Preparation method of traditional Chinese medicinal liquor

Abstract

The preparation method comprises the following steps: (1) soaking male silkworm moths in white spirit, extracting, and filtering to obtain a male silkworm moth extracting solution; (2) performing percolation extraction on herba epimedii, semen cuscutae, fructus lycii, cordyceps sinensis, herba cistanche, rhodiola rosea, radix astragali, radix rehmanniae praeparata and stigma croci with white spirit to obtain percolate; (3) combining the male silkworm moth extracting solution and the percolating solution to obtain a medicine extracting solution; and (4) filtering the medicine extracting solution by using a 0.22-1 mu m polypropylene filter membrane, standing for 30-60 days, then filtering by using a 0.22-1 mu m polyethersulfone filter membrane, mixing with rock candy liquid, adjusting the alcohol content to (39 + / -2) degrees, and filtering by using a 0.22-1 mu m polyethersulfone filter membrane to obtain the traditional Chinese medicine wine. The medicinal liquor prepared by the preparation method disclosed by the invention is high in stability, and the problem that precipitates are generated by an original production process is effectively solved.

Description

Technical Field

[0001] The present invention relates to a preparation method of a traditional Chinese medicine medicated wine, belonging to the field of traditional Chinese medicine. Background Art

[0002] Tongmai Qiangshen Wine is a marketed traditional Chinese medicine medicated wine exclusively produced by the applicant, which has the effects of tonifying the kidney and replenishing essence, activating blood circulation and dredging meridians, and is applicable to symptoms such as soreness and weakness of the waist and knees, fear of cold and cold limbs, dizziness and tinnitus, listlessness, and frequent nocturia caused by kidney deficiency. The effects are remarkable and it is deeply welcomed by consumers. The raw materials of Tongmai Qiangshen Wine are male silkworm moths, epimedium, dodder seeds, wolfberries, cordyceps sinensis, cistanche deserticola, rhodiola rosea, astragalus membranaceus, prepared rehmannia root, and saffron crocus. The original production process is as follows: Soak male silkworm moths in 50-degree liquor at 1-5 times the amount for more than 10 days, filter, soak the medicinal residues in an appropriate amount of 50-degree liquor for 2 days, filter, combine the two filtrates, and store them separately for later use; separately take the other nine flavors such as epimedium, crush them into coarse particles, soak them in 50-degree liquor for more than 2 days, percolate, collect the percolate, combine it with the above-mentioned male silkworm moth extract, add rock sugar solution (prepared by dissolving rock sugar in 2-4 times the amount of water), mix, adjust the alcohol content to (39±2) degrees, stand still, filter, and package to obtain the product.

[0003] For the medicated wine produced by the above process, a small amount of precipitate will appear after a period of time. Although it does not affect the efficacy of the medicated wine, it gives consumers an unpleasant visual experience, thereby triggering consumers' doubts about the product quality. There are many possible reasons for the precipitation problem, such as storage temperature, chemical component stability under the concentration of the medicated wine, and possible chemical reactions. Since the raw materials of this medicated wine contain multiple drugs with different physical and chemical properties at the same time, especially the male silkworm moth belongs to animal medicinal materials, which are covered with hair and scales all over the body and contain animal-derived components such as proteins and fatty acids, and the final solvent of the product is high-concentration liquor, the raw materials and process make it prone to precipitation. This medicated wine is an exclusive product, and there has been no research data on solving the precipitation problem of this medicated wine in the past. Since the raw materials and processes of other medicated wines are completely different from this medicated wine, it is difficult to obtain valuable reference information.

[0004] Therefore, it is necessary to improve the production process for the quality stability of this product, especially the precipitation problem. Summary of the Invention

[0005] In view of this, the purpose of the present invention is to provide an improved preparation method of the traditional Chinese medicine medicated wine Tongmai Qiangshen Wine to solve the precipitation problem of Tongmai Qiangshen Wine.

[0006] The present invention provides a preparation method of the traditional Chinese medicine medicated wine Tongmai Qiangshen Wine, which comprises the following steps:

[0007] (1) Soak and extract male silkworm moths with liquor, filter to obtain a male silkworm moth extract;

[0008] (2)Take epimedium, dodder seeds, wolfberries, cordyceps sinensis, cistanche, rhodiola rosea, astragalus membranaceus, prepared rehmannia root, and saffron crocus, and percolate and extract them with white liquor to obtain a percolate.

[0009] (3)Combine the male silkworm moth extract and the percolate to obtain a drug extract.

[0010] (4)Filter the drug extract through a 0.22 - 1 μm polypropylene filter membrane to obtain a first filtrate; let the first filtrate stand for 30 - 60 days, then filter it through a 0.22 - 1 μm polyethersulfone filter membrane to obtain a second filtrate; mix the second filtrate with rock sugar solution, adjust the alcohol content to (39 ± 2) degrees to obtain a blending liquid; filter the blending liquid through a 0.22 - 1 μm polyethersulfone filter membrane to obtain the traditional Chinese medicine medicated wine.

[0011] In the present invention, preferably, in step (1), the filtration is carried out using an 80 - 120 mesh stainless steel filter net.

[0012] In the present invention, preferably, in step (1), the number of times of soaking and extraction is 2 times. For the first time, soak and extract male silkworm moths with white liquor for 10 - 60 days, and then filter; add the filter residue to white liquor again for the second soaking and extraction for 1 - 7 days, and then filter; combine the filtrates to obtain a male silkworm moth extract.

[0013] In the present invention, preferably, in step (1), the concentration of the white liquor is 40 - 60 degrees by volume ratio.

[0014] In the present invention, preferably, in step (2), take epimedium, dodder seeds, wolfberries, cordyceps sinensis, cistanche, rhodiola rosea, astragalus membranaceus, prepared rehmannia root, and saffron crocus, first soak them in white liquor for 1 - 3 days, and then carry out percolation extraction.

[0015] In the present invention, preferably, in step (4), the standing time of the first filtrate is 35 - 50 days.

[0016] In the present invention, preferably, in step (4), the standing time of the first filtrate is 40 - 45 days.

[0017] In the present invention, preferably, in step (4), the pore size of the polypropylene filter membrane is 0.45 μm, and the pore size of the polyethersulfone filter membrane is 0.45 μm.

[0018] In the present invention, preferably, in step (4), the polypropylene filter membrane is placed in a plate - type filter or a pipeline filter, and the polyethersulfone filter membrane is placed in a plate - type filter or a pipeline filter.

[0019] In the present invention, preferably, in step (4), the rock sugar solution is prepared by mixing rock sugar and water at a weight ratio of 1:2 and filtering, and the filtering method is selected from suction filtration, ultrafiltration or microfiltration.

[0020] The traditional Chinese medicine medicated wine Tongmai Qiangshen Wine produced by the production process of the present invention has been subjected to a long-term storage stability experiment, and its quality is stable within the shelf life, and no precipitation phenomenon has occurred. Detailed implementation manners

[0021] The present invention will be further described in detail below.

[0022] Regarding the precipitation problem of the traditional Chinese medicine medicated wine Tongmai Qiangshen Wine, the inventor has carried out a detailed analysis on the physical and chemical properties of the intermediate products in each production link of the original production process and their changes over time, confirmed the key steps leading to precipitation in the original production process, and made targeted improvements to these steps. Finally, a production process for solving the precipitation problem has been determined, so that the product will no longer produce precipitation within the shelf life, and at the same time, the content of the active ingredients in the medicated wine will not decrease within the shelf life, thereby improving the appearance of the traditional Chinese medicine medicated wine without affecting the curative effect.

[0023] The production process of the Tongmai Qiangshen Wine of the present invention comprises the following steps:

[0024] (1) Soaking and extracting male silkworm moths with white liquor, and filtering to obtain a male silkworm moth extract;

[0025] (2) Taking epimedium, dodder seeds, wolfberries, cordyceps sinensis, cistanche deserticola, rhodiola rosea, astragalus membranaceus, prepared rehmannia root and saffron crocus, and percolating and extracting with white liquor to obtain a percolate;

[0026] (3) Combining the male silkworm moth extract and the percolate to obtain a medicament extract;

[0027] (4) Filtering the medicament extract with a 0.22 - 1 μm polypropylene filter membrane to obtain a first filtrate; standing the first filtrate for 30 - 60 days, then filtering with a 0.22 - 1 μm polyethersulfone filter membrane to obtain a second filtrate; mixing the second filtrate with the rock sugar solution, adjusting the alcohol content to (39 ± 2) degrees to obtain a blending liquid; filtering the blending liquid with a 0.22 - 1 μm polyethersulfone filter membrane to obtain the Tongmai Qiangshen Wine.

[0028] In the present invention, the raw materials of the medicated wine remain unchanged, and the composition of each raw material by weight parts is: 1500 - 2500 parts of male silkworm moths, 250 - 350 parts of epimedium, 200 - 300 parts of dodder seeds, 120 - 180 parts of wolfberries, 3 - 8 parts of cordyceps sinensis, 30 - 80 parts of cistanche deserticola, 3 - 8 parts of rhodiola rosea, 120 - 180 parts of astragalus membranaceus, 70 - 130 parts of prepared rehmannia root, 1 - 5 parts of saffron crocus.

[0029] In the present invention, preferably, the raw materials are composed by weight parts as follows: 1800 - 2200 parts of male silkworm moths, 280 - 320 parts of epimedium, 230 - 270 parts of dodder seeds, 140 - 160 parts of wolfberries, 5 - 7 parts of cordyceps sinensis, 40 - 60 parts of cistanche deserticola, 5 - 7 parts of rhodiola rosea, 140 - 160 parts of astragalus membranaceus, 90 - 110 parts of prepared rehmannia root, and 2 - 4 parts of saffron crocus.

[0030] According to a preferred embodiment of the present invention, the raw materials are composed by weight parts as follows: 2000 parts of male silkworm moths, 300 parts of epimedium, 250 parts of dodder seeds, 150 parts of wolfberries, 6 parts of cordyceps sinensis, 50 parts of cistanche deserticola, 6 parts of rhodiola rosea, 150 parts of astragalus membranaceus, 100 parts of prepared rehmannia root, and 3 parts of saffron crocus.

[0031] <Male silkworm moth extraction step>

[0032] In the present invention, in step (1), the male silkworm moths are soaked and extracted with white liquor, and then filtered to obtain the male silkworm moth extract.

[0033] According to a preferred embodiment of the present invention, the filtration is carried out using a stainless steel filter screen with 80 - 120 meshes.

[0034] In the present invention, the concentration of the white liquor is 40 - 60 degrees by volume ratio, preferably 45 - 55 degrees, and most preferably 50 degrees. The degree of the white liquor is the percentage by volume ratio. The white liquor can also be replaced by edible ethanol with a comparable concentration.

[0035] According to a preferred embodiment of the present invention, the number of times of the soaking extraction is 2 times. For the first time, the male silkworm moths are soaked and extracted with white liquor for 10 - 60 days, and then filtered; the filter residue is added with white liquor again for the second soaking extraction for 1 - 7 days, and then filtered; the filtrates are combined to obtain the male silkworm moth extract. In the present invention, for the first soaking extraction, the mass ratio of the white liquor to the male silkworm moths is 1 - 3:1, preferably 1 - 2:1, and more preferably 1.5:1. For the second soaking extraction, the mass ratio of the white liquor to the male silkworm moths is 0.3 - 3:1, preferably 0.5 - 2:1, and more preferably 0.5:1.

[0036] According to a preferred embodiment of the present invention, the soaking extraction time for the first time of the male silkworm moths is 10 - 30 days, more preferably 10 - 15 days; the soaking extraction time for the second time is 1 - 5 days, more preferably 1 - 3 days.

[0037] After the male silkworm moths are soaked in white liquor, the insect bodies become soft and rotten. After the soluble substances are dissolved out, it is difficult to filter. In addition, there are a large number of scale fragments of male silkworm moths in the leaching solution, and they are very likely to enter the filtrate after filtration.

[0038] Previously, gauze filtration, pressure filtration or suction filtration were used in the process. These filtration methods can filter out insect bodies and lepidopteran fragments, especially effectively filter out fine lepidopterans. However, they are extremely prone to clogging and require frequent replacement of the filter medium. Research has found that this filtration process has little impact on the precipitation of the finished medicinal liquor, but the overall efficiency is low.

[0039] In response to this, through various filtration process experiments, the inventor unexpectedly found that using a stainless steel filter mesh can achieve the effect of effectively and efficiently filtering out male silkworm moth bodies and lepidopteran fragments. Since the lepidopteran fragments are very small, it is generally believed that a low-mesh stainless steel filter mesh is difficult to effectively filter them out, and a high-mesh filter mesh will also become clogged and has a higher replacement cost. To ensure the filtration effect and control costs, the original process did not consider using a stainless steel filter mesh for filtration. The present invention discovers that a stainless steel filter mesh with an appropriate mesh number can not only filter out large-volume insect bodies, but also has an ideal effect of filtering out lepidopteran fragments at the same time. Meanwhile, the filtration time is shortened, the filtration efficiency is greatly improved, and a large amount of filter materials are saved.

[0040] According to a preferred embodiment of the present invention, a stainless steel filter mesh is used, and the mesh number of the stainless steel filter mesh is 80 - 120 meshes, preferably 80 - 100 meshes, and more preferably 80 meshes. The present invention discovers that when using a stainless steel filter mesh with the above-mentioned mesh number, a large number of lepidopteran fragments in the leaching solution adhere to the filter mesh and form a three-dimensional network structure in an interlaced manner, playing a role of rough filtration. This not only improves the filtration effect, but also avoids the clogging of the filter mesh by insect bodies and other large-volume filter residues, and the obtained filtrate has a high clarity. A stainless steel filter mesh with less than 80 meshes is difficult to effectively filter out lepidopteran fragments, and even a small amount of fine insect bodies will leak through. While a stainless steel filter mesh with more than 120 meshes is prone to clogging and has a low filtration efficiency. When the mesh number of the stainless steel filter mesh is 80 meshes, the filtration effect is the best.

[0041] <Other steps for extracting medicinal materials>

[0042] In the present invention, in step (2), epimedium, dodder, wolfberry fruit, cordyceps sinensis, cistanche deserticola, rhodiola rosea, astragalus membranaceus, rehmannia glutinosa, and crocus sativus are taken and percolated with white liquor to obtain a percolate.

[0043] The concentration of the white liquor is the same as described above.

[0044] The present invention discovers that this step does not have a significant impact on the final precipitation of the medicinal liquor. Therefore, the original percolation process is still retained, that is, first, the above nine medicinal materials except male silkworm moth are soaked in white liquor for 12 - 72 hours, preferably 12 - 54 hours, and more preferably 24 - 48 hours. According to a preferred embodiment of the present invention, the soaking time is 48 hours. After the nine medicinal materials are soaked, percolation is carried out, and the weight of the collected percolate is 3 - 6 times, more preferably 4 - 5 times, the total weight of the nine medicinal materials.

[0045] <Mixing step>

[0046] Mix the male silkworm moth extract obtained in step (1) and the percolate obtained in step (2) evenly to obtain a drug extract.

[0047] <Filtration step>

[0048] In the present invention, the filtration method is as follows: first filter the drug extract obtained in step (3) with a 0.22 - 1 μm polypropylene filter membrane to obtain a first filtrate; let the first filtrate stand for 30 - 60 days, and then filter it with a 0.22 - 1 μm polyethersulfone filter membrane to obtain a second filtrate; mix the second filtrate with rock sugar solution, adjust the ethanol content to (39 ± 2) degrees to obtain a blending solution, and filter the blending solution with a 0.22 - 1 μm polyethersulfone filter membrane to obtain the traditional Chinese medicine medicinal liquor Tongmai Qiangshen Wine.

[0049] The present invention discovers that the filtration step of the drug extract obtained in step (3) is the decisive factor for the precipitation of the medicinal liquor. After the male silkworm moth extract is mixed with the percolates of the other nine medicinal materials, tiny particles that cannot stably dissolve in the white liquor of the said concentration will be produced. After passing through the original filtration process, some of these tiny particles still enter the finished medicinal liquor. These tiny particles have little impact on the clarity of the medicinal liquor in a short time, but as time goes by, with these original particles as the core, they gradually aggregate and precipitate visible particles, resulting in the visible precipitation in the medicinal liquor. Therefore, the inventor believes that fully filtering out the tiny particles in the mixed drug extract can significantly reduce or even avoid the generation of precipitation.

[0050] Therefore, the inventor has conducted research on various different filtration methods for the said drug extract in order to effectively remove the tiny particles therein, and verified the effects of various filtration methods through accelerated stability experiments. The experiments found that the original suction filtration method is relatively fast, but the filtration effect is not good, and it will cause a large loss of the active ingredients of the medicinal liquor to a large extent. The ultrafiltration machine filtration method takes a long time, has low efficiency, and the loss of active ingredients in the medicinal liquor after filtration is large, which may cause the effect of the medicinal liquor to decrease. The inventor also tried a variety of microporous filter membranes and found that the method of first filtering the drug extract with a polypropylene filter membrane, then filtering it with a polyethersulfone filter membrane, mixing it with rock sugar solution and then filtering it with a polyethersulfone filter membrane can effectively remove the tiny particles in the medicinal liquor, keep the medicinal liquor stable without precipitation for a long time, with very little loss of active ingredients, and low cost.

[0051] In the present invention, both the polypropylene filter membrane and the polyethersulfone filter membrane can be placed in a conventional filter in the art for filtration operations without any restrictions. According to a preferred embodiment of the present invention, the polypropylene filter membrane and the polyethersulfone filter membrane are placed in a flat - type filter or a pipeline filter for filtration operations. According to a preferred embodiment of the present invention, both the polypropylene filter membrane and the polyethersulfone filter membrane are placed in a flat - type filter for filtration operations.

[0052] In the present invention, the rock sugar solution is prepared by mixing rock sugar and water in a volume ratio of 1:2 and then filtering. The filtering method includes, but is not limited to, suction filtration, ultrafiltration, microfiltration, etc. Preferably, the rock sugar solution is filtered by ultrafiltration. Since the composition of the rock sugar solution is single and most of the impurities are simple solid particle impurities, ultrafiltration can effectively remove these impurities, and the operation is convenient and the cost is low. In the present invention, the dosage of rock sugar is 1 / 8 to 1 / 5 of the total weight of the raw medicine, preferably about 1 / 7 to 1 / 6.

[0053] After the second filtrate is mixed with the rock sugar solution, the ethanol content is adjusted to (39±2) degrees by volume. The solvent for adjusting the ethanol content can be high-concentration liquor or edible alcohol.

[0054] In the dispensing solution, the drug-loading concentration is 0.25 to 0.35 g of medicinal materials / ml, preferably 0.28 to 0.32 g of medicinal materials / ml, and more preferably 0.3 g of medicinal materials / ml. The drug-loading concentration can be adjusted by high-concentration liquor, edible alcohol and / or purified water.

[0055] Regarding the pore sizes of the above-mentioned polypropylene filter membrane and polyethersulfone filter membrane, the inventor found that when the pore size is lower than 0.22 μm, the loss of active ingredients is relatively large; while when the pore size is larger than 1 μm, the clarity of the medicinal liquor is low and the filtration is incomplete. Therefore, the filter membranes for the above-mentioned filtration are all filtered with filter membranes having a pore size of 0.22 to 1 μm. According to a preferred embodiment of the present invention, the pore sizes of the filter membranes for the above-mentioned filtration are all 0.45 μm.

[0056] The present invention found that in the mixed drug extract, the tiny particles that are the core of precipitation can increase in about 30 to 60 days. Although it cannot be clearly observed by the naked eye, a decrease in the light transmittance can be detected. These tiny particles are the key reasons for the precipitation in the subsequent finished medicinal liquor. In order to precipitate them fully, after the first filtration in the present invention, it is left standing for 30 to 60 days, and then the second filtration is carried out, thereby effectively removing these particles and avoiding the formation of precipitation in the finished medicinal liquor. According to a preferred embodiment of the present invention, after the first filtration, it is left standing for 35 to 50 days, and then the second filtration is carried out. According to a more preferred embodiment of the present invention, after the first filtration, it is left standing for 40 to 45 days, and then the second filtration is carried out. According to the most preferred embodiment of the present invention, after the first filtration, it is left standing for 45 days, and then the second filtration is carried out.

[0057] Through the improvement of the production process, the present invention effectively solves the problem that precipitation may occur during the storage of the medicinal liquor, and the content of active ingredients does not decrease, thereby ensuring the appearance and quality of the medicinal liquor.

[0058] The present invention solves the problem of medicinal liquor precipitation through a large number of experimental studies. The following specific examples and comparative examples are selected to illustrate the implementation mode and technical effects of the present invention, but the protection scope of the present invention is not limited thereto.

[0059] In the following examples and comparative examples, the prescription of the medicinal composition of the medicinal liquor is as follows: 2000 g of male silkworm moths, 300 g of epimedium, 250 g of dodder seeds, 150 g of wolfberries, 6 g of cordyceps sinensis, 50 g of cistanche, 6 g of rhodiola rosea, 150 g of astragalus membranaceus, 100 g of rehmannia glutinosa, and 3 g of saffron crocus.

[0060] Example 1

[0061] Take 2000 g of male silkworm moths and soak and extract them with 3000 ml of 50-degree white liquor for 10 days. Filter with an 80-mesh stainless steel filter screen. Add the filter residue to 1000 ml of 50-degree white liquor again and soak and extract for 2 days. Filter with an 80-mesh stainless steel filter screen. Combine the filtrates to obtain a male silkworm moth extract.

[0062] Example 2

[0063] Take nine traditional Chinese medicines, namely 300 g of epimedium, 250 g of dodder seeds, 150 g of wolfberries, 6 g of cordyceps sinensis, 50 g of cistanche, 6 g of rhodiola rosea, 150 g of astragalus membranaceus, 100 g of rehmannia glutinosa, and 3 g of saffron crocus. After soaking them in 50-degree white liquor for 48 hours, perform percolation extraction at a percolation rate of 25 - 35 ml / min to obtain 4900 ml of percolate.

[0064] Example 3

[0065] Mix the male silkworm moth extract obtained by the method of Example 1 and the percolate obtained by the method of Example 2 evenly to obtain 7850 ml of a drug extract.

[0066] Example 4

[0067] Take 3500 ml of the drug extract obtained by the method of Example 3 and filter it with a 0.45-μm polypropylene filter membrane to obtain a first filtrate.

[0068] Example 5

[0069] Take 300 ml of the drug extract obtained by the method of Example 3 and filter it with a 0.22-μm polypropylene filter membrane to obtain a first filtrate.

[0070] Example 6

[0071] Take 300 ml of the drug extract obtained by the method of Example 3 and filter it with a 1-μm polypropylene filter membrane to obtain a first filtrate.

[0072] Comparative Example 1-1

[0073] Filter 300 ml of the drug extract obtained by the method of Example 3 through a 0.1-μm polypropylene filter membrane to obtain a first filtrate.

[0074] Comparative Example 1-2

[0075] Filter 300 ml of the drug extract obtained by the method of Example 3 through a 3-μm polypropylene filter membrane to obtain a first filtrate.

[0076] Comparative Example 1-3

[0077] Filter 300 ml of the drug extract obtained by the method of Example 3 through a 0.45-μm polyethersulfone filter membrane to obtain a first filtrate.

[0078] Comparative Example 1-4

[0079] Ultrafilter 300 ml of the drug extract obtained by the method of Example 3 using an ultrafiltration machine with an ultrafiltration membrane having a molecular weight cut-off of 3000 to obtain a first filtrate.

[0080] Comparative Example 1-5

[0081] Filter 300 ml of the drug extract obtained by the method of Example 3 by suction filtration (using filter paper) to obtain a first filtrate.

[0082] Example 7

[0083] Let 1200 ml of the first filtrate obtained by the method of Example 4 stand for 45 days, and then filter it through a 0.45-μm polyethersulfone filter membrane to obtain a second filtrate.

[0084] Take 900 ml of this second filtrate and mix it with rock sugar solution (prepared by dissolving 51.6 g of rock sugar in 103.2 ml of water and ultrafiltration and purification), adjust the ethanol content to (39 ± 2) degrees and adjust the total volume to 1146 ml to obtain a blending solution.

[0085] Example 8

[0086] Let 400 ml of the first filtrate obtained by the method of Example 4 stand for 45 days, and then filter it through a 0.22-μm polyethersulfone filter membrane to obtain a second filtrate.

[0087] Example 9

[0088] Let 400 ml of the first filtrate obtained by the method of Example 4 stand for 45 days, and then filter it through a 1-μm polyethersulfone filter membrane to obtain a second filtrate.

[0089] Comparative Example 2

[0090] Leave 400 ml of the first filtrate obtained by the method of Example 4 to stand for 45 days, and then filter it through a 0.45-μm polypropylene filter membrane to obtain a second filtrate.

[0091] Example 10

[0092] Mix 300 ml of the second filtrate obtained by the method of Example 5 with ml of rock sugar solution, adjust the alcohol content to (39°±2), and add it to 1000 ml to obtain a blending solution. Take 300 ml of the blending solution obtained by the method of Example 7 and filter it through a 0.45-μm polyethersulfone filter membrane to obtain a sample of Tongmai Qiangshen Wine.

[0093] Example 11

[0094] Take 300 ml of the blending solution obtained by the method of Example 7 and filter it through a 0.22-μm polyethersulfone filter membrane to obtain a sample of Tongmai Qiangshen Wine.

[0095] Example 12

[0096] Take 300 ml of the blending solution obtained by the method of Example 10 and filter it through a 1-μm polyethersulfone filter membrane to obtain a sample of Tongmai Qiangshen Wine.

[0097] Comparative Example 3

[0098] Filter 400 ml of the first filtrate obtained by the method of Example 4 directly through a 0.45-μm polyethersulfone filter membrane without standing for 45 days to obtain a second filtrate. Mix this second filtrate with a rock sugar solution (prepared from 23 g of rock sugar and 46 ml of water and ultrafiltered and purified), adjust the ethanol content to (39±2) degrees and adjust the total volume to 509.3 ml to obtain a blending solution. Filter the blending solution through a 0.45-μm polyethersulfone filter membrane to obtain a sample of Tongmai Qiangshen Wine.

[0099] Comparative Example 4

[0100] Mix 400 ml of the drug extract obtained by the method of Example 3 with a rock sugar solution (prepared from 23 g of rock sugar and 46 ml of water and ultrafiltered and purified) to obtain a blending solution. Filter the blending solution by suction filtration and sterilize it to obtain a sample of Tongmai Qiangshen Wine.

[0101] Experimental Example 1 - First Filtration Effect Experiment

[0102] 1 Main instruments and reagents

[0103] High performance liquid chromatograph: Agilent;

[0104] Flat filter, polypropylene filter membrane, polyethersulfone filter membrane: Shanghai Gesi Fluid Equipment Technology Co., Ltd.;

[0105] Chromatographic grade acetonitrile: Oceanpak, Sweden.

[0106] 2 Experimental methods

[0107] Filtration was carried out using the methods of Examples 4 - 6 and Comparative Examples 1-1 - 1-5 respectively to obtain the first filtrate. For the examples and comparative examples involving microfiltration membranes, a flat filter equipped with the corresponding microfiltration membrane was used for filtration, and the peristaltic pump speed was 80 r / min, and the temperature was room temperature. The content of icariin, the active ingredient, and the clarity of the sample in the first filtrate samples obtained from each example and comparative example were determined, and the filtration flux was observed. Three parallel operations were performed for each sample, and the average value was measured as the experimental result.

[0108] 2.1 Determination of icariin content

[0109] Chromatographic conditions and system suitability test Octadecylsilane chemically bonded silica was used as the filler; acetonitrile - 0.025 mol / L phosphoric acid solution (1.7 ml of phosphoric acid was added to 1000 ml of water, and the pH value was adjusted to 3.0 ± 0.1 with triethylamine) (25:75) was used as the mobile phase; the detection wavelength was 270 nm. The number of theoretical plates calculated based on the icariin peak should be not less than 2500.

[0110] Preparation of reference substance solution An appropriate amount of icariin reference substance was accurately weighed and dissolved in methanol to prepare a solution containing 0.045 mg per 1 ml, that is, obtained.

[0111] Preparation of test solution An appropriate amount of the sample was taken, filtered, and the subsequent filtrate was taken, that is, obtained.

[0112] Determination method 10 μl of the reference substance solution and the test solution were accurately pipetted respectively and injected into the liquid chromatograph for determination, that is, obtained.

[0113] 2.2 Clarity determination

[0114] The light transmittance was used as an index to evaluate the clarity of the sample. The greater the light transmittance, the better the clarity. The clarity was determined by spectrophotometry, using distilled water as the reference, and the light transmittance (T, %) was measured at 338 nm.

[0115] 3 Experimental results

[0116] 3.1 Results of icariin content determination and clarity determination

[0117]

[0118] Note: It is stipulated in the product standard that each 1 ml contains not less than 0.035 mg of icariin. The light transmittance of distilled water is 100%.

[0119] As can be seen from the data in Table 1, the ultrafiltration machine filtration method takes a long time, has low efficiency, and the content of icariin in the medicinal liquor after filtration is greatly reduced. The suction filtration method is relatively fast, but affected by the adsorption of the filter material, the content of icariin is also significantly reduced. After filtration by the microfiltration membrane method, the content of icariin in the medicinal liquor is generally high, and the clarity data is also good. When the pore size of the microfiltration membrane is between 0.22 - 1 μm, both the content of icariin and the clarity are ideal, and the overall effect is optimal at 0.45 μm. When the pore size of the microfiltration membrane is 0.1 μm, the content of icariin is significantly reduced. When the pore size of the microfiltration membrane is 3 μm, the clarity is significantly reduced.

[0120] From the two indicators of the content of active ingredients and clarity, the filtration effects of polypropylene filter membrane and polyethersulfone filter membrane are similar. However, during the operation process, the problem of polyethersulfone filter membrane blockage is relatively serious, and the filtration flux is low. When using the polypropylene filter membrane, most of the impurity particles and colloidal substances are intercepted on the polypropylene filter membrane, and it is not easy to be blocked, with a high filtration flux. At the same time, the indicators of the content of active ingredients and clarity are similar to those of the polyethersulfone filter membrane, and the cost is lower. Therefore, comprehensively, using a 0.45 μm polypropylene filter membrane for the first filtration is the optimal solution.

[0121] Experimental Example 2 - Second Filtration Effect Experiment

[0122] 1 Main Instruments and Reagents

[0123] Same as item 1 of Experimental Example 1.

[0124] 2 Experimental Methods

[0125] Filter respectively using the methods of Examples 7 - 9 and Comparative Example 2 to obtain the second filtrate. All use a plate filter with the corresponding microfiltration membrane, and the peristaltic pump speed is all 80 r / min, and the temperature is at room temperature. Measure the content of the active ingredient icariin, the clarity of the sample, and the microbial limit of the filtrate samples obtained from each example and comparative example, and observe the filtration flux situation. Take three parallel operations for each sample, and measure the average value as the experimental result.

[0126] 2.1 Determination of Icariin Content

[0127] Same as item 2.1 of Experimental Example 1.

[0128] 2.2 Clarity Determination

[0129] Same as item 2.2 of Experimental Example 1.

[0130] 2.3 Investigation of Microbial Limit

[0131] The controlled bacteria are Staphylococcus aureus and Pseudomonas aeruginosa.

[0132] Applicability test for the inspection method of controlled bacteria:

[0133] Preparation of test solution: Take 10 ml of the sample and prepare a 1:10 test solution according to "Microbial Limit Test for Non-sterile Products: Microbial Enumeration Test (General Principle 1105)".

[0134] Positive control group: Take 1 ml of Staphylococcus aureus and Pseudomonas aeruginosa bacterial solutions (colony count: 10 - 100 cfu) respectively and inoculate them into 100 ml of tryptic soy broth liquid medium to observe the colony morphology.

[0135] Test article control group: Take 10 ml of the 1:10 test solution and inoculate it into 100 ml of tryptic soy broth liquid medium. Then add 1 ml of Staphylococcus aureus and Pseudomonas aeruginosa bacterial solutions (colony count: 10 - 100 cfu) respectively to observe the colony morphology.

[0136] Negative control group: Take 10 ml of sterile sodium chloride - peptone buffer solution with pH 7.0 and inoculate it into 100 ml of tryptic soy broth liquid medium to observe the colony morphology.

[0137] 3 Experimental results

[0138] 3.1 Results of icariin content determination and clarity determination

[0139]

[0140] Note: It is stipulated in the product standard that each 1 ml contains not less than 0.035 mg of icariin. The light transmittance of distilled water is 100%.

[0141] 3.2 Results of microbial inspection experiment

[0142]

[0143] After the first filtrate was left standing for 45 days, it was still clear to the naked eye, but the detected light transmittance showed a decrease. As can be seen from Table 2 and Table 3, from the two indicators of the active ingredient content and clarity, the filtration effects of polypropylene filter membrane and polyethersulfone filter membrane are close. Since most of the impurity particles and colloidal substances have been removed in the first filtration, in the second filtration, neither the polyethersulfone filter membrane nor the polypropylene filter membrane was blocked, and the filtration flux was high. After this filtration, there are certain requirements for the microbial content in the medicinal wine, and the polypropylene filter membrane cannot effectively remove microorganisms. Generally speaking, a polyethersulfone filter membrane with a pore size of 0.22 - 1 μm can achieve a good filtration effect in the second filtration, and the 0.45 - μm polyethersulfone filter membrane is the optimal solution.

[0144] Experimental Example 3 - Third Filtration Effect Experiment

[0145] 1 Main instruments and reagents

[0146] Same as item 1 of Experimental Example 1.

[0147] 2 Experimental Methods

[0148] The filtering methods of Examples 10 - 12 were respectively adopted to obtain Tongmai Qiangshen Wine. Flat filters with corresponding microporous membranes were used for filtering, and the peristaltic pump speed was 80 r / min at room temperature. The filtrate samples obtained from each example were subjected to the determination of the content of icariin as the active ingredient, the determination of sample clarity, and the determination of microbial limit, and the filtration flux was observed. Three parallel operations were taken for each sample, and the average value was measured as the experimental result.

[0149] 2.1 Determination of Icariin Content

[0150] Same as item 2.1 of Experimental Example 1.

[0151] 2.2 Determination of Clarity

[0152] Same as item 2.2 of Experimental Example 1.

[0153] 2.3 Investigation of Microbial Limit

[0154] Same as item 2.3 of Experimental Example 1.

[0155] 3 Experimental Results

[0156] 3.1 Results of the Determination of Icariin Content and Clarity

[0157]

[0158] Note: The standard of this product stipulates that each 1 ml contains not less than 0.035 mg of icariin. The light transmittance of distilled water is 100%.

[0159] 3.2 Experimental Results of Microbial Investigation

[0160]

[0161] The third filtration, i.e., the filtration of the blending liquid, is the last filtration operation, and the microbial limit also needs to be considered. Therefore, only the polyethersulfone membrane is considered. The filtration flux is good and the filtration efficiency is high. Considering the content of icariin, the clarity of the medicinal wine and the microbial limit comprehensively, polyethersulfone membranes with pore sizes of 0.22 - 1 μm can all achieve good filtration effects, and the 0.45 - μm polyethersulfone membrane is the optimal solution.

[0162] Experimental Example 4 - Long-Term Stability Experiment

[0163] The traditional Chinese medicine medicinal wine Tongmai Qiangshen Wine of Examples 10, Comparative Example 3 and Comparative Example 4 was allowed to stand for 36 months, and the content of icariin, clarity, microbial examination (the controlled bacteria are Staphylococcus aureus and Pseudomonas aeruginosa), and lamp inspection for precipitation were detected. The detection methods are the same as above.

[0164]

[0165] As can be seen from Table 6, the traditional Chinese medicine medicated wine produced according to the process of the present invention effectively solves the problem of precipitation while ensuring that the active ingredients are not lost, improving the quality stability of the product. The static placement of the first filtrate is a key step. The medicated wine without static placement still shows precipitation after 36 months.

[0166] The present invention is not limited to the above embodiments. Any variations, improvements, and substitutions that can be conceived by those skilled in the art without departing from the essence of the present invention fall within the scope of the present invention.

Claims

1. A method for preparing Chinese medicinal liquor, comprising the following steps: (1) soaking the male silkworm moth in white wine, extracting the male silkworm moth, and filtering the male silkworm moth extract; (2) extracting epimedium, dodder seed, wolfberry fruit, cordyceps sinensis, cistanche deserticola, rhodiola rosea, astragalus, rehmannia root and saffron by percolation with liquor to obtain a percolation liquid; (3) combining the male silkworm moth extract and the percolated liquid to obtain a drug extract; (4) Filtering the drug extract with a 0.22-1 μm polypropylene filter membrane to obtain a first filtrate; allowing the first filtrate to stand for 30-60 days, and then filtering with a 0.22-1 μm polyethersulfone filter membrane to obtain a second filtrate; mixing the second filtrate with rock sugar solution, adjusting the alcohol content to (39±2) degrees, and obtaining a prepared solution; filtering the prepared solution with a 0.22-1 μm polyethersulfone filter membrane to obtain the Chinese herbal wine.

2. The preparation method according to claim 1, characterized in that: In step (1), filtration is performed using a stainless steel filter screen with mesh size of 80 to 120.

3. The preparation method according to claim 1, characterized in that: In step (1), the soaking extraction is performed twice. The male silkworm moth is soaked in white wine for 10 to 60 days and filtered. The filter residue is added into white wine again for a second soaking extraction, soaked for 1 to 7 days and filtered. The filtrate is combined to obtain a male silkworm moth extract.

4. The preparation method according to claim 3, characterized in that: In step (1), the concentration of the liquor is 40 to 60 degrees by volume.

5. The preparation method according to claim 1, characterized in that: In step (2), Herba Epimedii, Semen Cuscutae, Fructus Lycii, Cordyceps Sinensis, Herba Cistanches, Rhodiola Rosea, Radix Astragali, Radix Rehmanniae Preparata and Saffron are first soaked in liquor for 1 to 3 days and then subjected to percolation extraction.

6. The preparation method according to claim 1, characterized in that: In step (4), the first filtrate is allowed to stand for 35 to 50 days.

7. The preparation method according to claim 6, characterized in that: In step (4), the first filtrate is allowed to stand for 40 to 45 days.

8. The preparation method according to claim 1, characterized in that: In step (4), the pore size of the polypropylene filter membrane is 0.45 μm, and the pore size of the polyethersulfone filter membrane is 0.45 μm.

9. The preparation method according to claim 1, characterized in that: In step (4), the polypropylene filter membrane is placed in a flat plate filter or a pipe filter, and the polyethersulfone filter membrane is placed in a flat plate filter or a pipe filter.

10. The preparation method according to claim 1, characterized in that: In step (4), the rock sugar solution is prepared by mixing rock sugar and water in a volume ratio of 1:2 and filtering the mixture. The filtering method is selected from suction filtration, ultrafiltration or microfiltration.

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