CN103520359B - Preparation technology for fresh radix scrophulariae superfine powder - Google Patents
Preparation technology for fresh radix scrophulariae superfine powder Download PDFInfo
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Abstract
The invention relates to a processing method for fresh radix scrophulariae, and particularly relates to a preparation technology for fresh radix scrophulariae superfine powder. The preparation technology comprises the following steps of (1) selecting materials; (2) pulping: after preliminarily smashing the raw material fresh radix scrophulariae, adding microcrystalline cellulose powder accounting for 10-20wt% of the raw material, then fully mixing the raw material and the microcrystalline cellulose through rotating a charging bucket of a mixing machine, and then adding water and pulping; (3) pre-freezing: adding tween 80 accounting for 10-15wt% of the pulp before pre-freezing and stirring completely; (4) freeze drying: controlling the water content below 6wt%; and (5) grinding into superfine powder through a vibrating type superfine grinding mixing mill. The fresh radix scrophulariae superfine powder prepared by the preparation technology can reserve active ingredients of the fresh radix scrophulariae to the maximum degree.
Description
Technical field
The present invention relates to a kind of processing method of fresh Radix Scrophulariae, be specifically related to a kind of fresh radix scrophulariae superfine powder preparation technology.
Background technology
Prior art, when concocting this herb of fresh Radix Scrophulariae, is excavated when normally winter, stem and leaf was withered, and removing rhizome, sub-bud, fibrous root and silt, shine or be dried to half-dried, stacking 3 ~ 6 days, repeatedly for several times to dry.Modern study shows, traditional concocting method is by active component many for loss.
Summary of the invention
The active component that the object of the invention is for solving fresh radix scrophulariae superfine powder in prior art retains not high enough technical problem, provides a kind of preparation technology of fresh radix scrophulariae superfine powder.The method farthest can retain the active component in fresh Radix Scrophulariae, and obtained fresh radix scrophulariae superfine powder rehydration is also greatly improved.
Above-mentioned technical purpose of the present invention is achieved by the following technical programs:
A kind of fresh radix scrophulariae superfine powder preparation technology, comprises the following steps:
(1) select materials: get fresh Radix Scrophulariae and wash, remove impurity, drain;
(2) pull an oar: the fresh Radix Scrophulariae of raw material adds the microcrystalline Cellulose powder of raw materials quality 10 ~ 20wt% after tentatively pulverizing, then by the rotation of mixer batch can, described raw material is fully mixed with described microcrystalline Cellulose; Then the water making beating of raw materials quality 0.8 ~ 1.8 times is added;
(3) pre-freeze: pre-freeze after making beating, pre-freeze to be frozen into solid for standard, and maintains the solid state that is frozen into 5 ~ 10 hours, pre-freezing temperature-8 ~-18 DEG C; Described pre-freeze, also will add the Tween 80 of serosity quality 10 ~ 15wt% and fully stir before pre-freeze;
(4) lyophilization: pre-freeze postlyophilization, cryodesiccated controlled condition is at-45 ~-50 DEG C, 24 ~ 120 hours time, requires that moisture control is at below 6wt% simultaneously;
(5) micropowder is broken: the powder agglomates obtained after lyophilization is broken into micropowder by vibration type micronizing grinding mixing roll.
Preferred as technique scheme, step (5) is played micropowder specific requirement and is, makes grain size of micropowder more than 95% reach less than 10 μm.
Preferred as technique scheme, the moisture content of described fresh radix scrophulariae superfine powder is lower than 5%.
Chinese medicine is in traditional Preparation process process, and the effective ingredient such as vegetable protein, polysaccharide can be damaged.The present invention is by pre-freeze after the making beating that adds water, and fresh Radix Scrophulariae medical material is first through freezing before distillation dehydration, is formed stable " skeleton ", by low-temperature negative-pressure dehydrate, is prepared into fresh radix scrophulariae superfine powder finally by vibration type micronizing grinding mixing roll.According to the feature of micronizing, when Chinese medicine carries out superfine grinding, affected many factors: first, the various and complicated component of herbal species, not all medicine is all applicable to superfine grinding, neither powder more thin better.Containing the medical material of armaticity, volatile ingredient, sporoderm-broken rate is high, is conducive to the abundant exposure emission and absorption of effective ingredient, but while pulverizing, the loss of volatile component can not be ignored, and therefore this kind of medical material needs to be crushed to what degree needs to study further; Secondly, be macromolecular medical material for some active components, being crushed to what degree could not saboteur's structure also need to investigate further, and some medical material containing toxic component also will using the index of the stripping of toxic component as an investigation in addition.Except kind is different, also has moisture, former particle size distribution, pulverize the factors such as environment.Therefore, up to the present, realize the superfine grinding of same fineness with same equipment, same disintegrating process, also acquire a certain degree of difficulty.According to concrete medicine, super-fine processing can only be carried out for specific requirement.Therefore, the adjustment carrying out a large amount of tests and disintegrating process and pulverizing parameter is needed.
The present invention, in pulping process, with the addition of microcrystalline Cellulose.Microcrystalline Cellulose is a kind of conventional medical auxiliary materials, and it is present in reasonability in medicine and repeatedly proves with scientific being through, and therefore it can be used as adjuvant, is at least out of question at medical angle.In the present invention, the effect of microcrystalline Cellulose is not obviously traditional value as medical accessory, and it can help the effective ingredient of the making beating of raw material and protection raw material not to be destroyed in pulping process.
Because the extra interpolation of microcrystalline Cellulose it is also proposed new problem for present invention process, that is, during last micronizing, the resistance from material increases, and makes vibration type micronizing grind mixing roll usually overheated, and polishing effect is also undesirable.The present inventor, after employing Tween 80, solves this problem.Tween 80 is also a kind of conventional pharmaceutical auxiliaries, the same with microcrystalline Cellulose, is safe and reliable equally.The detailed directions of Tween 80 is: before pre-freeze, add the Tween 80 of serosity quality 10 ~ 15wt% and fully stir, then pre-freeze.
By fresh radix scrophulariae superfine powder steady quality prepared by the present invention, can preserve for a long time at normal temperatures, its rehydration is fabulous, and can absorb water rapidly recovery, and its color and luster, quality and fresh goods are substantially identical.In addition, tested by In Vitro Dissolution, the medical material under known unit mass, fresh radix scrophulariae superfine powder fresh and dried Radix Scrophulariae rear than the process of preparing Chinese medicine prepared by the inventive method, containing more effective ingredient.Also find in experimentation, fresh radix scrophulariae superfine powder prepared by the inventive method, after inhaling the recovery of a small amount of water, in thick, and the fresh radix scrophulariae superfine powder adopting traditional method to concoct, after restoring with waiting water gaging, sliminess is obviously not enough.Known by method of the present invention, the active component of fresh Radix Scrophulariae medical material can be remained to a greater degree.Found by pharmacodynamic study, fresh radix scrophulariae superfine powder prepared by the inventive method, the drug effect of its smaller dose can be equal to the drug effect of fresh and dried Radix Scrophulariae extractum clinical medicine dose.
The present invention has following technique effect:
(1) the fresh radix scrophulariae superfine powder adopting the inventive method to prepare, farthest can retain the active component in fresh Radix Scrophulariae;
(2) the fresh radix scrophulariae superfine powder adopting the inventive method to prepare, the drug effect of its smaller dose can be equal to the drug effect of fresh and dried Radix Scrophulariae extractum clinical medicine dose;
(3) the fresh radix scrophulariae superfine powder adopting the inventive method to prepare, steady quality, can preserve at normal temperatures for a long time;
(4) the fresh radix scrophulariae superfine powder adopting the inventive method to prepare, its rehydration is fabulous, and can absorb water rapidly recovery, and its color and luster, quality and fresh goods are substantially identical.
Accompanying drawing explanation
Fig. 1 is Radix Scrophulariae standard substance collection of illustrative plates;
Fig. 2 is that Radix Scrophulariae dries sample collection of illustrative plates;
Fig. 3 is the cold dry-eye disease collection of illustrative plates of Radix Scrophulariae;
Fig. 4 is that Radix Scrophulariae adds 80ml water sample collection of illustrative plates;
Fig. 5 is that Radix Scrophulariae adds 120ml water sample collection of illustrative plates;
Fig. 6 is that Radix Scrophulariae adds 160ml water sample collection of illustrative plates;
Fig. 7 is Harpagide In Vitro Dissolution curve chart in Radix Scrophulariae micropowder, common flour, extractum;
Fig. 8 is Harpagide In Vitro Dissolution curve chart in Radix Scrophulariae micropowder, common flour, extractum.
Detailed description of the invention
This detailed description of the invention is only explanation of the invention; it is not limitation of the present invention; as long as any change that those skilled in the art can be done after having read description of the present invention, within claim limited range of the present invention, all will be subject to the protection of Patent Law.
embodiment 1
A kind of fresh radix scrophulariae superfine powder preparation technology, comprises the following steps:
(1) select materials: get fresh Radix Scrophulariae and wash, remove impurity, drain;
(2) pull an oar: the fresh Radix Scrophulariae of raw material adds the microcrystalline Cellulose powder of raw materials quality 10wt% after tentatively pulverizing, then by the rotation of mixer batch can, described raw material is fully mixed with described microcrystalline Cellulose; Then the water making beating of raw materials quality 0.8 times is added;
(3) pre-freeze: pre-freeze after making beating, pre-freeze to be frozen into solid for standard, and maintains the solid state that is frozen into 5 ~ 10 hours, pre-freezing temperature-8 ~-18 DEG C; Described pre-freeze, also will add the Tween 80 of serosity quality 10wt% and fully stir before pre-freeze;
(4) lyophilization: pre-freeze postlyophilization, cryodesiccated controlled condition is at-45 ~-50 DEG C, 24 ~ 120 hours time, requires that moisture control is at below 6wt% simultaneously;
(5) micropowder is broken: the powder agglomates obtained after lyophilization is broken into micropowder by vibration type micronizing grinding mixing roll, and make grain size of micropowder more than 95% reach less than 10 μm, moisture content is lower than 5%.
embodiment 2
A kind of fresh radix scrophulariae superfine powder preparation technology, comprises the following steps:
(1) select materials: get fresh Radix Scrophulariae and wash, remove impurity, drain;
(2) pull an oar: the fresh Radix Scrophulariae of raw material adds the microcrystalline Cellulose powder of raw materials quality 12wt% after tentatively pulverizing, then by the rotation of mixer batch can, described raw material is fully mixed with described microcrystalline Cellulose; Then the water making beating of raw materials quality 1.0 times is added;
(3) pre-freeze: pre-freeze after making beating, pre-freeze to be frozen into solid for standard, and maintains the solid state that is frozen into 5 ~ 10 hours, pre-freezing temperature-8 ~-18 DEG C; Described pre-freeze, also will add the Tween 80 of serosity quality 11wt% and fully stir before pre-freeze;
(4) lyophilization: pre-freeze postlyophilization, cryodesiccated controlled condition is at-45 ~-50 DEG C, 24 ~ 120 hours time, requires that moisture control is at below 6wt% simultaneously;
(5) micropowder is broken: the powder agglomates obtained after lyophilization is broken into micropowder by vibration type micronizing grinding mixing roll, and make grain size of micropowder more than 95% reach less than 10 μm, moisture content is lower than 5%.
embodiment 3
A kind of fresh radix scrophulariae superfine powder preparation technology, comprises the following steps:
(1) select materials: get fresh Radix Scrophulariae and wash, remove impurity, drain;
(2) pull an oar: the fresh Radix Scrophulariae of raw material adds the microcrystalline Cellulose powder of raw materials quality 14wt% after tentatively pulverizing, then by the rotation of mixer batch can, described raw material is fully mixed with described microcrystalline Cellulose; Then the water making beating of raw materials quality 1.2 times is added;
(3) pre-freeze: pre-freeze after making beating, pre-freeze to be frozen into solid for standard, and maintains the solid state that is frozen into 5 ~ 10 hours, pre-freezing temperature-8 ~-18 DEG C; Described pre-freeze, also will add the Tween 80 of serosity quality 12wt% and fully stir before pre-freeze;
(4) lyophilization: pre-freeze postlyophilization, cryodesiccated controlled condition is at-45 ~-50 DEG C, 24 ~ 120 hours time, requires that moisture control is at below 6wt% simultaneously;
(5) micropowder is broken: the powder agglomates obtained after lyophilization is broken into micropowder by vibration type micronizing grinding mixing roll, and make grain size of micropowder more than 95% reach less than 10 μm, moisture content is lower than 5%.
embodiment 4
A kind of fresh radix scrophulariae superfine powder preparation technology, comprises the following steps:
(1) select materials: get fresh Radix Scrophulariae and wash, remove impurity, drain;
(2) pull an oar: the fresh Radix Scrophulariae of raw material adds the microcrystalline Cellulose powder of raw materials quality 16wt% after tentatively pulverizing, then by the rotation of mixer batch can, described raw material is fully mixed with described microcrystalline Cellulose; Then the water making beating of raw materials quality 1.4 times is added;
(3) pre-freeze: pre-freeze after making beating, pre-freeze to be frozen into solid for standard, and maintains the solid state that is frozen into 5 ~ 10 hours, pre-freezing temperature-8 ~-18 DEG C; Described pre-freeze, also will add the Tween 80 of serosity quality 13wt% and fully stir before pre-freeze;
(4) lyophilization: pre-freeze postlyophilization, cryodesiccated controlled condition is at-45 ~-50 DEG C, 24 ~ 120 hours time, requires that moisture control is at below 6wt% simultaneously;
(5) micropowder is broken: the powder agglomates obtained after lyophilization is broken into micropowder by vibration type micronizing grinding mixing roll, and make grain size of micropowder more than 95% reach less than 10 μm, moisture content is lower than 5%.
embodiment 5
A kind of fresh radix scrophulariae superfine powder preparation technology, comprises the following steps:
(1) select materials: get fresh Radix Scrophulariae and wash, remove impurity, drain;
(2) pull an oar: the fresh Radix Scrophulariae of raw material adds the microcrystalline Cellulose powder of raw materials quality 18wt% after tentatively pulverizing, then by the rotation of mixer batch can, described raw material is fully mixed with described microcrystalline Cellulose; Then the water making beating of raw materials quality 1.6 times is added;
(3) pre-freeze: pre-freeze after making beating, pre-freeze to be frozen into solid for standard, and maintains the solid state that is frozen into 5 ~ 10 hours, pre-freezing temperature-8 ~-18 DEG C; Described pre-freeze, also will add the Tween 80 of serosity quality 14wt% and fully stir before pre-freeze;
(4) lyophilization: pre-freeze postlyophilization, cryodesiccated controlled condition is at-45 ~-50 DEG C, 24 ~ 120 hours time, requires that moisture control is at below 6wt% simultaneously;
(5) micropowder is broken: the powder agglomates obtained after lyophilization is broken into micropowder by vibration type micronizing grinding mixing roll, and make grain size of micropowder more than 95% reach less than 10 μm, moisture content is lower than 5%.
embodiment 6
A kind of fresh radix scrophulariae superfine powder preparation technology, comprises the following steps:
(1) select materials: get fresh Radix Scrophulariae and wash, remove impurity, drain;
(2) pull an oar: the fresh Radix Scrophulariae of raw material adds the microcrystalline Cellulose powder of raw materials quality 20wt% after tentatively pulverizing, then by the rotation of mixer batch can, described raw material is fully mixed with described microcrystalline Cellulose; Then the water making beating of raw materials quality 1.8 times is added;
(3) pre-freeze: pre-freeze after making beating, pre-freeze to be frozen into solid for standard, and maintains the solid state that is frozen into 5 ~ 10 hours, pre-freezing temperature-8 ~-18 DEG C; Described pre-freeze, also will add the Tween 80 of serosity quality 15wt% and fully stir before pre-freeze;
(4) lyophilization: pre-freeze postlyophilization, cryodesiccated controlled condition is at-45 ~-50 DEG C, 24 ~ 120 hours time, requires that moisture control is at below 6wt% simultaneously;
(5) micropowder is broken: the powder agglomates obtained after lyophilization is broken into micropowder by vibration type micronizing grinding mixing roll, and make grain size of micropowder more than 95% reach less than 10 μm, moisture content is lower than 5%.
fresh medical material process
Fresh medical material is washed, removes impurity, drain, section.A part carries out diaphoresis process, and a part carries out drying and processing, and all the other carry out making beating process.
The medical material drained is added purified water according to the ratio of 80ml/100g, 120ml/100g, 160ml/100g respectively pull an oar with the method for embodiment, put into refrigerator freezing, then carry out lyophilization; Do the direct lyophilization of a crude drug in addition to contrast.
extractum method and interpretation of result
Extract mensuration: get test sample and be about 2g, accurately weighed, adding distil water 100ml, heating-condensing refluxes, and keeps micro-1h that boils, after placing 2h, accurately weighed, supply weightlessness, shake up, filter, get filtrate 10ml, put in dry constant weight evaporating dish, in water-bath after evaporate to dryness, in 105 DEG C of oven dryings, put in exsiccator and cool 30min, weighed weight.Calculate the extract content (%) in test sample.
As can be seen from the table, making beating can only increase the amount of Radix Scrophulariae extractum slightly, and effect is not clearly.
liquid content assay method and interpretation of result
methodological study
Chromatographic condition
Chromatographic column is octadecylsilane chemically bonded silica is filler; Take acetonitrile as mobile phase A, with 0.03% phosphoric acid solution for Mobile phase B, according to the form below regulation carries out gradient elution; Determined wavelength is 210nm.
The preparation of reference substance solution
Get Harpagide reference substance, harpagoside reference substance is appropriate, accurately weighed, add 30% methanol and make the mixed solution of every 1ml containing Harpagide 60 μ g, harpagoside 20 μ g, to obtain final product.
The preparation of need testing solution
Sample thief powder is about 0.5g, accurately weighed, puts in tool plug conical flask, closely add 50% methanol 50ml, close plug, weighed weight, soak 1 hour, supersound process (power 500W, frequency 40kHz) 45 minutes, let cool, more weighed, the methanol with 50% supplies the weight of less loss, shake up, filter, get subsequent filtrate, as need testing solution.
precision test
It is reference substance solution 10 μ L that precision measures concentration, continuous sample introduction 6 pin, measures peak area, calculates relative standard deviation (RSD), to investigate the precision of instrument.
Result shows that the relative standard deviation (RSD) of Harpagide reference substance, harpagoside reference substance is respectively 0.58%, 0.27%, shows that the method precision is good.
stability test
Get Radix Scrophulariae micropowder and be about 0.5g, closely weighed, put in tool plug conical flask, precision adds 50% methanol 50ml, weighed weight, soak 1 hour, supersound process 45 minutes, lets cool, weighed weight again, supplies the weight of less loss, shakes up with 50% methanol, filter, get subsequent filtrate, respectively at 0,2,4,8,16,44 hours sample introduction 10 μ L, measure peak area.Calculate relative standard deviation, to investigate the stability of sample in this analytical method.
In result show sample, the relative standard deviation of Harpagide and harpagoside is 0.44% and 0.46%, shows that this sample has good stability at 44h.
repeatability is tested
Get 6 batch sample by the parallel preparation of 2.2.2.1.3 preparation method 6 parts, sequentially determining also calculates content, and calculates its relative standard deviation, and whether verification sample solution batches difference is in credible scope.
It is 2.72% that result shows 6 batch sample Harpagide content relative standard deviations; Harpagoside content relative standard deviation is 2.99%, and the relative standard deviation of total content RSD is 2.86%, illustrates that the diversity between each batch is less.
average recovery
Get the sample of known content, totally 6 parts, prepare solution, by sample by need testing solution preparation method: the volume ratio of standard substance=2:1 adds the Harpagide standard substance of 220 μ g/ml, measures peak area by under identical chromatographic conditions, calculate the response rate.
the assay of Radix Scrophulariae
Get micropowder samples respectively, make need testing solution by need testing solution preparation method, sample introduction 10 μ l, by above-mentioned chromatographic condition, measure peak area, calculate Harpagide and harpagoside content by the dry product of Radix Scrophulariae micropowder.
Can find out thus, direct cryodesiccated sample size is higher than the sample of drying, pull an oar, and illustrates that Freeze Drying Technique can well preserve Harpagide and harpagoside, makes it not decompose in process of production.
Radix Scrophulariae standard substance collection of illustrative plates as shown in Figure 1; Radix Scrophulariae dries sample collection of illustrative plates as shown in Figure 2; The cold dry-eye disease collection of illustrative plates of Radix Scrophulariae as shown in Figure 3; Radix Scrophulariae adds 80ml water sample collection of illustrative plates as shown in Figure 4; Radix Scrophulariae adds 120ml water sample collection of illustrative plates as shown in Figure 5; Radix Scrophulariae adds 160ml water sample collection of illustrative plates as shown in Figure 6.
radix Scrophulariae micropowder quantitative dose-effect relationship
experimental technique is investigated
Chromatographic condition
Chromatographic column is octadecylsilane chemically bonded silica is filler; Take acetonitrile as mobile phase A, with 0.03% phosphoric acid solution for Mobile phase B, according to the form below regulation carries out gradient elution; Determined wavelength is 210nm; Flow velocity is 1ml/min.
The preparation of reference substance solution
Get Harpagide reference substance, harpagoside reference substance is appropriate, accurately weighed, add 30% methanol and make the mixed solution of every 1ml containing Harpagide 60 μ g, harpagoside 20 μ g, to obtain final product.
The preparation of need testing solution
Sample thief powder is about 0.5g, accurately weighed, puts in tool plug conical flask, closely add 50% methanol 50ml, close plug, weighed weight, soak 1 hour, supersound process (power 500W, frequency 40kHz) 45 minutes, let cool, more weighed, the methanol with 50% supplies the weight of less loss, shake up, filter, get subsequent filtrate, as need testing solution.
precision test
It is reference substance solution 10 μ L that precision measures concentration, continuous sample introduction 6 pin, measures peak area, calculates relative standard deviation (RSD), to investigate the precision of instrument.
Result shows that the relative standard deviation (RSD) of Harpagide reference substance, harpagoside reference substance is respectively 0.58%, 0.27%, shows that the method precision is good.
stability test
Get Radix Scrophulariae micropowder and be about 0.5g, closely weighed, put in tool plug conical flask, precision adds 50% methanol 50ml, weighed weight, soak 1 hour, supersound process 45 minutes, lets cool, weighed weight again, supplies the weight of less loss, shakes up with 50% methanol, filter, get subsequent filtrate, respectively at 0,2,4,8,16,44 hours sample introduction 10 μ L, measure peak area.Calculate relative standard deviation, to investigate the stability of sample in this analytical method.
In result show sample, the relative standard deviation of Harpagide and harpagoside is 0.44% and 0.46%, shows that this sample has good stability at 44h.
repeatability is tested
Get 6 batch sample by the parallel preparation of 2.2.2.1.3 preparation method 6 parts, sequentially determining also calculates content, and calculates its relative standard deviation, and whether verification sample solution batches difference is in credible scope.
It is 2.72% that result shows 6 batch sample Harpagide content relative standard deviations; Harpagoside content relative standard deviation is 2.99%, and the relative standard deviation of total content RSD is 2.86%, illustrates that the diversity between each batch is less.
average recovery
Get the sample of known content, totally 6 parts, prepare solution, by sample by need testing solution preparation method: the volume ratio of standard substance=2:1 adds the Harpagide standard substance of 220 μ g/ml, measures peak area by under identical chromatographic conditions, calculate the response rate.
radix Scrophulariae micropowder, coarse powder, extractum In Vitro Dissolution are tested
Get Radix Scrophulariae micropowder, each 15g of coarse powder respectively, accurately weighed, be fed in 500ml dissolution medium, Radix Scrophulariae decoction pieces 15g decocts to 100ml, drops in 400ml dissolution medium, according to Chinese Pharmacopoeia (version annex in 2010) dissolution method slurry processes, rotating speed 100r/min, temperature is (37 scholar 0.5) DEG C, respectively at 15,30,45,60,90,120min samples 5mL, in stripping rotor, supplement the water of identical temperature and volume, film crossed by sample simultaneously.Calculate this In Vitro Dissolution of various kinds percentage rate.
By Chinese Pharmacopoeia 2010 editions one Radix Scrophulariae high-efficient liquid phase method, in above-mentioned test sample, add methanol by 1:1, make the test sample that 50% methanol is solution, enter 10 μ L samples, measure peak area.
Fig. 7 is harpagoside In Vitro Dissolution curve chart in Radix Scrophulariae micropowder, common flour, extractum.
Fig. 8 is Harpagide In Vitro Dissolution curve chart in Radix Scrophulariae micropowder, common flour, extractum.
Interpretation of result and discussion
In this experimental design procedure, with Radix Scrophulariae main component Harpagide and harpagoside for index, weigh its dissolution in vitro, carry out the mensuration of dissolution respectively at 5,10,15,30,45,60min.Wherein from the stripping situation of Harpagide, micropowder just can stripping and cumulative leaching rate afterwards tend to be steady substantially for 15 minutes completely substantially, also tends towards stability after 15 minutes relative to extractum and coarse powder, but could not stripping completely.From the stripping situation of harpagoside, coarse powder does not almost have stripping, and micropowder just starts continuous decline after within 15 minutes, arriving peak, and this may be relevant with the character of harpagoside, and harpagoside belongs to iridoid, is very easily hydrolyzed by sour water.Extractum also may experienced by this process and reach a balance in decoction process, could not be hydrolyzed when stripping.
Claims (3)
1. a fresh radix scrophulariae superfine powder preparation technology, comprises the following steps:
(1) select materials: get fresh Radix Scrophulariae and wash, remove impurity, drain;
(2) pull an oar: the fresh Radix Scrophulariae of raw material adds the microcrystalline Cellulose powder of raw materials quality 10 ~ 20wt% after tentatively pulverizing, then by the rotation of mixer batch can, described raw material is fully mixed with described microcrystalline Cellulose; Then the water making beating of raw materials quality 0.8 ~ 1.8 times is added;
(3) pre-freeze: pre-freeze after making beating, pre-freeze to be frozen into solid for standard, and maintains the solid state that is frozen into 5 ~ 10 hours, pre-freezing temperature-8 ~-18 DEG C; Described pre-freeze, also will add the Tween 80 of serosity quality 10 ~ 15wt% and fully stir before pre-freeze;
(4) lyophilization: pre-freeze postlyophilization, cryodesiccated controlled condition is at-45 ~-50 DEG C, 24 ~ 120 hours time, requires that moisture control is at below 6wt% simultaneously;
(5) micropowder is broken: the powder agglomates obtained after lyophilization is broken into micropowder by vibration type micronizing grinding mixing roll.
2. the fresh radix scrophulariae superfine powder preparation technology of one according to claim 1, is characterized in that: step (5) is played micropowder specific requirement and is, makes grain size of micropowder more than 95% reach less than 10 μm.
3. the fresh radix scrophulariae superfine powder preparation technology of one according to claim 1 and 2, is characterized in that: the moisture content of described fresh radix scrophulariae superfine powder is lower than 5%.
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|---|---|
| CN103520359A (en) | 2014-01-22 |
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Address after: 313300 No.1 Road, health pharmaceutical garden, Anji Economic Development Zone, Huzhou, Zhejiang Patentee after: Zhejiang Zuo Libaicao prepared slices of Chinese crude drugs company limited Address before: 313300, Huzhou Anji Economic Development Zone, Zhejiang Province Health Medical Park No.1 road Zhejiang Chinese Herbal Medicine Co., Ltd. Patentee before: Zhejiang Baicao Traditional Chinese Medicine Pieces Co., Ltd. |