Preparation method of Polygonum multiflorum superfine powder

Abstract

The invention discloses a method for preparing superfine powder of Polygonum multiflorum, comprising: step 1, washing the raw medicinal material of Polygonum multiflorum, removing impurities, drying, and slicing; step 2, soaking Polygonum multiflorum, soaking in drinking water, boiling, filtering, obtaining Polygonum multiflorum water extract and Polygonum multiflorum water extract residue, placing Polygonum multiflorum water extract residue in drinking water, boiling, filtering, obtaining Polygonum multiflorum water extract and Polygonum multiflorum water extract residue; step 3, combining the water extract, vacuum rotary evaporation concentration, obtaining extract, vacuum drying, obtaining water extract particles, uniformly spraying embedding liquid, drying, microwave drying, obtaining water extract dry particles; step 4, crushing the water extract dry particles into coarse powder, fine powder, and superfine powder. The superfine powder prepared by the present invention has uniform powder body, high dissolution rate of effective ingredients, reduces production cost, saves the amount of medicinal materials, and is expected to be used for industrial production.

Description

Technical Field

[0001] The present invention relates to the technical field of Chinese medicinal material processing, and more specifically, to a method for preparing superfine powder of Polygonum multiflorum. Background Art

[0002] Polygonum multiflorum is the root of Polygonum multiflorum Thunb., a plant of the Polygonaceae family. It has the effects of nourishing essence and blood, detoxifying, stopping malaria, and moistening the intestines and relieving constipation. It is mainly used to treat deficiency of essence and blood, dizziness, premature graying of hair and beard, soreness of waist and knees, long-term malaria, carbuncle, scrofula, and constipation caused by dry intestines. Polygonum multiflorum is usually decocted and taken in the form of conventional slices, but the slices made of the root have a hard texture and irregular shape, and the effective ingredients are difficult to fully dissolve. Superfine powder technology can crush Chinese medicinal materials into powder, and can even be dissolved in water for drinking, which is conducive to retaining effective ingredients and improving dissolution rate. Applying it to Polygonum multiflorum slices is the research direction of this application. Directly crushing Polygonum multiflorum slices into superfine powder has the problem that the cell wall breaking rate is not high due to texture reasons, and the effective ingredients of Polygonum multiflorum are mainly fat-soluble compounds, which are not conducive to dissolution. How to improve the utilization of the effective ingredients of Polygonum multiflorum by superfine powder technology is a technical problem that this application aims to solve. Summary of the invention

[0003] The invention provides a method for preparing superfine powder of Polygonum multiflorum. The prepared superfine powder has uniform powder body and high dissolution rate of effective components, thus reducing production cost, saving the amount of medicinal materials, and is expected to be used in industrial production.

[0004] In order to achieve these purposes and other advantages according to the present invention, a method for preparing superfine powder of Polygonum multiflorum is provided, comprising:

[0005] Step 1: Wash the raw material of Polygonum multiflorum, remove impurities, dry it, and slice it;

[0006] Step 2: soak the Polygonum multiflorum in a 30-50% sucrose solution for 40-60 minutes, rinse and drain, soak the Polygonum multiflorum in drinking water at a ratio of 10kg / 30-50L, boil and keep for 40-60 minutes, filter to obtain a Polygonum multiflorum water extract and a Polygonum multiflorum water extract residue, and soak the Polygonum multiflorum water extract residue in drinking water at a ratio of 10kg / 10-20L, boil and keep for 20-40 minutes, filter to obtain a Polygonum multiflorum water extract and a Polygonum multiflorum water extract residue;

[0007] Step 3, combining the water extracts, concentrating them under reduced pressure at 60-80°C, obtaining an extract, vacuum drying, obtaining water extract particles, spraying the embedding solution evenly, drying at 50-60°C for 1-2h, and microwave drying until the moisture content is less than 10%, obtaining water extract dry particles;

[0008] Step 4: Grind the dry particles of the water extract into coarse powder with a particle size not exceeding 1 mm, then grind the coarse powder into fine powder with a particle size not exceeding 200 μm, and then ultrafine grind the fine powder into ultrafine Polygonum multiflorum powder with a particle size not exceeding 20 μm.

[0009] Preferably, the vacuum drying conditions are 50-60° C., the vacuum degree is 10-20 kPa, and the drying time is 24 h.

[0010] Preferably, the ratio of core material to wall material in the embedding process is 1:6, and the embedding solution comprises a mixed solution of dextrin, gum arabic, sodium bicarbonate and water in a mass ratio of 1:3:6:90.

[0011] Preferably, the embedding conditions are a spraying rate of 3 to 5 kg / min, a stirring rate of 5000 r / min, and a stirring time of 15 to 20 min.

[0012] Preferably, step 4 is replaced by:

[0013] Step 4: Combine the water-extracted residues, place them at 60-80° C. and 30-50 kPa for 40-60 minutes, crush them to a particle size of no more than 1 cm, then keep them at below -18° C. and 10-20 kPa for 4-6 hours, then transfer them to 60-80° C. and 30-50 kPa for 4-6 hours, crush them into particles, and microwave dry them until the moisture content is less than 10%, thereby obtaining dry particles of water-extracted residues;

[0014] Also includes:

[0015] Step 5: Combine the dry particles of the water extract and the dry particles of the water extract residue, and grind them into coarse powder with a particle size not exceeding 1 mm, then grind the coarse powder into fine powder with a particle size not exceeding 200 μm, and then ultrafinely grind the fine powder into ultrafine Polygonum multiflorum powder with a particle size not exceeding 20 μm.

[0016] Preferably, the power of microwave drying is 1000-1200W.

[0017] The superfine powder of Polygonum multiflorum obtained by the preparation method.

[0018] The present invention has at least the following beneficial effects:

[0019] The ultrafine powder of Polygonum multiflorum prepared by the invention has uniform crushing particle size and meets the standard, increases osmotic pressure by embedding, improves the embedding rate of effective ingredients, retains water extraction residue, improves the retention of effective ingredients, dehumidifies and embrittles the water extraction residue, increases the wall breaking rate of Chinese medicinal material cells, is conducive to ultrafine grinding, increases the added value of Polygonum multiflorum, reduces production costs, saves the amount of medicinal materials, and is expected to be used in industrial production.

[0020] Other advantages, objectives and features of the present invention will be embodied in part through the following description, and in part will be understood by those skilled in the art through study and practice of the present invention. DETAILED DESCRIPTION

[0021] The present invention is further described in detail below with reference to examples so that those skilled in the art can implement the invention with reference to the description.

[0022] It should be understood that the terms such as “having”, “including” and “comprising” used herein do not exclude the existence or addition of one or more other elements or combinations thereof.

[0023] It should be noted that the experimental methods described in the following embodiments are conventional methods unless otherwise specified, and the reagents and materials can be obtained from commercial channels unless otherwise specified.

[0024] <Example 1>

[0025] The method for preparing superfine powder of Polygonum multiflorum comprises:

[0026] Step 1: Wash the raw material of Polygonum multiflorum, remove impurities, dry it, and slice it;

[0027] Step 2: soak the Polygonum multiflorum in a 35% sucrose solution for 40 minutes, rinse and drain, soak the Polygonum multiflorum in drinking water at a ratio of 10kg / 35L, boil and keep for 40 minutes, filter to obtain a Polygonum multiflorum water extract and a Polygonum multiflorum water extract residue, and soak the Polygonum multiflorum water extract residue in drinking water at a ratio of 10kg / 15L, boil and keep for 20 minutes, filter to obtain a Polygonum multiflorum water extract and a Polygonum multiflorum water extract residue;

[0028] Step three, combining the water extracts, concentrating under reduced pressure rotary evaporation at 60-80°C to obtain an extract, vacuum drying, the vacuum drying conditions are 50-60°C, the vacuum degree is 10-20kPa, the drying time is 24h, the water extract particles are evenly sprayed into the embedding solution, and placed at 50-60°C for drying for 1h. The core material: wall material in the embedding process is 1:6, and the embedding solution includes a mixed solution of dextrin, gum arabic, sodium bicarbonate, and water in a mass ratio of 1:3:6:90. The embedding conditions are a spraying speed of 3-5kg / min, a stirring rate of 5000r / min, a stirring time of 15min, and microwave drying until the moisture content is less than 10%, and the microwave drying power is 1200W to obtain water extract dry particles;

[0029] Step 4: Grind the dry particles of the water extract into coarse powder with a particle size not exceeding 1 mm, then grind the coarse powder into fine powder with a particle size not exceeding 200 μm, and then ultrafine grind the fine powder into ultrafine Polygonum multiflorum powder with a particle size not exceeding 20 μm.

[0030] <Example 2>

[0031] The method for preparing superfine powder of Polygonum multiflorum comprises:

[0032] Step 1: Wash the raw material of Polygonum multiflorum, remove impurities, dry it, and slice it;

[0033] Step 2: soak the Polygonum multiflorum in a 40% sucrose solution for 45 minutes, rinse and drain, soak the Polygonum multiflorum in drinking water at a ratio of 10kg / 40L, boil and keep for 45 minutes, filter to obtain a Polygonum multiflorum water extract and a Polygonum multiflorum water extract residue, and soak the Polygonum multiflorum water extract residue in drinking water at a ratio of 10kg / 20L, boil and keep for 40 minutes, filter to obtain a Polygonum multiflorum water extract and a Polygonum multiflorum water extract residue;

[0034] Step three, combining the water extracts, concentrating under reduced pressure rotary evaporation at 60-80°C to obtain an extract, vacuum drying, the vacuum drying conditions are 50-60°C, the vacuum degree is 10-20kPa, the drying time is 24h, the water extract particles are evenly sprayed into the embedding solution, and placed at 50-60°C for drying for 2h. The core material: wall material in the embedding process is 1:6, and the embedding solution includes a mixed solution of dextrin, gum arabic, sodium bicarbonate, and water in a mass ratio of 1:3:6:90. The embedding conditions are a spraying speed of 3-5kg / min, a stirring rate of 5000r / min, a stirring time of 20min, and microwave drying until the moisture content is less than 10%, and the microwave drying power is 1200W to obtain water extract dry particles;

[0035] Step 4: Grind the dry particles of the water extract into coarse powder with a particle size not exceeding 1 mm, then grind the coarse powder into fine powder with a particle size not exceeding 200 μm, and then ultrafine grind the fine powder into ultrafine Polygonum multiflorum powder with a particle size not exceeding 20 μm.

[0036] <Example 3>

[0037] The method for preparing superfine powder of Polygonum multiflorum comprises:

[0038] Step 1: Wash the raw material of Polygonum multiflorum, remove impurities, dry it, and slice it;

[0039] Step 2: soak the Polygonum multiflorum in a 45% sucrose solution for 60 minutes, rinse and drain, soak the Polygonum multiflorum in drinking water at a ratio of 10kg / 30L, boil for 60 minutes, filter, and obtain a Polygonum multiflorum water extract and a Polygonum multiflorum water extract residue; and soak the Polygonum multiflorum water extract residue in drinking water at a ratio of 10kg / 20L, boil for 30 minutes, and filter, and obtain a Polygonum multiflorum water extract and a Polygonum multiflorum water extract residue;

[0040] Step three, combining the water extracts, concentrating under reduced pressure rotary evaporation at 60-80°C to obtain an extract, vacuum drying, the vacuum drying conditions are 50-60°C, the vacuum degree is 10-20kPa, the drying time is 24h, the water extract particles are evenly sprayed into the embedding solution, and placed at 50-60°C for drying for 2h. The core material: wall material in the embedding process is 1:6, and the embedding solution includes a mixed solution of dextrin, gum arabic, sodium bicarbonate, and water in a mass ratio of 1:3:6:90. The embedding conditions are a spraying speed of 3-5kg / min, a stirring rate of 5000r / min, a stirring time of 20min, and microwave drying until the moisture content is less than 10%, and the microwave drying power is 1200W to obtain water extract dry particles;

[0041] Step 4: Grind the dry particles of the water extract into coarse powder with a particle size not exceeding 1 mm, then grind the coarse powder into fine powder with a particle size not exceeding 200 μm, and then ultrafine grind the fine powder into ultrafine Polygonum multiflorum powder with a particle size not exceeding 20 μm.

[0042] <Example 4>

[0043] The method for preparing superfine powder of Polygonum multiflorum comprises:

[0044] Step 1: Wash the raw material of Polygonum multiflorum, remove impurities, dry it, and slice it;

[0045] Step 2: soak the Polygonum multiflorum in a 35% sucrose solution for 40 minutes, rinse and drain, soak the Polygonum multiflorum in drinking water at a ratio of 10kg / 35L, boil and keep for 40 minutes, filter to obtain a Polygonum multiflorum water extract and a Polygonum multiflorum water extract residue, and soak the Polygonum multiflorum water extract residue in drinking water at a ratio of 10kg / 15L, boil and keep for 20 minutes, filter to obtain a Polygonum multiflorum water extract and a Polygonum multiflorum water extract residue;

[0046] Step three, combining the water extracts, concentrating under reduced pressure rotary evaporation at 60-80°C to obtain an extract, vacuum drying, the vacuum drying conditions are 50-60°C, the vacuum degree is 10-20kPa, the drying time is 24h, the water extract particles are evenly sprayed into the embedding solution, and placed at 50-60°C for drying for 1h. The core material: wall material in the embedding process is 1:6, and the embedding solution includes a mixed solution of dextrin, gum arabic, sodium bicarbonate, and water in a mass ratio of 1:3:6:90. The embedding conditions are a spraying speed of 3-5kg / min, a stirring rate of 5000r / min, a stirring time of 15min, and microwave drying until the moisture content is less than 10%, and the microwave drying power is 1200W to obtain water extract dry particles;

[0047] Step 4: Combine the water-extracted residues, place them at 60-80° C. and 30-50 kPa for 45 minutes, crush them to a particle size of no more than 1 cm, then keep them at below -18° C. and 10-20 kPa for 4 hours, then transfer them to 60-80° C. and 30-50 kPa for 4 hours, crush them into particles, and microwave dry them until the moisture content is less than 10%. The microwave drying power is 1200 W, and dry particles of water-extracted residues are obtained;

[0048] Step 5: Combine the dry particles of the water extract and the dry particles of the water extract residue, and grind them into coarse powder with a particle size not exceeding 1 mm, then grind the coarse powder into fine powder with a particle size not exceeding 200 μm, and then ultrafinely grind the fine powder into ultrafine Polygonum multiflorum powder with a particle size not exceeding 20 μm.

[0049] <Example 5>

[0050] The method for preparing superfine powder of Polygonum multiflorum comprises:

[0051] Step 1: Wash the raw material of Polygonum multiflorum, remove impurities, dry it, and slice it;

[0052] Step 2: soak the Polygonum multiflorum in a 40% sucrose solution for 45 minutes, rinse and drain, soak the Polygonum multiflorum in drinking water at a ratio of 10kg / 40L, boil and keep for 45 minutes, filter to obtain a Polygonum multiflorum water extract and a Polygonum multiflorum water extract residue, and soak the Polygonum multiflorum water extract residue in drinking water at a ratio of 10kg / 20L, boil and keep for 40 minutes, filter to obtain a Polygonum multiflorum water extract and a Polygonum multiflorum water extract residue;

[0053] Step three, combining the water extracts, concentrating under reduced pressure rotary evaporation at 60-80°C to obtain an extract, vacuum drying, the vacuum drying conditions are 50-60°C, the vacuum degree is 10-20kPa, the drying time is 24h, the water extract particles are evenly sprayed into the embedding solution, and placed at 50-60°C for drying for 2h. The core material: wall material in the embedding process is 1:6, and the embedding solution includes a mixed solution of dextrin, gum arabic, sodium bicarbonate, and water in a mass ratio of 1:3:6:90. The embedding conditions are a spraying speed of 3-5kg / min, a stirring rate of 5000r / min, a stirring time of 20min, and microwave drying until the moisture content is less than 10%, and the microwave drying power is 1000-1200W to obtain water extract dry particles;

[0054] Step 4: Combine the water-extracted residues, place them at 60-80° C. and 30-50 kPa for 60 minutes, crush them to a particle size of no more than 1 cm, then keep them at below -18° C. and 10-20 kPa for 5 hours, then transfer them to 60-80° C. and 30-50 kPa for 5 hours, crush them into particles, and microwave dry them until the moisture content is less than 10%. The microwave drying power is 1200 W, and dry particles of water-extracted residues are obtained;

[0055] Step 5: Combine the dry particles of the water extract and the dry particles of the water extract residue, and grind them into coarse powder with a particle size not exceeding 1 mm, then grind the coarse powder into fine powder with a particle size not exceeding 200 μm, and then ultrafinely grind the fine powder into ultrafine Polygonum multiflorum powder with a particle size not exceeding 20 μm.

[0056] <Example 6>

[0057] The method for preparing superfine powder of Polygonum multiflorum comprises:

[0058] Step 1: Wash the raw material of Polygonum multiflorum, remove impurities, dry it, and slice it;

[0059] Step 2: soak the Polygonum multiflorum in a 45% sucrose solution for 60 minutes, rinse and drain, soak the Polygonum multiflorum in drinking water at a ratio of 10kg / 30L, boil for 60 minutes, filter, and obtain a Polygonum multiflorum water extract and a Polygonum multiflorum water extract residue; and soak the Polygonum multiflorum water extract residue in drinking water at a ratio of 10kg / 20L, boil for 30 minutes, and filter, and obtain a Polygonum multiflorum water extract and a Polygonum multiflorum water extract residue;

[0060] Step three, combining the water extracts, concentrating under reduced pressure rotary evaporation at 60-80°C to obtain an extract, vacuum drying, the vacuum drying conditions are 50-60°C, the vacuum degree is 10-20kPa, the drying time is 24h, the water extract particles are evenly sprayed into the embedding solution, and placed at 50-60°C for drying for 2h. The core material: wall material in the embedding process is 1:6, and the embedding solution includes a mixed solution of dextrin, gum arabic, sodium bicarbonate, and water in a mass ratio of 1:3:6:90. The embedding conditions are a spraying speed of 3-5kg / min, a stirring rate of 5000r / min, a stirring time of 20min, and microwave drying until the moisture content is less than 10%, and the microwave drying power is 1000-1200W to obtain water extract dry particles;

[0061] Step 4: Combine the water-extracted residues, place them at 60-80° C. and 30-50 kPa for 60 minutes, crush them to a particle size of no more than 1 cm, then keep them at below -18° C. and 10-20 kPa for 6 hours, then transfer them to 60-80° C. and 30-50 kPa for 6 hours, crush them into particles, and microwave dry them until the moisture content is less than 10%. The microwave drying power is 1200 W, and the water-extracted residue dry particles are obtained;

[0062] Step 5: Combine the dry particles of the water extract and the dry particles of the water extract residue, and grind them into coarse powder with a particle size not exceeding 1 mm, then grind the coarse powder into fine powder with a particle size not exceeding 200 μm, and then ultrafinely grind the fine powder into ultrafine Polygonum multiflorum powder with a particle size not exceeding 20 μm.

[0063] <Comparative Example 1>

[0064] The method for preparing superfine powder of Polygonum multiflorum comprises:

[0065] Step 1: Wash the raw material of Polygonum multiflorum, remove impurities, dry it, and slice it;

[0066] Step 2: soak the Polygonum multiflorum in a 45% sucrose solution for 60 minutes, rinse and drain, soak the Polygonum multiflorum in drinking water at a ratio of 10kg / 30L, boil for 60 minutes, filter, and obtain a Polygonum multiflorum water extract and a Polygonum multiflorum water extract residue; and soak the Polygonum multiflorum water extract residue in drinking water at a ratio of 10kg / 20L, boil for 30 minutes, and filter, and obtain a Polygonum multiflorum water extract and a Polygonum multiflorum water extract residue;

[0067] Step 3, combining the water extracts, concentrating them by rotary evaporation at 60-80° C. to obtain an extract, vacuum drying them at 50-60° C., a vacuum degree of 10-20 kPa, and a drying time of 24 h to obtain water extract particles, and microwave drying them until the moisture content is less than 10%, and the microwave drying power is 1200 W to obtain water extract dry particles;

[0068] Step 4: Grind the dry particles of the water extract into coarse powder with a particle size not exceeding 1 mm, then grind the coarse powder into fine powder with a particle size not exceeding 200 μm, and then ultrafine grind the fine powder into ultrafine Polygonum multiflorum powder with a particle size not exceeding 20 μm.

[0069] <Comparative Example 2>

[0070] The method for preparing superfine powder of Polygonum multiflorum comprises:

[0071] Step 1: Wash the raw material of Polygonum multiflorum, remove impurities, dry it, and slice it;

[0072] Step 2: soak the Polygonum multiflorum in a 45% sucrose solution for 60 minutes, rinse and drain, soak the Polygonum multiflorum in drinking water at a ratio of 10kg / 30L, boil for 60 minutes, filter, and obtain a Polygonum multiflorum water extract and a Polygonum multiflorum water extract residue; and soak the Polygonum multiflorum water extract residue in drinking water at a ratio of 10kg / 20L, boil for 30 minutes, and filter, and obtain a Polygonum multiflorum water extract and a Polygonum multiflorum water extract residue;

[0073] Step 3, combining the water extracts, concentrating under reduced pressure rotary evaporation at 60-80°C to obtain an extract, vacuum drying, the vacuum drying conditions are 50-60°C, the vacuum degree is 10-20kPa, the drying time is 24h, the water extract particles are evenly sprayed into the embedding solution, placed at 50-60°C for drying for 2h, the core material: wall material in the embedding process is 1:6, the embedding solution is a 2wt.% dextrin aqueous solution, the embedding conditions are a spraying speed of 3-5kg / min, a stirring rate of 5000r / min, a stirring time of 20min, microwave drying until the moisture content is less than 10%, and the microwave drying power is 1200W to obtain water extract dry particles;

[0074] Step 4: Grind the dry particles of the water extract into coarse powder with a particle size not exceeding 1 mm, then grind the coarse powder into fine powder with a particle size not exceeding 200 μm, and then ultrafine grind the fine powder into ultrafine Polygonum multiflorum powder with a particle size not exceeding 20 μm.

[0075] <Comparative Example 3>

[0076] The method for preparing superfine powder of Polygonum multiflorum comprises:

[0077] Step 1: Wash the raw material of Polygonum multiflorum, remove impurities, dry it, and slice it;

[0078] Step 2: soak the Polygonum multiflorum in a 45% sucrose solution for 60 minutes, rinse and drain, soak the Polygonum multiflorum in drinking water at a ratio of 10kg / 30L, boil for 60 minutes, filter, and obtain a Polygonum multiflorum water extract and a Polygonum multiflorum water extract residue; and soak the Polygonum multiflorum water extract residue in drinking water at a ratio of 10kg / 20L, boil for 30 minutes, and filter, and obtain a Polygonum multiflorum water extract and a Polygonum multiflorum water extract residue;

[0079] Step three, combining the water extracts, concentrating under reduced pressure rotary evaporation at 60-80°C to obtain an extract, vacuum drying, the vacuum drying conditions are 50-60°C, the vacuum degree is 10-20kPa, the drying time is 24h, the water extract particles are evenly sprayed into the embedding solution, and placed at 50-60°C for drying for 2h. The core material: wall material in the embedding process is 1:6, and the embedding solution includes a mixed solution of dextrin, gum arabic, sodium bicarbonate, and water in a mass ratio of 1:3:6:90. The embedding conditions are a spraying speed of 3-5kg / min, a stirring rate of 5000r / min, a stirring time of 20min, and microwave drying until the moisture content is less than 10%, and the microwave drying power is 1000-1200W to obtain water extract dry particles;

[0080] Step 4, combining the water-extracted residues, placing them at 60-80° C. and 30-50 kPa for 60 min, crushing them to a particle size of no more than 1 cm, crushing them into particles, and drying them with microwaves until the moisture content is less than 10%, with a microwave drying power of 1200 W, to obtain water-extracted residue dry particles;

[0081] Step 5: Combine the dry particles of the water extract and the dry particles of the water extract residue, and grind them into coarse powder with a particle size not exceeding 1 mm, then grind the coarse powder into fine powder with a particle size not exceeding 200 μm, and then ultrafinely grind the fine powder into ultrafine Polygonum multiflorum powder with a particle size not exceeding 20 μm.

[0082] <Content Identification of the Active Ingredients in Polygonum multiflorum>

[0083] 1. The active ingredients of Polygonum multiflorum are anthraquinone and diphenylethylene glycosides. Anthraquinone is divided into bound anthraquinone and free anthraquinone, mainly bound and free rhamnosin and rhamnosin methyl ether. Diphenylethylene glycosides are mainly 2,3,5,4-tetrahydroxydiphenylethylene-2-O-β-D-glucoside, which can be determined by HPLC.

[0084] (1) Determination of anthraquinone content

[0085] Chromatographic conditions: ZORBAX SB-C 18 Chromatographic column, mobile phase methanol-0.1% phosphoric acid solution (80:20), flow rate 1.0 mL / min, column temperature 30°C, injection volume 10 μL, detection wavelength 254 nm.

[0086] Preparation of reference solution: Take 3 mg and 2 mg of the reference substance of rheum officinale and rheum officinale methyl ether respectively, which are dried to constant weight, accurately weighed, and diluted to 10 mL with methanol to obtain a mixed solution containing 300 μg / 1 mL of rheum officinale and 200 μg / 1 mL of rheum officinale methyl ether for use. Dilute the mixed reference solution of rheum officinale and rheum officinale methyl ether to concentrations of 150 μg / mL, 75 μg / mL, 30 μg / mL, 15 μg / mL, 1 μg / mL, 100 μg / mL, 50 μg / mL, 20 μg / mL, and 10 μg / mL, and determine according to the chromatographic conditions. Draw the rheum officinale standard curve and the mixed rheum officinale methyl ether standard curve with the peak area as the ordinate and the concentration as the abscissa.

[0087] Preparation of test solution: Take 1g of raw Polygonum multiflorum powder (passed through No. 4 sieve), Polygonum multiflorum superfine powder prepared in Example 3 and Comparative Example 1-2, place them in a 50mL stoppered conical flask, accurately add 50mL of methanol, weigh the mass, heat and reflux for 1h, cool to room temperature, weigh the weight again, make up with methanol, let stand, and take 5mL of the filtrate as test solution A (for measuring free anthraquinone). Another 25 mL of filtrate was precisely measured and placed in a stoppered conical flask, evaporated in a water bath, accurately added with 8% hydrochloric acid solution and ultrasonically treated for 5 min, 20 mL of chloroform was added, heated and refluxed in a water bath for 1 h, taken out, immediately cooled, placed in a separatory funnel, and the container was washed with chloroform in small amounts for multiple times, and the washing liquid was added to the separatory funnel, and the chloroform solution was separated, and the acid solution was extracted with chloroform by shaking for 3 times, 15 mL each time, and the chloroform solution was combined, and the solvent was recovered to dryness, and the residue was dissolved with methanol, transferred to a 10 mL volumetric flask, and methanol was added to the volume, shaken, filtered, and the filtrate was taken as the test solution B (for measuring total anthraquinone). The measurement results are shown in Table 1.

[0088] (2) Determination of the content of diphenylethylene glycosides

[0089] Chromatographic conditions: ZORBAX SB-C 18Chromatographic column, mobile phase acetonitrile-water (20:80), flow rate 1.0 mL / min, column temperature 30 °C, injection volume 10 μL, detection wavelength 320 nm.

[0090] Preparation of reference solution: Take 5 mg of 2,3,5,4'-tetrahydroxystilbene-2-O-β-D-glucoside reference substance dried to constant weight, add ethanol to 10 mL, and obtain a 0.5 mg / l mL solution for use. Dilute to 250 μg / mL, 125 μg / mL, 25 μg / mL, and 1 μg / mL in sequence, and determine according to chromatographic conditions. Draw a standard curve with peak area as the ordinate and concentration as the abscissa.

[0091] Preparation of the test solution: Take 0.2 g of raw Polygonum multiflorum powder (passed through a No. 4 sieve), Example 3, and the Polygonum multiflorum superfine powder prepared in Comparative Examples 1-2, place them in a 50 mL stoppered conical flask, accurately add 25 mL of ethanol, weigh the mass, heat and reflux for 30 min, cool to room temperature, weigh the weight again, make up with ethanol, let stand, take the filtrate, pass it through a 0.45 μm microporous filter membrane, and obtain the measurement results as shown in Table 1.

[0092] Table 1

[0093]

[0094] Anthraquinone and diphenylethylene glycosides in Polygonum multiflorum are considered to be its main active ingredients. During the preparation of ultrafine powder, the contents of bound anthraquinone and diphenylethylene glycosides decreased, while the content of free anthraquinone increased. This may be due to the conversion of bound anthraquinone into free anthraquinone. The decrease in the content of diphenylethylene glycosides may be due to structural destruction and conversion into other substances (cis-diphenylethylene glycosides or hydrolysis into aglycones).

[0095] Anthraquinone and diphenylethylene glycosides are the active ingredients of Polygonum multiflorum, and may also be its adverse reactions or toxic ingredients. Combined anthraquinone is the combination of free anthraquinone and glycosides. In the process of preparing ultrafine powder, free anthraquinone and sugar are generated. The laxative effect and hepatotoxicity of combined anthraquinone are greater than those of free anthraquinone. The changes in the content of combined anthraquinone and diphenylethylene glycosides may reduce its harshness and reduce side effects, thereby making the medicinal properties of Polygonum multiflorum mild and achieving the effect of increasing efficacy and reducing toxicity.

[0096] 2. The content of lecithin can be determined by photometer.

[0097] Preparation of phosphorus standard solution: Take 0.136 g of potassium dihydrogen phosphate dried to constant weight, add water to make up to 100 mL as the phosphorus stock solution, take 1.0 mL of the phosphorus stock solution and dilute to 10 mL to obtain the phosphorus standard solution.

[0098] Preparation of color developer: Solution A: Take 1.25g of ammonium molybdate and 4.1g of anhydrous sodium acetate dried to constant weight, dissolve in distilled water, and dilute to 500mL. Solution B: 10% ascorbic acid aqueous solution. Mix solution A and solution B in a ratio of 9:1.

[0099] Preparation of standard curve: Accurately pipette 0.05, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6mL of phosphorus standard solution into 10mL stoppered colorimetric tubes, add 1.2mL of 2.5mol / L sulfuric acid solution, 0.8mL of 10% hydrochloric acid, and then add 4.0mL of color developer, and finally add water to the scale, shake well, boil in water bath for 5min, adjust to zero with reagent blank after cooling, and measure absorbance at 820nm. Plot a curve with phosphorus mass as the horizontal axis and absorbance as the vertical axis to obtain a linear regression equation.

[0100] Preparation of test solution: Take 2g of the ultrafine powder of Polygonum multiflorum prepared in Examples 3, 6 and Comparative Example 3, accurately add 20mL of chloroform-methanol (2:1) solvent, ultrasonically extract for 35min, make up for the weight loss after cooling, and take the subsequent filtrate. Accurately draw 2mL of the subsequent filtrate and place it in a crucible in a water bath to evaporate the solvent, ash it in a muffle furnace at 600℃ for about 1h, dissolve the residue with 1mL of 10% hydrochloric acid, and transfer it to a 5mL volumetric flask. Accurately draw 2mL in a 10mL stoppered colorimetric tube, add 1.2ml of 2.5mol / L sulfuric acid solution and 4.0ml of color developer, and finally add water to the scale, shake well, heat in boiling water for 5min, and measure the absorbance at 820nm. The measurement results are shown in Table 2.

[0101] Table 2

[0102] Group Lecithin content (mg / g) Example 3 0.1520 Example 6 0.2076 Comparative Example 3 0.1739

[0103] The lecithin component of Polygonum multiflorum has the effect of lowering serum cholesterol. The content of lecithin in the water-extracted residue cannot be ignored. In the process of preparing ultrafine powder, retaining the water-extracted residue and performing dehumidification and embrittlement treatment can increase the cell wall breaking rate of Chinese medicinal materials and improve the release of lecithin.

[0104] <Storage test of Polygonum multiflorum ultrafine powder>

[0105] The ultrafine powder of Polygonum multiflorum prepared in Examples 1-6 of the present invention has uniform particle size distribution, large specific surface area and porosity. The powder is dry and loose and can be completely dissolved in water or alcohol solution. After being sealed and stored in an environment of 20-30° C. and 40-50% humidity for 9 months, the total number of bacteria (CFU / g) was determined. The ultrafine powder of Polygonum multiflorum prepared in Examples 1-6 of the present invention had no moisture absorption and agglomeration phenomenon, and no bacteria were detected.

[0106] The number of devices and processing scales described here are used to simplify the description of the present invention. Applications, modifications and variations of the present invention will be obvious to those skilled in the art.

[0107] Although the embodiments of the present invention have been disclosed as above, they are not limited to the applications listed in the specification and the implementation modes, and they can be fully applied to various fields suitable for the present invention. For those familiar with the art, additional modifications can be easily implemented. Therefore, without departing from the general concept defined by the claims and the scope of equivalents, the present invention is not limited to the specific details and the details shown and described herein.

Claims

1. Preparation method of Polygonum multiflorum superfine powder, It is characterized in that include: Step 1: Wash the raw material of Polygonum multiflorum, remove impurities, dry it, and slice it; Step 2: soak the Polygonum multiflorum in a 30-50% sucrose solution for 40-60 minutes, rinse and drain, soak the Polygonum multiflorum in drinking water at a ratio of 10 kg / 30-50 L, boil and keep for 40-60 minutes, filter to obtain a Polygonum multiflorum water extract and a Polygonum multiflorum water extract residue, and soak the Polygonum multiflorum water extract residue in drinking water at a ratio of 10 kg / 10-20 L, boil and keep for 20-40 minutes, filter to obtain a Polygonum multiflorum water extract and a Polygonum multiflorum water extract residue; Step 3, combining the water extracts, concentrating under reduced pressure rotary evaporation at 60-80°C to obtain an extract, vacuum drying to obtain water extract particles, and spraying the embedding solution evenly, wherein the core material: wall material in the embedding process is 1:6, and the embedding solution includes a mixed solution of dextrin, gum arabic, sodium bicarbonate, and water in a mass ratio of 1:3:6:90, placing the mixture at 50-60°C for 1-2h, and microwave drying until the moisture content is less than 10%, to obtain water extract dry particles; Step 4: Combine the water-extracted residues, place them at 60-80°C and 30-50 kPa for 40-60 minutes, crush them to a particle size of no more than 1 cm, then keep them at below -18°C and 10-20 kPa for 4-6 hours, then transfer them to 60-80°C and 30-50 kPa for 4-6 hours, crush them into particles, and microwave dry them until the moisture content is less than 10%, thereby obtaining dry particles of water-extracted residues; Step 5: Combine the dry particles of the water extract and the dry particles of the water extract residue, and grind them into coarse powder with a particle size not exceeding 1 mm, then grind the coarse powder into fine powder with a particle size not exceeding 200 μm, and then ultrafinely grind the fine powder into ultrafine Polygonum multiflorum powder with a particle size not exceeding 20 μm.

2. The method for preparing the superfine powder of Polygonum multiflorum as claimed in claim 1, It is characterized in that The vacuum drying conditions are 50~60℃, the vacuum degree is 10~20kPa, and the drying time is 24h.

3. The method for preparing the superfine powder of Polygonum multiflorum as claimed in claim 1, It is characterized in that The embedding conditions are as follows: a spraying speed of 3-5 kg / min, a stirring rate of 5000 r / min, and a stirring time of 15-20 min.

4. The method for preparing the superfine powder of Polygonum multiflorum according to claim 1, It is characterized in that The power of microwave drying is 1000~1200W.

5. The superfine powder of Polygonum multiflorum obtained by the preparation method according to any one of claims 1 to 4.

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