CN103463211A - Sugar-free prepared multiflower knotweed tuber granules, preparation method and quality control method thereof - Google Patents
Sugar-free prepared multiflower knotweed tuber granules, preparation method and quality control method thereof Download PDFInfo
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- CN103463211A CN103463211A CN2013104230262A CN201310423026A CN103463211A CN 103463211 A CN103463211 A CN 103463211A CN 2013104230262 A CN2013104230262 A CN 2013104230262A CN 201310423026 A CN201310423026 A CN 201310423026A CN 103463211 A CN103463211 A CN 103463211A
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Abstract
The invention discloses sugar-free prepared multiflower knotweed tuber granules, which are prepared from 5 to 15 parts by weight of prepared multiflower knotweed tuber extract, 5 to 15 parts by weight of mannitol, 20 to 40 parts by weight of lactose and 0.05 to 0.25 part by weight of acesulfame potassium. Meanwhile, the present invention also discloses a preparation method and a quality control method for the sugar-free prepared multiflower knotweed tuber granules. The granules are stable and controllable in quality, and have the advantage of convenience in storage, transportation, carrying and administration compared with the traditional decoction. The granules are good in mouthfeel and high in patient compliance, can be used by patients of diabetes, obesity, dental caries and the like in the absence of sucrose, and have a wide application prospect.
Description
Technical field
The present invention relates to the Chinese medicine preparation technical field, relate in particular to a kind of Sugarless type Radix Polygoni Multiflori Preparata granule, preparation method and method of quality control thereof.
Background technology
The Preparation process product that Radix Polygoni Multiflori Preparata is Radix Polygoni Multiflori, have invigorating the liver and kidney, benefiting essence-blood, black beard and hair, bone and muscle strengthening, change the effect of turbid blood fat reducing, for blood deficiency and yellow complexion, dizzy ear toot, early whitening of beard and hair, soreness of the waist and knees, numb limbs and tense tendons, bleeding not during menses, hyperlipemia.The method of tradition application Radix Polygoni Multiflori Preparata is mainly Chinese medicine decoction, use to carry and store inconvenience, and the bitterness of decoction also can reduce patient's compliance, thereby limit the application and development of Radix Polygoni Multiflori Preparata.The exploitation that develops into Radix Polygoni Multiflori Preparata of Chinese medicine granules provides condition, but, exist at present some problems in the Chinese medicine granules preparation method, as adopted the traditional static boiling, extract, extraction ratio is not high, also can make some effective ingredient and steam azeotropic distillation cause the loss of composition; Traditional excipient problem is also more, and the moisture absorption as easy as sucrose makes the granule produced unstable, and the patient such as diabetes, obesity, dental caries should not take.It is not satisfactory etc. that dextrin and starch rush dissolubility.
Summary of the invention
The object of the invention is to overcome existing Radix Polygoni Multiflori Preparata preparation and be not suitable for the patients such as diabetes obesity, dental caries and take, a kind of preparation method of Sugarless type Radix Polygoni Multiflori Preparata granule stable and controllable for quality is provided; The present invention also aims to provide a kind of method of quality control of Sugarless type Radix Polygoni Multiflori Preparata granule.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
Granule of the present invention is prepared from by the following method:
According to listed as parts by weight, Radix Polygoni Multiflori Preparata granule of the present invention is to be prepared from by Radix Polygoni Multiflori Preparata extractum 5-15 part, mannitol 5-15 part, lactose 20-40 part, acesulfame potassium 0.05-0.25 part.
As preferred technical scheme, above-mentioned Radix Polygoni Multiflori Preparata granule is to be prepared from by 0.1 part of 10 parts of Radix Polygoni Multiflori Preparata extractum, 10 parts, mannitol, 29.9 parts of lactose, acesulfame potassium.
Above-mentioned Radix Polygoni Multiflori Preparata process for producing granula: get Radix Polygoni Multiflori Preparata extractum, mannitol, lactose, acesulfame potassium mix homogeneously, add the ethanol soft material processed of 95wt%, 16 eye mesh screen sieve series grains for soft material, drying, the screening of 10 orders and 65 order mesh screens, packing and get final product.
Above-mentioned Radix Polygoni Multiflori Preparata extractum is made like this: get the Radix Polygoni Multiflori Preparata medical material, pulverize, the ethanol that adds respectively the 20%-70% of 2-12 times of weight, under the condition of 20 ℃-90 ℃, extract 30 minutes-120 minutes, extract 1-3 time, filter, merging filtrate, filtrate is concentrated into the thick paste that relative density is 1.25-1.35 and get final product.
As preferred technical scheme, above-mentioned preparation method is: get the Radix Polygoni Multiflori Preparata medical material, pulverize, the ethanol that adds respectively the 30%-50% of 6-8 times of weight, under the condition of 60 ℃-80 ℃, extract 70 minutes-90 minutes, extract 2-3 time, filter, merging filtrate, filtrate is concentrated into the thick paste that relative density is 1.27-1.33 and get final product
As optimum technical scheme, above-mentioned preparation method is: get the Radix Polygoni Multiflori Preparata medical material, pulverize, add respectively 40% ethanol of 7 times of weight, under the condition of 70 ℃, extract 80 minutes, extract 2 times, filter, merging filtrate, filtrate is concentrated into the thick paste that relative density is 1.30 and get final product.
Method of quality control of the present invention is achieved by the following technical solution:
Qualitative identification (according to thin layer chromatography): get the Radix Polygoni Multiflori Preparata granule and put in right amount in flask, add ethanol 20mL, reflux 50min, filter, and filtrate is concentrated into 1mL as need testing solution; Except Radix Polygoni Multiflori Preparata, prepare granule by the technique of Radix Polygoni Multiflori Preparata granule, press the need testing solution preparation method, prepare the Radix Polygoni Multiflori negative controls; Get the Radix Polygoni Multiflori control medicinal material appropriate, put in flask, add ethanol 20mL, reflux 50min, make solution, filters, and filtrate is concentrated into 1mL medical material solution in contrast.Get respectively each 5 μ L of above-mentioned 3 kinds of solution, put respectively in same and take on the silica gel H lamellae that sodium carboxymethyl cellulose is adhesive, launch 6-7:5-6:1.0-1.5:0.5-1.0 the upper solution of ethyl acetate-acetone-water-toluene mixed solution is developing solvent, take out, dry.Under the 365nm uviol lamp, inspection is known, and in the test sample chromatograph with on reference substance chromatograph relevant position, the speckle of same color occurs, and negative control is noiseless.
Assay (according to high performance liquid chromatography): get the Radix Polygoni Multiflori Preparata granule appropriate, put in tool plug conical flask, add Diluted Alcohol 25mL, supersound extraction 30min, let cool, supply the weight of less loss with Diluted Alcohol, shake up, microporous filter membrane for supernatant (0.45 μ m) filters, and obtains need testing solution.The Diluted Alcohol solution of stilbene glucoside of take is contrast, uses the octadecylsilane chemically bonded silica post, and the 15-35:65:-85 acetonitrile-water is mobile phase, and 10 ℃-50 ℃ of column temperatures detect wavelength 320nm.Every 1 gram finished particle is not less than 2.1-3.1mg containing the amount of stilbene glucoside.
As preferred technical scheme, above-mentioned method of quality control is:
Qualitative identification (according to thin layer chromatography): get the Radix Polygoni Multiflori Preparata granule and put in right amount in flask, add ethanol 20mL, reflux 50min, filter, and filtrate is concentrated into 1mL as need testing solution; Except Radix Polygoni Multiflori Preparata, prepare granule by the technique of Radix Polygoni Multiflori Preparata granule, press the need testing solution preparation method, prepare the Radix Polygoni Multiflori negative controls; Get the Radix Polygoni Multiflori control medicinal material appropriate, put in flask, add ethanol 20mL, reflux 50min, make solution, filters, and filtrate is concentrated into 1mL medical material solution in contrast.Get respectively each 5 μ L of above-mentioned 3 kinds of solution, put respectively in same and take on the silica gel H lamellae that sodium carboxymethyl cellulose is adhesive, 6.5: 5.5: 1.2: the upper solution of 0.7 ethyl acetate-acetone-water-toluene mixed solution was that developing solvent launches, and takes out, and dries.Under the 365nm uviol lamp, inspection is known, and in the test sample chromatograph, and occurs the speckle of same color on reference substance chromatograph relevant position, and negative control is noiseless.
Assay (according to high performance liquid chromatography): get the Radix Polygoni Multiflori Preparata granule appropriate, put in tool plug conical flask, add Diluted Alcohol 25mL, supersound extraction 30min, let cool, supply the weight of less loss with Diluted Alcohol, shake up, microporous filter membrane for supernatant (0.45 μ m) filters, and obtains need testing solution.The Diluted Alcohol solution of stilbene glucoside of take is contrast, uses the octadecylsilane chemically bonded silica post, and the 25:75 acetonitrile-water is mobile phase, and 30 ℃ of column temperatures detect wavelength 320nm, and every 1 gram finished particle is not less than 2.1-3.1mg containing the amount of stilbene glucoside.
Above-mentioned technology is that the inventor verifies out through the handsome choosing of a large amount of experiments:
The Study on extraction of experiment one, Radix Polygoni Multiflori Preparata
1. instrument and reagent
SPECORD50 type ultraviolet-uisible spectrophotometer (Analytik Jena AG); Thermostat water bath (Shanghai No.5 Medical Equipment Factory); Sai Duolisi BT-25-S electronic analytical balance (Beijing Sai Duolisi instrument system company limited); Stilbene glucoside reference substance (Chinese medicine bioassay institute product, lot number is 0844-200003); Ethanol is analytical pure, the distilled water self-control.Radix Polygoni Multiflori Preparata is purchased from Bozhou City and justice hall Chinese crude drug company.
2. method and result
2.1 the preparation of reference substance solution
Precision takes 5.8mg stilbene glucoside standard substance, uses 95% dissolve with ethanol, and standardize solution, in the 25mL volumetric flask, shakes up product solution in contrast.
2.2 the preparation of Radix Polygoni Multiflori Preparata need testing solution
Take Radix Polygoni Multiflori Preparata powder 10g and be placed in the 250mL round-bottomed flask, add 40% ethanol 70mL, in 70 ℃ of water-baths, heat 1h.Filter, filtrate is placed in the 250mL volumetric flask, uses the distilled water standardize solution, obtains A.Get again the volumetric flask that 5mL is placed in 100mL from A, use the distilled water standardize solution, obtain B.Draw again 5.0mL and be placed in the 50mL volumetric flask from B, with 95% ethanol standardize solution, obtain need testing solution.
2.3 determining of maximum absorption wavelength
Draw the 2.5mL reference substance solution and be placed in the 50mL volumetric flask, with 95% ethanol standardize solution, separately to get the Radix Polygoni Multiflori sample solution and measure absorbance at 300nm～400nm respectively, the two absorption spectrum is basically identical, and all at the 324nm place, absorption maximum is arranged, therefore select 324nm as measuring wavelength.
2.4 stilbene glucoside stability test
Get the Radix Polygoni Multiflori sample solution and measure respectively its absorbance when 0min, 10min, 20min, 30min, 40min, 50min, 60min, 80min/, 100min, 150min, 200min.Result shows, the prolongation in time between 0min～60min of the absorbance of stilbene glucoside descends very fast, but can reach stable after 60min, and RSD=1.15% carries out therefore select 1h after preparation during the mensuration of each sample.
2.5 the drafting of stilbene glucoside standard curve
From reference substance solution, accurately absorption 0.5mL, 1.0mL, 1.5mL, 2.0mL, 2.5mL are placed in the 50mL volumetric flask, with 95% ethanol standardize solution, measure absorbance with ultraviolet-uisible spectrophotometer, obtain stilbene glucoside standard curve regression equation: Y=0.0927x+0.0093, R
2=0.9995.Y is absorbance A, and X is concentration (mg/L).
2.6 the mensuration of precision
Parallel absorption 2mL5 part from sample liquid, be placed in respectively the volumetric flask of 10mL, with 95% ethanol standardize solution.Measure absorbance with ultraviolet-uisible spectrophotometer.Calculate RSD=1.53%, illustrate that precision is good.
2.7 repeatability test
Get respectively 5 parts of each 10g of Radix Polygoni Multiflori powder, accurately weighed, prepare sample solution by the sample solution preparation method, measure absorbance, calculate the RSD=2.17% of absorbance, show favorable reproducibility.
2.8 recovery test
Parallel extracting sample solution 1.0m1 is in the volumetric flask of 6 10mL, add wherein respectively standard stock solution 0.2mL, 0.2mL, 0.3mL, 0.3mL, 0.4mL, 0.4mL, with 95% ethanol standardize solution, measure absorbance with ultraviolet-uisible spectrophotometer, the substitution standard curve calculates the content of stilbene glucoside, calculate recovery rate, average recovery is that 99.27%, RSD is 0.65% as a result.
2.9 Orthogonal Experiment and Design
According to the preliminary experiment result, adopt orthogonal test method to affect 4 larger factors to Extraction technique: temperature (A), time (B), solid-liquid ratio (C), 4 factors of concentration of alcohol (D) are investigated.With L9 (34) orthogonal table arrangement test, factor level and experimental result in Table 1, table 2.
Table 1 orthogonal test factor level
Table 2 orthogonal experiments
Can find out that by the quadrature result each factor affects size to stilbene glucoside extraction ratio in Radix Polygoni Multiflori and is followed successively by: D>A>B>C, in conjunction with the size of data of each factor intuitive analysis K1, K2, K3, determine that the optimum level combination of this experiment is A
3b
3c
2d
1, optimum process condition is: extract temperature 70 C, extraction time is 80min, solid-liquid ratio 1:7, concentration of alcohol 40%.
The screening of experiment two, adjuvant
1. instrument and reagent
Sai Duolisi BT-25-S electronic analytical balance (Beijing Sai Duolisi instrument system company limited); RE-52A type Rotary Evaporators (Shanghai refined flourish biochemical equipment Instrument Ltd.); Radix Polygoni Multiflori Preparata is purchased from Bozhou City and justice hall Chinese crude drug company; Lactose, mannitol, soluble starch, dextrin, beta-schardinger dextrin-all originate from Tianjin and cause chemical reagent company limited far away; 95% ethanol (Tianjin chemical industry all generations company limited)
2. method and result
2.1 producing of extractum:
Take Radix Polygoni Multiflori Preparata medical material 2000g, pulverize, by optimum extraction process, extract and concentrate, the extractum that must obtain relative density 1.30 is stand-by.
2.2 single adjuvant screening:
Get 5 parts of extractum, every part of 10g, mix with dextrin, soluble starch, lactose, beta-schardinger dextrin-, each 30g of mannitol respectively, then, with appropriate 95% ethanol soft material processed, cross 16 mesh sieves and granulate, and No. 1 sieve and No. 4 sieves are crossed in 55 ℃ of oven dry successively, weigh, and calculate ratio of briquetting; Get the about 1g of above-mentioned each finished particle, after 60 ℃ of constant weights, accurately weighed, the close drying device that to be placed in relative humidity be 75%, room temperature is placed 24h, calculates its hydroscopicity.The ratio of briquetting of the granule that different adjuvants is made and moisture absorption percentage rate carry out comprehensive grading, the results are shown in Table 3
Ratio of briquetting and hydroscopicity comprehensive grading table that each adjuvant of table 3 is granulated
As shown in Table 3, lactose, mannitol are high as the grain forming rate of adjuvant, and hygroscopicity is little, and integrate score is high.
2.3 the screening of mixed accessories
Lactose in varing proportions and mannitol form mixed accessories, with Radix Polygoni Multiflori Preparata extractum, under 2.2, are granulated, and measure its ratio of briquetting and hydroscopicity, and carry out comprehensive grading, the results are shown in Table 4, table 5.
The screening table of table 4 mixed accessories
Table 5 mixed accessories ratio of briquetting and hydroscopicity comprehensive grading table
Known when usining mannitol by table 4, table 5: when lactose=1:3 granulates as mixed accessories, ratio of briquetting is high, and hygroscopicity is little, and integrate score is high.
2.4 the screening of extractum and mixed accessories ratio
Using mannitol: lactose=1:3 as mixed accessories, granulated under 2.2 with Radix Polygoni Multiflori Preparata extractum, measure its ratio of briquetting and hydroscopicity, and carry out comprehensive grading, the preferred weight ratio of mixed accessories and Radix Polygoni Multiflori Preparata extractum, the results are shown in Table 6, table 7.
The screening table of table 6 extractum and mixed accessories ratio
| Tested number | 1 | 2 | 3 |
| Radix Polygoni Multiflori Preparata extractum g | 10 | 10 | 10 |
| Mixed accessories g | 30 | 40 | 50 |
The screening comprehensive grading table of table 7 extractum and mixed accessories ratio
From table 6, table 7, extractum: mixed accessories=1:4 and extractum: total points during mixed accessories=1:5 is apparently higher than extractum: score during mixed accessories=1:4, and the ratio phase-splitting difference of extractum: mixed accessories=1:4 and extractum: mixed accessories=1:5 is very little, the consumption of considering pharmacopeia regulation adjuvant can not surpass the extractum of 5 times, so the best proportion of the weight portion of extractum and mixed accessories is extractum: mixed accessories=1:4
2.5 the screening of correctives consumption
In prescription, Radix Polygoni Multiflori Preparata extract has certain bitterness, should add correctives, correctives commonly used has aspartame, acesulfame potassium etc., due to the report that aspartame neurotoxicity and carcinogenecity were once arranged, so the correctives that this experiment is selected is acesulfame potassium, and take mouthfeel as screening index, the results are shown in Table 8.
Table 8 correctives consumption screening table
| Tested number | 0.1％ | 0.2％ | 0.3％ |
| Mouthfeel | Hardship, can not accept | Sweet, micro-hardship, can accept | Sweet, micro-hardship, can accept |
Result shows, the acesulfame potassium consumption is 0.2% to be advisable.
2.6 the formula of Data processing application:
Ratio of briquetting (%)=by No. 1 sieve, can not weigh * 100% by No. 5 sieve granule weight/sample particles
Weight * 100% before moisture absorption percentage rate (%)=(the front weight of weight-moisture absorption after moisture absorption)/moisture absorption
Score=grain forming rate * 30+ (1-moisture absorption percentage rate) * 70 (the grain forming rate accounts for 30 minutes, moisture absorption percentage rate and accounts for 70 minutes, full marks 100 minutes)
Experiment three, method of quality control
1, medical material, reagent and instrument
2, qualitative identification
2.1 thin layer is differentiated: get Radix Polygoni Multiflori Preparata granule 2g and put in flask, add ethanol 20mL, reflux 50min, filter, and filtrate is waved to about 1mL as need testing solution; Press the preparation of Radix Polygoni Multiflori Preparata granule technique not containing the granule of Radix Polygoni Multiflori Preparata, press the need testing solution preparation method, the preparation negative controls; Get Radix Polygoni Multiflori control medicinal material 2g, pulverize and to add ethanol 20mL, reflux 50min, filter, and filtrate is waved the medical material solution in contrast to about 1mL.Get respectively each 5 μ L of above-mentioned 3 kinds of solution, put respectively in same and take on the silica gel H lamellae that sodium carboxymethyl cellulose is adhesive, take ethyl acetate: acetone: water: (6.5: 5.5: 1.2: 0.7) upper solution of mixed solution was that developing solvent launches to toluene, and taking-up is dried.Under the 365nm uviol lamp, inspection is known, and in the test sample chromatograph with on reference substance chromatograph relevant position, the speckle of same color occurs, and negative control is noiseless, the results are shown in Figure 1.
3, assay:
3.1 chromatographic condition
Chromatographic column: HypersilC18 (150mm * 4.6mm); Mobile phase: acetonitrile-water (25:75); Flow velocity: 1.0mL/min; Column temperature: 30 ℃; Detect wavelength: 320nm; Sample size: 10 μ L.
3.2 the preparation of reference substance solution
Precision takes stilbene glucoside reference substance 5.92mg, is placed in the 10mL volumetric flask, with 50% dissolve with ethanol and be settled to scale, obtains the reference substance mother solution.Accurate stilbene glucoside reference substance mother solution 0.5,1.0,1.5,2.0, the 2.5ml of drawing, standardize solution, in the 10mL measuring bottle, obtains respectively reference substance solution A, B, C, D, E.
3.3 the preparation of need testing solution
Accurately weighed fleece-flower root particulate agent 1.16g, precision adds Diluted Alcohol 25mL, weighed weight, supersound extraction 30min, let cool, and supplies the weight of less loss with Diluted Alcohol, shakes up, and microporous filter membrane for supernatant (0.45 μ m) filters, and obtains.
3.4 the preparation of negative control product
Press Radix Polygoni Multiflori Preparata granule prescription and preparation technology's preparation not containing the negative control product of Radix Polygoni Multiflori Preparata, precision takes negative control product 1.02 grams, by " a 3.3 " standby negative control solution of below legal system.
3.5 interference experiment
Draw respectively reference substance solution E, need testing solution, negative control solution 10 μ L and record the elution curve of chromatographic peak under 3.1 conditions, the results are shown in Figure 2,3,4, negative control solution, occurring without chromatographic peak with stilbene glucoside retention time same position, shows measurement result without impact.
3.6 linear relationship is investigated
Essence is got reference substance solution A, B, C, D, each 10 μ L of E, by " 3.1 " lower chromatographic condition, measures.The peak area integrated value (Y) of take is vertical coordinate, and reference substance solution concentration (X), for abscissa carries out linear regression, the results are shown in Figure 5.
3.7, precision test
The accurate molten C10 μ of the reference substance L that draws, repeat sample introduction 6 times by above-mentioned chromatographic condition, measures peak area, the results are shown in Table 9, RSD=1.1% (n=6), shows that precision is good.
Table 9 precision test
3.8, stability test
Get reference substance solution B, respectively at 0,2,4,6,8,12,24,48h is by above-mentioned chromatographic condition sample introduction 10 μ L, measures peak area.The results are shown in Table 10, RSD=0.92% (n=8), show that need testing solution is stable in 48h.
Table 10 stability test
3.9 repeatability test
Precision takes with a collection of fleece-flower root particulate agent, by " 3.3 " lower 6 parts of need testing solutions of the parallel preparation of method, by above-mentioned chromatographic condition sample introduction measuring and calculating.The results are shown in Table 11, RSD=1.7%, show that repeatability is good.
The test of table 11 repeatability
3.10 average recovery test
Essence is got 6 parts of the sample solutions of known content, every part of 10mL, accurately weighed, it is appropriate that precision adds the stilbene glucoside reference substance respectively, makes need testing solution according to " 2.3 " below method, by above-mentioned chromatographic condition, calculate average recovery, the results are shown in Table 12, RSD%=1.1% (n=6), show that average recovery is good.
The test of table 12 average recovery
3.10 sample size is measured
Prescription and preparation technology by the Radix Polygoni Multiflori Preparata granule prepare 5 batches of Radix Polygoni Multiflori Preparata granules, make need testing solution by " 2.3 " below method respectively, sample size 10 μ L, and by above-mentioned chromatographic condition, the content of measuring and calculating stilbene glucoside, the results are shown in Table 13.
The stilbene glucoside content of the different lot number Radix Polygoni Multiflori Preparata of table 13 granule
Granule of the present invention is stable and controllable for quality, with traditional decoction, compares, and has advantages of storage, transports, carries, taking convenience.Granule mouthfeel of the present invention is good, and patient compliance is high, and owing to not adding sucrose, the patients such as diabetes, obesity, dental caries can use, and have a extensive future.
Figure of description
Fig. 1, Radix Polygoni Multiflori Preparata thin layer of particulate are differentiated figure;
The high-efficient liquid phase chromatogram of Fig. 2, reference substance solution E;
The high-efficient liquid phase chromatogram of Fig. 3, need testing solution;
The high-efficient liquid phase chromatogram of Fig. 4, negative control solution;
Fig. 5 reference substance linear relationship chart.
The specific embodiment
Below in conjunction with embodiment, further set forth the present invention.
Embodiment 1: gets the Radix Polygoni Multiflori Preparata medical material, is ground into coarse powder, extract 2 times, add respectively 40% ethanol of 7 times of weight, under the condition of 70 ℃, extract 80 minutes, filter, and merging filtrate, it is standby that filtrate is concentrated into the thick paste that relative density is 1.30.Get mannitol 100g, lactose 299g, acesulfame potassium 1g crosses 100 mesh sieves, mix homogeneously, obtain mixed accessories.Get above-mentioned extractum 100g and the mixed accessories of producing and mix, add 95% ethanol soft material processed, 16 eye mesh screen sieve series grains for soft material, drying, 10 orders and the screening of 65 order mesh screens, packing obtains Sugarless type Radix Polygoni Multiflori Preparata granule.
Get above-mentioned granule 2g and put in flask, add ethanol 20mL, reflux 50min, filter, and filtrate is waved to about 1mL as need testing solution; Press the preparation of Radix Polygoni Multiflori Preparata granule technique not containing the granule of Radix Polygoni Multiflori Preparata, press the need testing solution preparation method, the preparation negative controls; Get Radix Polygoni Multiflori control medicinal material 2g, pulverize and to add ethanol 20mL, reflux 50min, filter, and filtrate is waved the medical material solution in contrast to about 1mL.Get respectively each 5 μ L of above-mentioned 3 kinds of solution, put respectively in same and take on the silica gel H lamellae that sodium carboxymethyl cellulose is adhesive, take ethyl acetate: acetone: water: (6.5:5.5: 1.2:0.7) upper solution of mixed solution is that developing solvent launches to toluene, and taking-up is dried.Under the 365nm uviol lamp, inspection is known, and in the test sample chromatograph with on reference substance chromatograph relevant position, the speckle of same color occurs, and negative control is noiseless.
Get above-mentioned granule 1g, put in tool plug conical flask, add Diluted Alcohol 25mL, supersound extraction 30min, let cool, and supplies the weight of less loss with Diluted Alcohol, shakes up, and microporous filter membrane for supernatant (0.45 μ m) filters, and obtains need testing solution.The Diluted Alcohol solution of stilbene glucoside of take is contrast, uses the octadecylsilane chemically bonded silica post, and the 25:75 acetonitrile-water is mobile phase, and 30 ℃ of column temperatures detect wavelength 320nm, and every 1 gram finished particle is not less than 2.1-3.1mg containing the amount of stilbene glucoside.
Embodiment 2: gets the Radix Polygoni Multiflori Preparata medical material, is ground into coarse powder, extract 2 times, add respectively 50% ethanol of 6 times of weight, under the condition of 80 ℃, extract 100 minutes, filter, and merging filtrate, it is standby that filtrate is concentrated into the thick paste that relative density is 1.30.Get mannitol 130g, lactose 269g, acesulfame potassium 1.5g crosses 100 mesh sieves, mix homogeneously, obtain mixed accessories.Get above-mentioned extractum 100g and the mixed accessories of producing and mix, add 95% ethanol soft material processed, 16 eye mesh screen sieve series grains for soft material, drying, 10 orders and the screening of 65 order mesh screens, packing obtains Sugarless type Radix Polygoni Multiflori Preparata granule.
Get above-mentioned granule 2g and put in flask, add ethanol 20mL, reflux 50min, filter, and filtrate is waved to about 1mL as need testing solution; Press the preparation of Radix Polygoni Multiflori Preparata granule technique not containing the granule of Radix Polygoni Multiflori Preparata, press the need testing solution preparation method, the preparation negative controls; Get Radix Polygoni Multiflori control medicinal material 2g, pulverize and to add ethanol 20mL, reflux 50min, filter, and filtrate is waved the medical material solution in contrast to about 1mL.Get respectively each 5 μ L of above-mentioned 3 kinds of solution, put respectively in same and take on the silica gel H lamellae that sodium carboxymethyl cellulose is adhesive, take ethyl acetate: acetone: water: the upper solution of toluene (6.5:5.5:1.2:0.7) mixed solution is that developing solvent launches, and taking-up is dried.Under the 365nm uviol lamp, inspection is known, and in the test sample chromatograph with on reference substance chromatograph relevant position, the speckle of same color occurs, and negative control is noiseless.
Get above-mentioned granule 1g, put in tool plug conical flask, add Diluted Alcohol 25mL, supersound extraction 30min, let cool, and supplies the weight of less loss with Diluted Alcohol, shakes up, and microporous filter membrane for supernatant (0.45 μ m) filters, and obtains need testing solution.The Diluted Alcohol solution of stilbene glucoside of take is contrast, uses the octadecylsilane chemically bonded silica post, and the 25:75 acetonitrile-water is mobile phase, and 30 ℃ of column temperatures detect wavelength 320nm, and every 1 gram finished particle is not less than 2.1-3.1mg containing the amount of stilbene glucoside.
Embodiment 3: gets the Radix Polygoni Multiflori Preparata medical material, is ground into coarse powder, extract 2 times, add respectively 60% ethanol of 8 times of weight, under the condition of 80 ℃, extract 60 minutes, filter, and merging filtrate, it is standby that filtrate is concentrated into the thick paste that relative density is 1.30.Get mannitol 150g, lactose 500g, acesulfame potassium 2g crosses 100 mesh sieves, mix homogeneously, obtain mixed accessories.Get above-mentioned extractum 150g and the mixed accessories of producing and mix, add 95% ethanol soft material processed, 16 eye mesh screen sieve series grains for soft material, drying, 10 orders and the screening of 65 order mesh screens, packing obtains Sugarless type Radix Polygoni Multiflori Preparata granule.
Get Radix Polygoni Multiflori Preparata granule 2g and put in flask, add ethanol 20mL, reflux 50min, filter, and filtrate is waved to about 1mL as need testing solution; Press the preparation of Radix Polygoni Multiflori Preparata granule technique not containing the granule of Radix Polygoni Multiflori Preparata, press the need testing solution preparation method, the preparation negative controls; Get Radix Polygoni Multiflori control medicinal material 2g, pulverize and to add ethanol 20mL, reflux 50min, filter, and filtrate is waved the medical material solution in contrast to about 1mL.Get respectively each 5 μ L of above-mentioned 3 kinds of solution, put respectively in same and take on the silica gel H lamellae that sodium carboxymethyl cellulose is adhesive, take ethyl acetate: acetone: water: the upper solution of toluene (6.5:5.5:1.2:0.7) mixed solution is that developing solvent launches, and taking-up is dried.Under the 365nm uviol lamp, inspection is known, and in the test sample chromatograph with on reference substance chromatograph relevant position, the speckle of same color occurs, and negative control is noiseless
Get above-mentioned granule 1g, put in tool plug conical flask, add Diluted Alcohol 25mL, supersound extraction 30min, let cool, and supplies the weight of less loss with Diluted Alcohol, shakes up, and microporous filter membrane for supernatant (0.45 μ m) filters, and obtains need testing solution.The Diluted Alcohol solution of stilbene glucoside of take is contrast, uses the octadecylsilane chemically bonded silica post, and the 25:75 acetonitrile-water is mobile phase, and 30 ℃ of column temperatures detect wavelength 320nm, and every 1 gram finished particle is not less than 2.1-3.1mg containing the amount of stilbene glucoside.
Claims (8)
1. a Sugarless type Radix Polygoni Multiflori Preparata granule, is characterized in that: by Radix Polygoni Multiflori Preparata extractum 5-15 weight portion, mannitol 5-15 weight portion, lactose 20-40 weight portion, acesulfame potassium 0.05-0.25 weight portion, be prepared from.
2. a kind of Sugarless type Radix Polygoni Multiflori Preparata granule as claimed in claim 1, is characterized in that: by Radix Polygoni Multiflori Preparata extractum 10 weight portions, mannitol 10 weight portions, lactose 29.9 weight portions, acesulfame potassium 0.1 weight portion, be prepared from.
3. a kind of Sugarless type Radix Polygoni Multiflori Preparata granule as claimed in claim 1, it is characterized in that: described Radix Polygoni Multiflori Preparata extractum preparation method is as follows: get the Radix Polygoni Multiflori Preparata medical material, pulverize, the ethanol that adds respectively the 20wt%-70wt% of 2-12 times of weight, under the condition of 20 ℃-90 ℃, extract 30 minutes-120 minutes, extract 1-3 time, filter, merging filtrate, filtrate is concentrated into the thick paste that relative density is 1.25-1.35 and get final product.
4. a kind of Sugarless type Radix Polygoni Multiflori Preparata granule as claimed in claim 3, it is characterized in that: described Radix Polygoni Multiflori Preparata extractum preparation method is as follows: get the Radix Polygoni Multiflori Preparata medical material, pulverize, the ethanol that adds respectively the 30wt%-50wt% of 6-8 times of weight, under the condition of 60 ℃-80 ℃, extract 70 minutes-90 minutes, extract 2-3 time, filter, merging filtrate, filtrate is concentrated into the thick paste that relative density is 1.27-1.33 and get final product.
5. a kind of Sugarless type Radix Polygoni Multiflori Preparata granule as claimed in claim 4, it is characterized in that: described Radix Polygoni Multiflori Preparata extractum preparation method is as follows: get the Radix Polygoni Multiflori Preparata medical material, pulverize, the ethanol that adds respectively the 40wt% of 7 times of weight, under the condition of 70 ℃, extract 80 minutes, extract 2 times, filter, merging filtrate, filtrate is concentrated into the thick paste that relative density is 1.30 and get final product.
6. the method prepared as Sugarless type Radix Polygoni Multiflori Preparata granule as described in claim 1-5 any one, it is characterized in that: step is as follows: get Radix Polygoni Multiflori Preparata extractum, mannitol, lactose, acesulfame potassium mix homogeneously, the ethanol soft material processed that adds 95wt%, 16 eye mesh screen sieve series grains for soft material, dry, the screening of 10 orders and 65 order mesh screens, packing and get final product.
7. the method for quality control as Sugarless type Radix Polygoni Multiflori Preparata granule as described in claim 1-5 any one is characterized in that:
Qualitative identification: adopt according to thin layer chromatography, get the Radix Polygoni Multiflori Preparata granule and put in right amount in flask, add ethanol 20mL, reflux 50min, filter, and filtrate is concentrated into 1mL as need testing solution; Except Radix Polygoni Multiflori Preparata, prepare granule by the technique of Radix Polygoni Multiflori Preparata granule, press the need testing solution preparation method, prepare the Radix Polygoni Multiflori negative controls; Get the Radix Polygoni Multiflori control medicinal material appropriate, put in flask, add ethanol 20mL, reflux 50min, make solution, filters, and filtrate is concentrated into 1mL medical material solution in contrast; Get respectively each 5 μ L of above-mentioned 3 kinds of solution, put respectively in same and take on the silica gel H lamellae that sodium carboxymethyl cellulose is adhesive, 6-7:5-6:1.0-1.5: the upper solution of 0.5-1.0 ethyl acetate-acetone-water-toluene mixed solution is that developing solvent launches, and takes out, and dries; Under the 365nm uviol lamp, inspection is known, and in the test sample chromatograph with on reference substance chromatograph relevant position, the speckle of same color occurs, and negative control is noiseless;
Assay: adopt according to high performance liquid chromatography, get the Radix Polygoni Multiflori Preparata granule appropriate, put in tool plug conical flask, add Diluted Alcohol 25mL, supersound extraction 30min, let cool, supply the weight of less loss with Diluted Alcohol, shake up, supernatant filters with 0.45 μ m microporous filter membrane, need testing solution, the Diluted Alcohol solution of stilbene glucoside of take is contrast, uses the octadecylsilane chemically bonded silica post, the 15-35:65:-85 acetonitrile-water is mobile phase, 10 ℃-50 ℃ of column temperatures, detect wavelength 320nm, and every 1 gram finished particle is not less than 2.1-3.1mg containing the amount of stilbene glucoside.
8. the method for quality control of Sugarless type Radix Polygoni Multiflori Preparata granule as claimed in claim 7 is characterized in that:
Qualitative identification: get the Radix Polygoni Multiflori Preparata granule and put in right amount in flask, add ethanol 20mL, reflux 50min, filter, and filtrate is concentrated into 1mL as need testing solution; Except Radix Polygoni Multiflori Preparata, prepare granule by the technique of Radix Polygoni Multiflori Preparata granule, press the need testing solution preparation method, prepare the Radix Polygoni Multiflori negative controls; Get the Radix Polygoni Multiflori control medicinal material appropriate, put in flask, add ethanol 20mL, reflux 50min, make solution, filters, and filtrate is concentrated into 1mL medical material solution in contrast; Get respectively each 5 μ L of above-mentioned 3 kinds of solution, put respectively in same and take on the silica gel H lamellae that sodium carboxymethyl cellulose is adhesive, the upper solution of 6.5:5.5:1.2:0.7 ethyl acetate-acetone-water-toluene mixed solution is that developing solvent launches, and takes out, and dries; Under the 365nm uviol lamp, inspection is known, and in the test sample chromatograph, and occurs the speckle of same color on reference substance chromatograph relevant position, and negative control is noiseless;
Assay: get the Radix Polygoni Multiflori Preparata granule appropriate, put in tool plug conical flask, add Diluted Alcohol 25mL, supersound extraction 30min, let cool, and supplies the weight of less loss with Diluted Alcohol, shakes up, and supernatant filters with 0.45 μ m microporous filter membrane, obtains need testing solution; The Diluted Alcohol solution of stilbene glucoside of take is contrast, uses the octadecylsilane chemically bonded silica post, and the 25:75 acetonitrile-water is mobile phase, and 30 ℃ of column temperatures detect wavelength 320nm, and every 1 gram finished particle is not less than 2.1-3.1mg containing the amount of stilbene glucoside.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105265955A (en) * | 2015-10-20 | 2016-01-27 | 紫云紫源生物科技有限公司 | Solid Moringa oleifera leaf drink |
| CN109481511A (en) * | 2018-11-20 | 2019-03-19 | 贵州云上苗家康养有限公司 | A kind of RADIX POLYGONI MULTIFLORI PREPARATA sugar-free type granular formulation and preparation method thereof |
| CN109953164A (en) * | 2018-11-20 | 2019-07-02 | 贵州云上苗家康养有限公司 | A kind of preparation method of fleece-flower root beauty treatment mind easing tea |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105265955A (en) * | 2015-10-20 | 2016-01-27 | 紫云紫源生物科技有限公司 | Solid Moringa oleifera leaf drink |
| CN109481511A (en) * | 2018-11-20 | 2019-03-19 | 贵州云上苗家康养有限公司 | A kind of RADIX POLYGONI MULTIFLORI PREPARATA sugar-free type granular formulation and preparation method thereof |
| CN109953164A (en) * | 2018-11-20 | 2019-07-02 | 贵州云上苗家康养有限公司 | A kind of preparation method of fleece-flower root beauty treatment mind easing tea |
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Application publication date: 20131225 |