Processing method of radix ophiopogonis decoction pieces
By using isostearamide propyl betaine as the infiltration liquid and ultra-high pressure water jet technology and pyridine diimide as the dispersant, the problems of Ophiopogon japonicus loss and low cinnabar pulverization efficiency are solved, and high purity and high efficiency are achieved The production of Ophiopogon japonicus and cinnabar granules.
Patent Information
- Application Number
- CN202411084073.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-08-08
- Publication Date
- 2024-12-06
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
During the infiltration and flattening process, the effective ingredients of Ophiopogon japonicus are severely lost, which affects the efficacy of the medicine. The traditional water-flying method has low efficiency in crushing cinnabar, resulting in poor powder quality.
Isostearamide propyl betaine was used as the infiltration solution to improve the adhesion and stability of Ophiopogon japonicus, and ultra-high pressure water jet technology and pyridine diimide as dispersant were used to improve the cinnabar crushing efficiency.
Effectively retain the active ingredients of Ophiopogon japonicus, improve the purity and particle uniformity of Ophiopogon japonicus, and at the same time improve the cinnabar crushing efficiency to obtain high-quality Ophiopogon japonicus and cinnabar particles.
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Abstract
Description
Technical Field
[0001] The invention belongs to the field of traditional Chinese medicine, and particularly relates to a method for preparing Radix Ophiopogonis decoction pieces. Background Art
[0002] Ophiopogon japonicus is an important medicine for nourishing yin. It has the effects of moistening the lungs, promoting fluid production, clearing away heat and nourishing yin. It is often used clinically to treat symptoms such as yin deficiency, fatigue cough, and dry cough due to lung dryness. However, Ophiopogon japonicus must be processed before clinical application.
[0003] Studies have shown that after Ophiopogon japonicus is infiltrated and cored, the content of chemical components in the core of Ophiopogon japonicus is high, but the proportion in the medicinal material is small. This means that although core removal can increase the content of certain key components, the proportion of these components in the entire medicinal material is not high. In addition, the polysaccharide content of Ophiopogon japonicus increases after core removal, while the total flavonoid content decreases. This indicates that core removal may change the main chemical components of Ophiopogon japonicus, thereby affecting its pharmacological activity. During the infiltration process of Chinese medicinal materials, some effective ingredients may be lost due to the action of solvents, resulting in a decrease in efficacy. Therefore, improving the Ophiopogon japonicus infiltration solution to reduce the loss of effective ingredients is one of the research directions of the present invention.
[0004] In the process of flattening Ophiopogon japonicus, in the process of using the flattening machine, due to the pressure and the Van der Waals force and surface tension between the material surface and the roller, the fine materials will adhere to the roller in large quantities. The adhered materials will cause the surface of the roller steel to be uneven, increase the cleaning cost and cause the loss of nutrients in Ophiopogon japonicus, as well as the quality of the subsequent Ophiopogon japonicus slices. Therefore, preparing an anti-sticking layer on the roller surface is one of the key directions of the present invention.
[0005] GMT-421 is a highly efficient surface treatment agent that can prevent sticky materials from adhering. It consists of two components, liquid A and liquid B. It needs to be diluted with an organic solvent when used. However, organic solutions are prone to cause environmental pollution, so replacing the organic solution to reduce the pollution of the solution to the environment is the research focus of this invention.
[0006] Cinnabar, also known as cinnabar, cinnabar, and mercury sand, is a natural cinnabar ore of the sulfide type. It has the effects of clearing the heart and calming the nerves, soothing the nerves and detoxifying. It has a wide range of clinical applications. It is often mixed with minerals such as realgar, apatite, asphaltene, magnesium sulfide, and 25 trace elements such as bismuth, iron, lead, zinc, barium, copper, manganese, antimony, silicon, and arsenic. Among them, free mercury, barium, lead, antimony, and arsenic are harmful to the human body.
[0007] Ultra-high pressure water jet technology is applied in the field of industrial cutting, and is currently widely used in cleaning, crushing and medical fields. High-pressure water jet crushing technology is to use a high-pressure water jet carrying huge energy to act on the material to be crushed in a certain way, generating pressure transients in the cracks and joints of the material, thereby crushing the material.
[0008] Compared with the traditional water jet method, the ultra-high pressure water jet pulverization has high efficiency and better effect. The process uses distilled water as the solution, and requires a large amount of water and multiple repetitions to obtain cinnabar with good powder quality. Therefore, the present invention improves the aqueous solution with additives and studies the addition of dispersants to improve the efficiency of the process and the quality of the powder. Summary of the invention
[0009] The present invention discloses a method for preparing Radix Ophiopogonis decoction pieces to solve the above and any potential problems in the prior art. In order to solve the above technical problems, the method for preparing the present invention is as follows:
[0010] Soak the Ophiopogon japonicus for 30-60 minutes, then draw out the core, flatten it into slices, dry it at 60°C for 10 minutes, spray 0.5%-1% clean water on the surface of the Ophiopogon japonicus slices, add 2kg of cinnabar powder for every 100kg of Ophiopogon japonicus, stir, take out, and dry at 50-60°C for 3-5 minutes.
[0011] The infiltration solution is a solution of isostearamidopropyl betaine with a mass fraction of 5-8% added according to a solid-liquid ratio of 1:2.
[0012] The flattened sheet also includes an anti-sticking layer prepared for this product, and its preparation process includes: mixing GMT-421A:GMT-421B in a mass ratio of 10:1, adding diluent to dilute 1-3 times to prepare a working solution, first coating a layer of silica sol with a mass fraction of 10% on the surface of the roller, and after drying, putting it in an oven at 140-150°C, baking for 2-3 minutes, taking out the working solution and applying it to the roller with silica sol by brushing, the temperature is 150-160°C, and baking for 4-6 hours.
[0013] The diluent is a 20% by mass diethyl 2-fluoromalonate solution.
[0014] The cinnabar fine powder is prepared by ultra-high pressure water jet technology, and the specific process is as follows: cinnabar dispersion and distilled water are mixed in a ratio of 1:3, the pressure of the high-pressure water jet is 260-300Mpa, the cinnabar suspension crushed by the ultra-high pressure water jet is collected at the nozzle, the upper layer of clear water is poured off, the remaining part is transferred to a watch glass, and placed in an oven to dry at 40°C for use.
[0015] The cinnabar dispersion is prepared by preparing a 5-8% dispersion solution of a dispersant, adding cinnabar powder in equal proportion, and oscillating ultrasonically at a low frequency of 40 Hz for 10 minutes.
[0016] Wherein, the dispersant is pyridine diimide.
[0017] The advantages and beneficial effects of the present invention are:
[0018] 1. The present invention provides a method for preparing Radix Ophiopogonis slices, which comprises soaking Radix Ophiopogonis, flattening, removing the core, drying, spraying with clean water, and mixing with cinnabar fine powder to retain the effective ingredients to the greatest extent to obtain Radix Ophiopogonis slices with high purity and uniform particles.
[0019] 2. The present invention selects alkaline isostearamidopropyl betaine as the infiltration liquid. Since the alkaline isostearamidopropyl betaine has the function of a betaine surfactant, it can improve the adhesion of the solvent on the surface of the Ophiopogon japonicus and increase the diffusion and penetration of the solvent into the Ophiopogon japonicus. Secondly, since the solvent is alkaline at a certain concentration, the phenomenon of excessive loss of effective ingredients during the infiltration process is reduced, thereby ensuring the quality and efficacy of the Chinese medicinal materials.
[0020] 3. In addition, the long hydrophobic fatty amide chain contained in isostearamide can also combine with the fat-soluble components in Ophiopogon japonicus to form micelles during the infiltration process, thereby improving its stability and helping to maintain the relative content and activity of the fat-soluble components in Ophiopogon japonicus.
[0021] 4. The present invention uses diethyl 2-fluoromalonate to replace the organic solution, which has good solubility and stability, can reduce the use of organic solvents, and reduce environmental pollution. The carbonyl group in the diethyl 2-fluoromalonate molecule enables the two components in GMT-421 to undergo cross-linking and curing reactions in a wider temperature range; and the ethyl ester group in the molecule gives GMT-421 better flexibility, adhesion and solvent solubility, thereby obtaining a product with better anti-sticking, wear resistance and good bonding strength with stainless steel rollers, and better temperature resistance and corrosion resistance.
[0022] 5. In addition, diethyl 2-fluoromalonate also has certain antibacterial properties, which can inhibit the growth of microorganisms and help maintain the cleanliness of materials or products. The anti-sticking flattened Ophiopogon japonicus slices can effectively reduce the cracking of Chinese medicinal materials during the flattening process and improve the overall quality of Ophiopogon japonicus slices.
[0023] 6. Compared with the traditional water jet method, ultra-high pressure water jet crushing has high efficiency and better effect. Pyridine diimide is a cationic dispersant that can be used as a dispersant for cinnabar powder. It has a good dispersion effect when combined with ultrasonic treatment. Pyridine diimide can effectively prevent cinnabar powder from agglomerating during stirring. By reducing the mutual attraction between particles, pyridine diimide can keep cinnabar powder in a stable dispersed state, thereby avoiding the occurrence of agglomeration. It can also improve the fluidity and compressibility of cinnabar powder, making it more susceptible to the action of ultra-high pressure water jets and improving crushing efficiency. In this way, the required degree of crushing can be achieved in a shorter time, thereby improving production efficiency.
[0024] 7. Compared with the commonly used N, N-dimethylformamide dispersant, pyridine diimide is more environmentally friendly, safer, has better dispersing effect and wider applicability, and is more preferred in this invention. The pyridine group in pyridine diimide can also serve as a metal ligand, can form a stable complex with impurities and heavy metals in cinnabar, and can avoid the reduction of mercury in HgS caused by grinding cinnabar, increase the content of free mercury in cinnabar, thereby obtaining cinnabar particles with higher purity and better quality. DETAILED DESCRIPTION
[0025] The present invention is further described in detail below in conjunction with the embodiments. The flattening machines used in the following flattening process are all ZYJ-160 type flattening machines.
[0026] Example 1
[0027] Anti-sticking layer of the flattening machine: Mix GMT-421A and GMT-421B in a mass ratio of 10:1, add 20% by mass fraction of diethyl 2-fluoromalonate solution to dilute it 2 times to make a working solution, first apply a layer of 10% by mass fraction of silica sol on the surface of the roller, after drying, put it in an oven at 145°C, bake for 2-3 minutes, take out and apply the working solution on the roller with silica sol by brushing, the temperature is 155°C, and bake for 5 hours.
[0028] The preparation of cinnabar fine powder is as follows: pyridine diimide is prepared into a 6% dispersion solution, cinnabar powder is added in equal proportion, and cinnabar dispersion is obtained at a low frequency of 40 Hz for 10 minutes by ultrasonic oscillation. The cinnabar dispersion and distilled water are mixed in a ratio of 1:3, the pressure of the high-pressure water jet is 280 MPa, and the cinnabar suspension crushed by the ultra-high pressure water jet is collected at the nozzle, the upper layer of clear water is poured off, and the remaining part is transferred to a watch glass, and dried in an oven at 40°C for later use.
[0029] Add 6% isostearamidopropyl betaine solution by mass into Ophiopogon japonicus according to the solid-liquid ratio of 1:2, soak for 45 minutes and then draw the core; flatten into slices by anti-sticking flattening machine, dry at 60°C for 10 minutes, spray 0.8% clean water on the surface of Ophiopogon japonicus slices, add 2kg of cinnabar powder for every 100kg of Ophiopogon japonicus, stir, take out, and dry at 55°C for 4 minutes.
[0030] Example 2
[0031] Anti-sticking layer of the flattening machine: Mix GMT-421A and GMT-421B in a mass ratio of 10:1, add 20% by mass fraction of diethyl 2-fluoromalonate solution to dilute it by 1 time to prepare the working solution, first apply a layer of 10% by mass fraction of silica sol on the surface of the roller, after drying, put it in an oven at 150°C, bake for 2 minutes, take out and apply the working solution on the roller with silica sol by brushing, the temperature is 160°C, and bake for 4 hours.
[0032] The preparation of cinnabar fine powder is as follows: pyridine diimide is prepared into an 8% dispersion solution, cinnabar powder is added in equal proportion, and cinnabar dispersion is obtained at a low frequency of 40 Hz for 10 minutes by ultrasonic oscillation, the cinnabar dispersion and distilled water are mixed in a ratio of 1:3, the pressure of the high-pressure water jet is 300 MPa, the cinnabar suspension crushed by the ultra-high pressure water jet is collected at the nozzle, the upper layer of clear water is poured off, the remaining part is transferred to a watch glass, and dried in an oven at 40°C for later use.
[0033] Add 8% isostearamidopropyl betaine solution by mass into Ophiopogon japonicus according to the solid-liquid ratio of 1:2, soak for 30 minutes and then draw the core; flatten into slices by anti-sticking flattening machine, dry at 60°C for 10 minutes, spray 1% clean water on the surface of Ophiopogon japonicus slices, add 2kg of cinnabar powder for every 100kg of Ophiopogon japonicus, stir, take out, and dry at 50°C for 5 minutes.
[0034] Example 3
[0035] Anti-sticking layer of the flattening machine: Mix GMT-421A and GMT-421B in a mass ratio of 10:1, add 20% by mass fraction of diethyl 2-fluoromalonate solution to dilute it 3 times to make a working solution, first apply a layer of 10% by mass fraction of silica sol on the surface of the roller, after drying, put it in an oven at 140°C, bake for 3 minutes, take out the working solution and apply it to the roller with silica sol by brushing, the temperature is 150°C, and bake for 6 hours.
[0036] The preparation of cinnabar fine powder is as follows: prepare pyridine diimide into a 5% dispersion solution, add cinnabar powder in equal proportion, ultrasonically oscillate at a low frequency of 40 Hz for 10 minutes to obtain a cinnabar dispersion, mix the cinnabar dispersion and distilled water in a ratio of 1:3, the high-pressure water jet pressure is 260 MPa, collect the cinnabar suspension crushed by the ultra-high pressure water jet at the nozzle, pour off the upper clear water, transfer the remaining part to a watch glass, place it in an oven at 40°C to dry, and set aside.
[0037] Add 5% isostearamidopropyl betaine solution by mass into Ophiopogon japonicus according to the solid-liquid ratio of 1:2, soak for 60 minutes and then draw the core; flatten into slices by anti-sticking flattening machine, dry at 60°C for 10 minutes, spray 0.5% clean water on the surface of Ophiopogon japonicus slices, add 2kg of cinnabar powder for every 100kg of Ophiopogon japonicus, stir, take out, and dry at 60°C for 3min.
[0038] Comparative Example 1
[0039] The difference between this comparative example and Example 1 is that in this comparative example, Ophiopogon japonicus is soaked in clean water, and the specific process is: add clean water to Ophiopogon japonicus according to a solid-liquid ratio of 1:2 and soak for 60 minutes, then extract the core; flatten it into slices with an anti-sticking flattening machine, dry it at 60°C for 10 minutes, spray 0.5% clean water on the surface of the Ophiopogon japonicus slices, use 2kg of cinnabar powder for every 100kg of Ophiopogon japonicus, stir it, take it out, and dry it at 60°C for 3min; the rest is the same as Example 1.
[0040] Comparative Example 2
[0041] The difference between this comparative example and Example 1 is that isostearamidopropyl betaine is N-acylglutamic acid, and the rest is the same as Example 1.
[0042] Comparative Example 3
[0043] The difference between this comparative example and Example 1 is that the amount of isostearamidopropyl betaine solution added in this comparative example is different, and the specific process is as follows: add 30% isostearamidopropyl betaine solution by mass fraction to Ophiopogon japonicus according to a solid-liquid ratio of 1:2, soak for 45 minutes, and then draw the core; flatten it into slices with an anti-sticking flattening machine, dry it at 60°C for 10 minutes, spray 0.8% clean water on the surface of the Ophiopogon japonicus slices, use 2 kg of cinnabar powder for every 100 kg of Ophiopogon japonicus, stir it, take it out, and dry it at 55°C for 4 minutes; the rest is the same as Example 1.
[0044] Comparative Example 4
[0045] The difference between this comparative example and Example 1 is that the amount of isostearamidopropyl betaine solution added in this comparative example is different, and the specific process is as follows: add 2% isostearamidopropyl betaine solution by mass at a solid-liquid ratio of 1:2 to Ophiopogon japonicus, soak for 45 minutes, and then draw the core; flatten it into slices with an anti-sticking flattening machine, dry it at 60°C for 10 minutes, spray 0.8% clean water on the surface of the Ophiopogon japonicus slices, use 2kg of cinnabar powder for every 100kg of Ophiopogon japonicus, stir it, take it out, and dry it at 55°C for 4 minutes; the rest is the same as Example 1.
[0046] Comparative Example 5
[0047] The difference between this comparative example and Example 1 is that the anti-stick coating is not applied to the flattening machine. Specifically, the Ophiopogon japonicus is soaked in a 6% isostearamidopropyl betaine solution at a solid-liquid ratio of 1:2 for 45 minutes and then the core is extracted; the Ophiopogon japonicus is flattened into slices by a flattening machine, and after drying at 60°C for 10 minutes, 0.8% clean water is sprayed on the surface of the Ophiopogon japonicus slices, 2 kg of cinnabar powder is used for every 100 kg of Ophiopogon japonicus, the slices are stirred, taken out, and dried at 55°C for 4 minutes; the rest is the same as Example 1.
[0048] Comparative Example 6
[0049] The difference between this comparative example and Example 1 is that the 2-fluoromalonic acid diethyl ester solution of the anti-sticking layer of the flattening machine is a trichloroethylene solution; the rest is the same as Example 1.
[0050] Comparative Example 7
[0051] The difference between this comparative example and Example 1 is that the amount of 2-fluoromalonate solution added is different. The specific process for preparing the anti-sticking layer of the flattening machine is as follows: GMT-421A: GMT-421B are mixed in a mass ratio of 10:1, and 50% of 2-fluoromalonate solution is added to dilute it by 2 times to prepare a working solution. First, a layer of 10% silica sol is coated on the surface of the roller. After drying, it is placed in an oven at 145°C. After baking for 2-3 minutes, the working solution is taken out and coated on the roller with silica sol by brushing. The temperature is 155°C and baked for 5 hours. The rest is the same as Example 1.
[0052] Comparative Example 8
[0053] The difference between this comparative example and Example 1 is that the amount of 2-fluoromalonate solution added is different. The specific process for preparing the anti-sticking layer of the flattening machine is as follows: GMT-421A: GMT-421B are mixed in a mass ratio of 10:1, and a 10% mass fraction of 2-fluoromalonate solution is added to dilute it by 2 times to prepare a working solution. First, a layer of 10% mass fraction of silica sol is coated on the surface of the roller. After drying, it is placed in an oven at 145°C. After baking for 2-3 minutes, the working solution is taken out and coated on the roller with silica sol by brushing. The temperature is 155°C and baked for 5 hours. The rest is the same as Example 1.
[0054] Test 1: Anti-sticking layer performance test
[0055] The above-mentioned anti-stick coating was applied on a stainless steel plate of 200×200×2 mm and the following test was performed:
[0056] The adhesion of the coating was measured according to GB / T 9286-88 Paints and varnishes - Cross-cut test for coating films; the anti-sticking property of the coating or the roller of the flattening machine was measured using a FibDAT 1100 contact angle tester; the wear resistance was measured using a CM unglazed tile resistance tester, and the wear resistance effect was expressed by the friction chord length. The results are shown in Table 1.
[0057] Table 1 Performance test results
[0058] Group Anti-stickiness(°) Wear resistance(mm) Example 1 135.9 5.50 Example 2 132.6 5.30 Example 3 134.8 5.35 Comparative Example 5 86.5 3.50 Comparative Example 6 95.9 4.20 Comparative Example 7 126.7 4.85 Comparative Example 8 115.6 4.30
[0059] Comparative Example 9
[0060] The difference between this comparative example and Example 1 is that the traditional water milling method is used to obtain cinnabar fine powder in this comparative example. The specific process is: put 220 parts of cinnabar with impurities removed in a grinding cylinder, add 400g of grinding zirconium balls with diameters of 1, 2, 3, and 4mm, the ratio of which is 1.5:1.5:0.5:0.5, add 420 parts of pure water, grind at a speed of 800r / min for 120min, add 600 parts of pure water, pour out all the suspension, let it stand for 72h, take the precipitate, dry at 40℃ for 2h, grind through an 80-mesh sieve to obtain cinnabar fine powder for use; the rest is the same as Example 1.
[0061] Comparative Example 10
[0062] The difference between this comparative example and Example 1 is that the pyridine diimide is N,N-dimethylformamide solution, and the rest is the same as Example 1.
[0063] Comparative Example 11
[0064] The difference between this comparative example and Example 1 lies in the different amounts of pyridine diimide added. The specific cinnabar fine powder process is as follows: prepare a 12% dispersion solution of pyridine diimide, add cinnabar powder in equal proportion, ultrasonically oscillate at a low frequency of 40 Hz for 10 min to obtain a cinnabar dispersion, mix the cinnabar dispersion and distilled water in a ratio of 1:3, the high-pressure water jet pressure is 280 MPa, collect the cinnabar suspension crushed by the ultra-high pressure water jet at the nozzle, pour off the upper clear water, transfer the remaining part to a watch glass, dry in an oven at 40°C for use; the rest is the same as Example 1.
[0065] Comparative Example 12
[0066] The difference between this comparative example and Example 1 lies in the different amounts of pyridine diimide added. The specific cinnabar fine powder process is as follows: prepare 2% pyridine diimide into a dispersion solution, add cinnabar powder in equal proportion, ultrasonically oscillate at a low frequency of 40 Hz for 10 min to obtain a cinnabar dispersion, mix the cinnabar dispersion and distilled water in a ratio of 1:3, the high-pressure water jet pressure is 280 MPa, collect the cinnabar suspension crushed by the ultra-high pressure water jet at the nozzle, pour off the upper clear water, transfer the remaining part to a watch glass, dry in an oven at 40°C for use; the rest is the same as Example 1.
[0067] Test 2: Determination of properties of cinnabar powder
[0068] The cinnabar used in the above embodiments and comparative examples were purchased from Shijiazhuang Chen High-tech Material Technology Co., Ltd. The content of mercuric sulfide in the crude cinnabar is 84.96%, which is lower than the requirement of the 2005 edition of the Chinese Pharmacopoeia (the content of mercuric sulfide, the main component of cinnabar, shall not be less than 96%). Therefore, cinnabar needs to undergo a certain processing process before it can be used as a qualified medicine.
[0069] With reference to the content determination methods under Cinnabar and its decoction pieces in Volume 1 of the Chinese Pharmacopoeia (2015 edition), the content of mercuric sulfide after ball milling was determined.
[0070] Process yield = weight of collected drug / dosage
[0071] The test results are shown in Table 2 below:
[0072] Table 2 Cinnabar properties test results
[0073] Group Mercury sulfide content (%) Yield (%) Example 1 99.85 99.20 Example 2 99.64 98.86 Example 3 99.56 98.76 Comparative Example 9 96.45 95.63 Comparative Example 10 97.45 96.45 Comparative Example 11 99.31 98.23 Comparative Example 12 98.25 97.51
[0074] Experiment 3: Measurement of Ophiopogon japonicus polysaccharides
[0075] Preparation of glucose reference solution: Dry anhydrous glucose at 105°C to constant weight, accurately weigh 0.0495 g, place in a 50 mL volumetric flask, add water to dissolve and make up to volume to obtain a glucose reference solution with a concentration of 0.990 mg / mL.
[0076] Drawing of standard curve: Accurately measure 0, 1.0, 2.0, 3.0, 4.0, and 5.0 mL of glucose reference solution, place them in 50 mL volumetric flasks, and add water to make up the volume. Take 1.0 mL of the above solution and add it to 5 stoppered test tubes, add 1.0 mL of 5% phenol solution, and then quickly add 5.0 mL of concentrated sulfuric acid vertically, stopper, and shake well. Heat in a boiling water bath for 30 minutes, take out and cool to room temperature with ice water, and perform the same operation with 1 mL of double distilled water as the blank control solution. According to the UV-visible spectrophotometry, measure the absorbance at a wavelength of 488 nm. With the absorbance as the ordinate (Y) and the concentration of the glucose standard solution as the abscissa (X), perform linear regression to obtain the standard curve.
[0077] Determination of conversion factor: 30g of Ophiopogon japonicus powder was extracted 3 times with 75% ethanol at 60℃ water bath (2h each time), the ethanol was evaporated from the residue, and distilled water was added to heat and extract 3 times at 90℃, filtered, the combined solution was concentrated to 40mL under reduced pressure, anhydrous ethanol was added to the concentrate to make the alcohol content reach 80%, and the concentrate was placed in a 4℃ refrigerator for alcohol precipitation overnight. The precipitate was centrifuged and dried to obtain crude polysaccharide. The crude polysaccharide was deproteinized by Servage method, and then precipitated with alcohol (80% alcohol content, the same operation as above) twice. The precipitate was washed with anhydrous ethanol, acetone, and ether respectively, and vacuum dried at 60℃ to constant weight to obtain Ophiopogon japonicus refined polysaccharide. 0.0159g of Ophiopogon japonicus refined polysaccharide was accurately weighed and placed in a 50mL volumetric flask. After adding water to the volume, a 0.318mg / mL polysaccharide solution was obtained.
[0078] Take 1.0 mL of Ophiopogon japonicus refined polysaccharide solution, put it in a stoppered test tube, measure the absorbance at a wavelength of 488 nm, and calculate the concentration C (mg / mL) of glucose in the Ophiopogon japonicus refined polysaccharide solution by the regression equation. Calculate the conversion factor according to the formula f=W / (CxD), where is the weight of the polysaccharide (mg), C is the glucose concentration in the polysaccharide (mg / mL), and D is the dilution multiple.
[0079] Preparation of sample solution: respectively crush the raw Ophiopogon japonicus, Examples 1-3, and Comparative Examples 1-12 into pieces, take 1.0 g of each sample powder, accurately weigh, heat and reflux with 50 ml 80% ethanol twice (2 h each time), filter, wash the filter residue with 80% hot ethanol 3 times (10 mL each time), evaporate the ethanol, extract with 50 ml water 3 times (2 h each time), filter while hot, wash the filter residue with hot purified water 3 times (10 mL each time), combine the filtrate and the washing solution and concentrate, cool and transfer to a 50 ml volumetric flask, add water to volume, shake well, and obtain.
[0080] Determination of polysaccharide content in samples: Accurately pipette 0.5 ml of each of the above sample solutions into a 10 ml volumetric flask, dilute to the mark with water and shake well, take 1.0 ml into a stoppered graduated test tube, measure the absorbance at a wavelength of 488 nm, and then calculate the concentration of glucose in each test solution according to the regression equation, and calculate the polysaccharide content therein according to the formula (CxDxf / W)x100%, where C is the concentration (mg / mL) of glucose in the sample solution to be tested, D is the dilution multiple, f is the polysaccharide conversion factor, and W is the dry weight of the sample to be tested. The results are shown in Table 3.
[0081] Table 3 Ophiopogon japonicus polysaccharide content
[0082]
[0083]
Claims
1. A method for preparing Radix Ophiopogonis decoction pieces, characterized in that: The processing method specifically comprises the following steps: Soak the Ophiopogon japonicus for 30-60 minutes, then draw out the core, flatten it into slices, dry it at 60℃ for 10 minutes, spray 0.5%-1% clean water on the surface of the Ophiopogon japonicus slices, add 2kg of cinnabar powder for every 100kg of Ophiopogon japonicus, stir, take out, and dry it at 50-60℃ for 3-5 minutes. The infiltration solution is a solution of isostearamidopropyl betaine with a mass fraction of 5-8% added according to a solid-liquid ratio of 1:
2.
2. The method for preparing the Radix Ophiopogonis decoction pieces according to claim 1, characterized in that: The flattened sheet also includes an anti-sticking layer prepared for this product, and its preparation process includes: mixing GMT-421A:GMT-421B in a mass ratio of 10:1, adding a diluent to dilute 1-3 times to prepare a working solution, first coating a layer of silica sol with a mass fraction of 10% on the surface of the roller, and after drying, putting it in an oven at 140-150°C, baking for 2-3 minutes, taking out the working solution and applying it to the roller with silica sol by brushing, the temperature is 150-160°C, and baking for 4-6 hours.
3. A method for preparing Radix Ophiopogonis japonicus slices according to claim 2, characterized in that: The diluent is a 20% by mass diethyl 2-fluoromalonate solution.
4. The method for preparing the Radix Ophiopogonis decoction pieces according to claim 1, characterized in that: The cinnabar fine powder is prepared by ultra-high pressure water jet technology, and the specific process is as follows: cinnabar dispersion and distilled water are mixed in a ratio of 1:3, the pressure of the high-pressure water jet is 260-300Mpa, the cinnabar suspension crushed by the ultra-high pressure water jet is collected at the nozzle, the upper layer of clear water is poured off, the remaining part is transferred to a watch glass, and placed in an oven to dry at 40°C for use.
5. The method for preparing the Radix Ophiopogonis decoction pieces according to claim 4, characterized in that: The cinnabar dispersion is prepared by preparing a 5-8% dispersion solution of a dispersant, adding cinnabar powder in equal proportion, and oscillating ultrasonically at a low frequency of 40 Hz for 10 minutes.
6. The method for preparing the Radix Ophiopogonis decoction pieces according to claim 5, characterized in that: in, The dispersant is pyridine diimide.
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