis spine, 260 parts by mass of Bupleurum chinense var. glabrum, 40 parts by mass of Mentha haplocalyx, 195 parts by mass of Glycyrrhiza uralensis. For the above nine herbs, except for Angelica sinensis, Atractylodes macrocephala, and Mentha haplocalyx, volatile oils are extracted by steam distillation, and the volatile oils are reserved. The medicinal residues and the other six herbs such as Paeonia lactiflora are decocted with water twice, each time for 2 hours. Filter in batches: first filter through a double - layer filter with a 100 - mesh sieve of Φ230×750 DN50, and then filter through a ceramic membrane filter of JSMST - MF100 - 23 - 2 (100 nm pore - size ceramic membrane) at 2000 kg / h. Combine the filtrates and concentrate to a thick paste with a relative density of 1.37 - 1.43 (50 °C). The specific concentration process is carried out with an EJZN - 2500 double - effect energy - saving concentrator at 2500 kg / h.

[0062] Dry, pulverize, add appropriate amounts of starch and magnesium stearate, mix well, make granules with 95% ethanol, spray in the above volatile oil, seal for 12 hours, tableting (when each 1 part by mass is 1 g, 1000 tablets can be made), coat with film coating, and obtain the product.

[0063] Comparative Example 4

[0064] A production process of Honghua Xiaoyao tablets. Compared with Example 1, vacuum concentration is omitted, and the rest are the same.

[0065] 260 parts by mass of Angelica sinensis, 260 parts by mass of Paeonia lactiflora, 260 parts by mass of Atractylodes macrocephala, 260 parts by mass of Poria cocos, 50 parts by mass of Carthamus tinctorius, 80 parts by mass of Gleditsia sinensis thorn, 260 parts by mass of Bupleurum chinense DC. var. glabrum, 40 parts by mass of Mentha haplocalyx Briq., 195 parts by mass of Glycyrrhiza uralensis Fisch. For the above nine herbs, except for Angelica sinensis, Atractylodes macrocephala, and Mentha haplocalyx Briq., steam distillation is used to extract the volatile oil, and the volatile oil is reserved. The medicinal residues and the other six herbs including Paeonia lactiflora are decocted with water twice, each time for 2 hours. Filter in batches: first filter through a double filter with a 100-mesh sieve of Φ230×750 DN50, and then filter through a ceramic membrane filter of JSMST-MF100-23-2 (ceramic membrane with a pore size of 100 nm) at 2000 kg / h. Combine the filtrates and concentrate to a thick paste with a relative density of 1.37 - 1.43 (50 °C). The specific concentration process is carried out with a JSMST-RO-8040-12 reverse osmosis organic membrane concentrator at 2000 kg / h.

[0066] Dry, pulverize, add appropriate amounts of starch and magnesium stearate, mix well, make granules with 95% ethanol, spray in the above volatile oil, seal for 12 hours, tableting (when each 1 part by mass is 1 g, 1000 tablets can be made), coat with film coating, and obtain the product.

[0067] Comparative Example 5

[0068] A production process of Honghua Xiaoyao tablets. Compared with Example 1, ceramic membrane filtration is omitted, and the rest are the same.

[0069] 260 parts by mass of Angelica sinensis, 260 parts by mass of Paeonia lactiflora, 260 parts by mass of Atractylodes macrocephala, 260 parts by mass of Poria cocos, 50 parts by mass of Carthamus tinctorius, 80 parts by mass of Gleditsia sinensis spine, 260 parts by mass of Bupleurum chinense DC. var. glabrum, 40 parts by mass of Mentha haplocalyx Briq., 195 parts by mass of Glycyrrhiza uralensis Fisch. For the above nine herbs, except for Angelica sinensis, Atractylodes macrocephala, and Mentha haplocalyx Briq. which are subjected to steam distillation to extract volatile oils and the volatile oils are reserved, the medicinal residues and the other six herbs such as Paeonia lactiflora are decocted with water twice, each time for 2 hours. Filter through a double - layer filter with a 100 - mesh sieve of Φ230×750 DN50. Combine the filtrates and concentrate to a thick paste with a relative density of 1.37 - 1.43 (50 °C). The specific concentration process is to concentrate with a JSMST - RO - 8040 - 12 reverse osmosis organic membrane concentrator at 2000 kg / h to 10% of the original volume, and then concentrate with an EJZN - 2500 double - effect energy - saving concentrator at 2500 kg / h.

[0070] Dry, pulverize, add appropriate amounts of starch and magnesium stearate, mix evenly, make granules with 95% ethanol, spray in the above - mentioned volatile oils, seal for 12 hours, press tablets (when each 1 part by mass is 1 g, 1000 tablets can be pressed), and coat with a film - coating to obtain the product.

[0071] Comparative Example 6

[0072] A production process of Honghua Xiaoyao tablets. Compared with Example 1, sieve filtration is omitted, and the rest are the same.

[0073] 260 parts by mass of Angelica sinensis, 260 parts by mass of Paeonia lactiflora, 260 parts by mass of Atractylodes macrocephala, 260 parts by mass of Poria cocos, 50 parts by mass of Carthamus tinctorius, 80 parts by mass of Gleditsia sinensis spine, 260 parts by mass of Bupleurum chinense DC. var. glabrum, 40 parts by mass of Mentha haplocalyx Briq., 195 parts by mass of Glycyrrhiza uralensis Fisch. For the above nine herbs, except for Angelica sinensis, Atractylodes macrocephala, and Mentha haplocalyx Briq. which are subjected to steam distillation to extract volatile oils and the volatile oils are reserved, the medicinal residues and the other six herbs such as Paeonia lactiflora are decocted with water twice, each time for 2 hours. Filter through a ceramic membrane filter of JSMST - MF100 - 23 - 2 with a pore size of 100 nm ceramic membrane at 2000 kg / h. Combine the filtrates and concentrate to a thick paste with a relative density of 1.37 - 1.43 (50 °C). The specific concentration process is to concentrate with a JSMST - RO - 8040 - 12 reverse osmosis organic membrane concentrator at 2000 kg / h to 10% of the original volume, and then concentrate with an EJZN - 2500 double - effect energy - saving concentrator at 2500 kg / h.

[0074] Dry, pulverize, add appropriate amounts of starch and magnesium stearate, mix evenly, make granules with 95% ethanol, spray in the above - mentioned volatile oils, seal for 12 hours, press tablets (when each 1 part by mass is 1 g, 1000 tablets can be pressed), and coat with a film - coating to obtain the product.

[0075] In Examples 1 - 7 and Comparative Examples 1 - 6, the material of the ceramic membrane filter used is alumina, and the material of the organic membrane concentrator used is polyamide.

[0076] Comparative Example 7

[0077] A production process of Honghua Xiaoyao tablets. It is the same as that of Example 1 except that the ceramic membrane is changed to a ceramic membrane made of silicon carbide.

[0078] Comparative Example 8

[0079] A production process of Honghua Xiaoyao tablets. Compared with Example 1, the organic membrane is changed to an organic membrane made of polyvinylidene fluoride, and the rest are the same.

[0080] Effect Example 1

[0081] Energy consumption cost accounting

[0082] Using the production methods of Examples 1 - 7 and Comparative Examples 1 - 8 to produce the same amount (10 kg) of Honghua Xiaoyao tablets, the energy consumption cost and ratio are shown in Table 1.

[0083] Table 1

[0084]

[0085] It can be seen that for the Honghua Xiaoyao tablets of the same weight obtained by the production methods of each example, their energy consumption cost is less than that of the Honghua Xiaoyao tablets obtained by the production methods provided in each comparative example. It should be noted that in Comparative Example 5, concentration was carried out by the method of organic membrane concentration plus decompression concentration, but ceramic membrane filtration was not used. Since organic membrane concentration requires the turbidity of the liquid to be concentrated to be low within a certain range, and when ceramic membrane filtration is not used, the turbidity of the liquid to be concentrated cannot meet the requirements of organic membrane concentration, and the organic membrane concentration process cannot proceed normally, and the process cannot continue continuously.

[0086] Effect Example 2

[0087] Characterization method of Honghua Xiaoyao tablets.

[0088] 1. Determination of multi - component content.

[0089] 1.1. Determination conditions and analysis methods

[0090] Chromatographic conditions and system suitability: Using octadecylsilane - bonded silica gel as the filler; using acetonitrile as mobile phase A and 0.1% phosphoric acid as mobile phase B, gradient elution was carried out according to the regulations in Table 2; the detection wavelength was 230 nm; the flow rate was 1.0 mL / min, and the column temperature was 30 °C.

[0091] Table 2

[0092] Time (min) Mobile phase A (%) Mobile phase B (%) 0 15 85 15 14 86 20 17 83 25 35 65 45 50 50 50 15 85 53 15 85

[0093] Preparation of reference substance solution: Weigh appropriate amounts of albiflorin lactone, albiflorin, and ammonium glycyrrhizinate reference substances accurately, dissolve them in methanol to prepare a mixed solution containing 50 μg of albiflorin lactone, albiflorin, and ammonium glycyrrhizinate in each 1 mL, and you will get it.

[0094] Preparation of test solution: Take 20 tablets of this product, remove the film coating, grind them finely, accurately weigh 0.25 g of the powder of this product and place it in a stoppered conical flask, add 30 mL of ether, ultrasonicate (90 W, 59 KHz) for 5 minutes, filter, dry the residue of the drug and the filter paper to remove the solvent, place it in a stoppered conical flask, accurately add 25 mL of methanol, stopper tightly, weigh, ultrasonicate (90 W, 59 KHz) for 25 minutes, let it cool, weigh again, make up the lost weight with methanol, shake well, and take the subsequent filtrate, and you will get it.

[0095] Determination method: Accurately pipette 10 μL of the reference substance solution and the test solution respectively, inject them into the liquid chromatograph for determination, and you will get it.

[0096] Using the above method, detect the concentrations of albiflorin lactone, albiflorin, and ammonium glycyrrhizinate in the Safflower Xiaoyao Tablets prepared in Examples 1 - 7 and Comparative Examples 1 - 8, and repeat the measurement 5 times and take the average value. The results are shown in Table 3.

[0097] Table 3

[0098]

[0099]

[0100] The contents of albiflorin lactone, albiflorin, and ammonium glycyrrhizinate in the Safflower Xiaoyao Tablets produced by the production processes provided in Examples 1 - 7 are in the ranges of 4.00 - 4.12 mg / g, 6.33 - 6.80 mg / g, and 5.35 - 5.69 mg / g, respectively. It should be particularly noted that, compared with each of the examples, Comparative Example 1 did not adopt ceramic membrane filtration and membrane concentration, and the contents of albiflorin lactone, albiflorin, and ammonium glycyrrhizinate in the Safflower Xiaoyao Tablets produced thereby were 4.03 mg / g, 6.58 mg / g, and 5.47 mg / g, respectively, with levels comparable to those of each of the examples. However, since the production energy consumption cost of Comparative Example 1 was significantly higher than that of each of the examples, each of the examples had obvious technological progress compared with Comparative Example 1. Comparative Example 2 prepared Safflower Xiaoyao Tablets using the prior art. The contents of albiflorin lactone, albiflorin, and ammonium glycyrrhizinate in the Safflower Xiaoyao Tablets produced in Comparative Example 2 were 4.23 mg / g, 6.85 mg / g, and 5.62 mg / g, respectively. The contents of albiflorin lactone and albiflorin were slightly higher than those of each of the examples, and the content level of ammonium glycyrrhizinate was comparable to that of each of the examples. However, the relative value of the production energy consumption cost of Comparative Example 2 was 1.58, while the relative values of the energy consumption costs of Examples 1 - 7 were 0.57 - 0.77. It can be calculated that the energy consumption cost of Comparative Example 2 was 2.05 - 2.77 times that of Examples 1 - 7, and the reduction amplitude of its energy consumption was significantly higher than the increase amplitude of the contents of albiflorin lactone and albiflorin in the Safflower Xiaoyao Tablets prepared in Comparative Example 2. It can be seen that each of the examples had obvious technological progress compared with Comparative Example 2.

[0101] In summary, combining the energy consumption cost and the determination results of multiple component contents, the preparation processes provided in each of the examples of the present invention can significantly reduce the production energy consumption cost by improving the filtration and concentration process steps on the basis of maintaining the contents of albiflorin lactone, albiflorin, and ammonium glycyrrhizinate within a certain range, thereby substantially reducing the process cost as a whole.

[0102] Finally, it should be noted that the above content is only used to illustrate the technical solution of the present invention, rather than to limit the protection scope of the present invention. Any simple modification or equivalent replacement made by those of ordinary skill in the art to the technical solution of the present invention shall not depart from the essence and scope of the technical solution of the present invention.

Claims

1. A production process of Honghua Xiaoyao Tablets, characterized in that: The following steps are involved: S1. Extracting volatile oil from angelica, atractylodes macrocephala and mint to obtain a volatile oil mixture and medicinal residues; S2, mixing the residue obtained in step S1 with white peony root, Poria cocos, safflower, Gleditsia sinensis, Bupleurum chinense and Licorice, boiling with water, filtering and concentrating the filtrate to obtain a thick paste; S3, drying and crushing the thick paste obtained in step S2, mixing with auxiliary materials, granulating, mixing with the volatile oil mixture obtained in step S1, sealing, tableting, coating, and obtaining Honghua Xiaoyao Tablets; Wherein, in step S2, the filtration includes screen filtration and ceramic membrane filtration, and the concentrated filtrate includes membrane concentration and reduced pressure concentration. In step S2, the ceramic membrane filtration uses a ceramic membrane filter with a pore size of 5-200nm, and the membrane concentration uses a reverse osmosis organic membrane concentrator or a nanofiltration organic membrane concentrator.

2. The production process according to claim 1, characterized in that: In step S2, the ceramic membrane filtration uses a ceramic membrane filter with a pore size of 100 nm, and the membrane concentration uses a reverse osmosis organic membrane concentrator.

3. The production process according to claim 1, characterized in that: In step S2, the concentrated filtrate comprises the following steps: the filtrate is concentrated to 5%-30% of the original volume through a membrane, and then concentrated under reduced pressure at 75-85°C to a relative density of 1.37-1.

43.

4. The production process according to claim 3, characterized in that: In step S2, the filtrate is concentrated to 10%-30% of the original volume through a membrane, and then concentrated under reduced pressure at 80°C to a relative density of 1.37-1.

43.

5. The production process according to claim 1, characterized in that: In step S2, the auxiliary materials include fillers and lubricants, the fillers are selected from one or more of dextrin, starch, lactose, lactose monohydrate and sucrose, and the lubricants are selected from one or more of magnesium stearate, talc, micro-powdered silica gel and polyvinyl alcohol.

6. The production process according to claim 1, characterized in that: In step S2, the granulation is performed using a 90%-99% ethanol aqueous solution.

7. The production process according to claim 1, characterized in that: The mass ratio of the angelica, atractylodes, and mint in step S1 to the white peony root, Poria, safflower, Gleditsia sinensis, Bupleurum chinense, and Licorice in step S2 is 20-32:20-32:2-6:20-32:20-32:3-7:6-10:20-32:15-24.

8. The production process according to claim 7, characterized in that: The mass ratio of the angelica, atractylodes, and mint in step S1 to the white peony root, Poria, safflower, Gleditsia sinensis, Bupleurum chinense, and Licorice in step S2 is 26:26:4:26:26:5:8:26:19.

5.

9. A safflower Xiaoyao tablet, characterized in that: The product is produced by the production process described in any one of claims 1 to 8.

10. Use of the production process described in any one of claims 1 to 8 in the production of Honghua Xiaoyao Tablets.

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