CN102670667A - Compressed traditional Chinese medicine decoction pieces and preparation method thereof - Google Patents
Compressed traditional Chinese medicine decoction pieces and preparation method thereof Download PDFInfo
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- CN102670667A CN102670667A CN2012101391427A CN201210139142A CN102670667A CN 102670667 A CN102670667 A CN 102670667A CN 2012101391427 A CN2012101391427 A CN 2012101391427A CN 201210139142 A CN201210139142 A CN 201210139142A CN 102670667 A CN102670667 A CN 102670667A
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Abstract
The invention provides compressed traditional Chinese medicine decoction pieces and a preparation method thereof. According to the compressed traditional Chinese medicine decoction pieces, traditional Chinese medicine decoction pieces or crude drugs are used as a raw material. The compressed traditional Chinese medicine decoction pieces are objects with a stable geometric shape, the self shapes of the traditional Chinese medicine decoction pieces or the crude drugs can be seen at the surfaces of the compressed traditional Chinese medicine decoction pieces, and the properties of the traditional Chinese medicine decoction pieces or the crude drugs in the compressed traditional Chinese medicine decoction pieces are unchanged. The compressed traditional Chinese medicine decoction pieces provided by the invention have small volume, are beneficial to warehousing and are convenient to package, store and transport; the stability of the components of the traditional Chinese medicines of the compressed decoction pieces is increased according to the compressed decoction pieces; moreover, the volatility of the components which are easy to volatilize is reduced; the compressed traditional Chinese medicine decoction pieces are not easy to pollute and are not easy to damage by worms; the quantitative compressed decoction pieces facilitate for regulating a formula of traditional Chinese medicines, so that the regulation of the formula is more accurate, and the regulation efficiency is higher; and the preparation method is simple, is low in cost and is suitable for industrialized production.
Description
Technical field
The present invention relates to the prepared slices of Chinese crude drugs and preparing technical field thereof, be meant a kind of compression prepared slices of Chinese crude drugs and preparation method thereof especially.
Background technology
Three big pillars of Chinese medicine industry are Chinese crude drug (crude drug), the prepared slices of Chinese crude drugs, Chinese patent medicine.Wherein, the prepared slices of Chinese crude drugs are to concoct processing by Chinese crude drug, take after the decoction; Also be the raw material of Chinese patent medicine production simultaneously.The traditional Chinese medicines decoction pieces is on the basis of Chinese crude drug (crude drug), simply to be processed into; Because raw materials of traditional Chinese medicinal materials (crude drug) is agricultural byproducts mostly; Its out-of-shape, quality is uneven, and causing the prepared slices of Chinese crude drugs is out-of-shape equally; Quality is uneven, and is difficult to realize the standardization and the automatization of metering, packing.
This present situation has seriously hindered the modernization of the field of Chinese medicines.For a change this present situation of Chinese medicine worker both domestic and external has been carried out extensive work.For example, CN1362059A, 2002.8.7, Chinese invention patent disclose a kind of nanometer prepared slices of Chinese crude drugs and preparation method thereof: be that Chinese medicine powder is broken into the superfines below 500 nanometers.The preparation process of this superfines, preparation cost is too high, and has smashed the cell wall of plant or animal Chinese medicine, has than big difference with the structure of Chinese medicine decoction pieces.The effect same that whether can reach the Chinese medicine decoction pieces needs checking.Simultaneously, the granularity of this superfines is too tiny, and is mobile unstable; If realize automatization's weighing, divide packing, might cause the obstruction of pipeline through equipment such as pipelines.
Main is: this superfines has been destroyed the cell tissue of the plant in the crude drug, animal, makes that the state of this superfines and Chinese medicine decoction pieces is inconsistent, on drug effect, does not possess equity.
In addition, preparation, automatization's fractional pack and quality standard research Project Study content thereof about the compression prepared slices of Chinese crude drugs reduce: 1. decoction pieces granule; Claim to exempt to decoct granule again; Though solved flowability problem, the basic principle gap that is considered to boil altogether with Chinese medicine crowd medicine is bigger, and dispute is fierce; So far the approval of medical circles in not obtaining as yet, it is very big that difficulty is promoted in commercialization; 2. decoction pieces granule (decoction pieces fourth), abroad, Japan's hall of following the mandate of heaven is cut into slices raw medicinal herbs, be cut into silk, is cut into granule again, complex process, loss is big, promotes in China to face cost pressure; 3. granule decoction pieces, CN1362059A, 2002.8.7, single-minded kind of nanometer prepared slices of Chinese crude drugs of China's invention, technology is different, and granular size is different, and product form is different.
The fractional pack of the prepared slices of Chinese crude drugs is as the term suggests be packaged in traditional decoction pieces in the small plastic bag his release; Though improved at present the prescription quality of the prepared slices of Chinese crude drugs, solved that Chinese medicine pharmacy's staff is few, the place is little, the problem of environment difference, be actually and marry again manufacturing enterprise to these problems and gone; Because of decoction pieces does not have flowability, production process is craft, make enterprise difficult negative its heavy the time; Be absorbed in fractional pack and do not have bar code; Do not have labelled amount, do not have lot number, difference between batch apart from more greatly, especially among the inhomogenous difficult situation of product quality.
In view of this, it is inhomogeneous how to break away from decoction pieces, and quality gap is bigger between criticizing and criticizing, and fractional pack is difficult to the difficult situation of automatization, also needs further research and development; In addition, the production standardization of the prepared slices of Chinese crude drugs and quality standardization still do not have solution so far.
Summary of the invention
The present invention proposes a kind of compression prepared slices of Chinese crude drugs and preparation method thereof, has solved in the prior art Chinese medicine problem of quantitatively filling a prescription; Also solved the problem of prepared slices of Chinese crude drugs production standardization and quality standardization.
Technical scheme of the present invention is achieved in that
A kind of compression prepared slices of Chinese crude drugs; These compression prepared slices of Chinese crude drugs are raw material with Chinese medicine decoction pieces or crude drug; The said compression prepared slices of Chinese crude drugs are the object of geometrical shape stability; The shape of the prepared slices of Chinese crude drugs or crude drug itself can be seen in the surface of the compression prepared slices of Chinese crude drugs, and the prepared slices of Chinese crude drugs in the compression prepared slices of Chinese crude drugs or the character of crude drug are constant.
Further, the water content of the described compression prepared slices of Chinese crude drugs is lower than 15%; Better numerical value is: water content is lower than 10%; Optimum is: water content is lower than 5%.
Further, said geometry is cylindric, flat column, cuboid, sphere etc.
Further, the single weight of the said compression prepared slices of Chinese crude drugs is 1g-200g.
Further, the said compression prepared slices of Chinese crude drugs are cylindric or flat column, and diameter is 5mm-200mm, and thickness is 2mm-100mm.Further, diameter is 10～180mm; Optimum is diameter 12mm～120mm; Further, thickness is 5mm-90mm; Better thickness is 10mm-80mm; Optimum is: thickness is at 12mm-75mm.
The described compression prepared slices of Chinese crude drugs are after decocting 1min-8min, but decoction made from powder reverts to the character of former medicine.Decocting time is 2～8min preferably; Better decocting time is 2～6min; Optimum is that the hardness decocting time is 3～5min.
Above-mentioned prepared slices of Chinese crude drugs raw material is 2010 editions, and " first one of Chinese pharmacopoeia recorded herbal species, comprises animal drugs, plant amedica and mineral drug.Said crude drug raw material is animal drugs, plant amedica and the mineral drug kind that Shanghai science tech publishing house " Chinese medicine voluminous dictionary " records.
The above-mentioned prepared slices of Chinese crude drugs or crude drug meet existing Chinese Pharmacopoeia standard, Ministry of Public Health ministry standard, local Chinese crude drug standard and local concocted specification.
Processing method of the present invention changes face shaping, but properties and characteristics is constant, and identical with the Chinese medicine decoction pieces, purposes is constant.
A kind of method for preparing of compressing the prepared slices of Chinese crude drugs comprises:
(1) gets the prepared slices of Chinese crude drugs or crude drug, clean, remove impurity;
(2) prepared slices of Chinese crude drugs or the crude drug with above-mentioned removal impurity gets into suppression process, promptly gets and compresses the prepared slices of Chinese crude drugs; Technological parameter does, pressure is 30t-200t, and the time is 2s-20s.
Further, the described prepared slices of Chinese crude drugs or crude drug are put into compacting tool set suppress, wherein the geometry of compacting tool set is cylindric, flat column, cuboid, sphere etc.
Further, soften earlier, make its water content, getting into suppression process afterwards at 5%-15% for the medical material or the decoction pieces of difficult pressure.
Further, pressure is 40t-160t; Better numerical value is: 50t-120t; Press time is at 3s-15.5s; Better numerical value is: 5s-12s.
Further, the prepared compression prepared slices of Chinese crude drugs are carried out drying, sterilization is packed then, corresponding sign amount is arranged, date of manufacture, the sign of manufacturer and manufacturer on the packaging material.
The compression prepared slices of Chinese crude drugs of the present invention have solved the quantitative prescription problem of the prepared slices of Chinese crude drugs; Can be different according to crude drug content, adopt Electronic Data Processing to feed intake, solve the inhomogeneity problem of the prepared slices of Chinese crude drugs; And make automated package, quantification, the commercialization of the prepared slices of Chinese crude drugs become possibility.This compression prepared slices of Chinese crude drugs are on the basis of the prepared slices of Chinese crude drugs, use modern pressing process the prepared slices of Chinese crude drugs or crude drug directly are pressed into the footpath at 5mm～200mm; Thickness is at 2mm-100mm; Single weight is at the novel decoction pieces of 1g-200g, and wherein the plant amedica of compression, animal drugs can return to the character of original decoction pieces or crude drug again in the process that decocts, and compression process only is the change of volume and shape, does not change the properties and characteristics of decoction pieces or crude drug.Utilize present compact technique to be prepared into geometry, drying, sterilization, packing.The reform of the compression prepared slices of Chinese crude drugs meets the Chinese medicine traditional theory, meets the big production of modernization again.
The compression decoction pieces is compared with traditional decoction pieces, has following beneficial effect:
(1) the compression prepared slices of Chinese crude drugs are compared with traditional decoction pieces or raw medicinal herbs, have reduced the prepared slices of Chinese crude drugs or raw medicinal herbs volume, and institute takes up space little, is beneficial to storage, is convenient to packing, storage, transportation; The compression decoction pieces has increased the stability of its Chinese medicine ingredients, and has reduced the diversity of effumability composition; Compression decoction pieces volume is little, is difficult for polluting, and is difficult for damaging by worms, and quantitative compression decoction pieces is convenient to Chinese medicine preparation and is adjusted, and it is more accurate that prescription is adjusted, and the efficient of adjusting is higher; Because the compression decoction pieces does not change the character of the prepared slices of Chinese crude drugs or raw medicinal herbs, can not change herbal nature, meet the theory of Chinese medicine " crowd boils altogether and fries in shallow oil ", be easy to mechanization production, be convenient to promote;
(2) compression decoction pieces of the present invention is a raw material with Chinese medicine decoction pieces or raw medicinal herbs, does not add any adjuvant, forms through the compacting of modern Chinese medicine press, and this technology is simple, and cost is low, is suitable for suitability for industrialized production;
(3) the compression prepared slices of Chinese crude drugs are compared with the Chinese medicine decoction pieces, in the process that decocts, soak fully more easily, and decocting rate is higher, and the decoction pieces utilization rate is higher.
(4) the alternative traditional Chinese medicines decoction pieces of the compression prepared slices of Chinese crude drugs of the present invention had both met Chinese traditional medicine principle; Meet the modern production requirement again; Not only satisfying the requirement of the preventing and treating diseases that the people improves constantly, and be the requirement of social progress, also is the step that prepared slices of Chinese crude drugs industry must be stepped out.
Description of drawings
In order to be illustrated more clearly in the embodiment of the invention or technical scheme of the prior art; To do to introduce simply to the accompanying drawing of required use in embodiment or the description of the Prior Art below; Obviously, the accompanying drawing in describing below only is some embodiments of the present invention, for those of ordinary skills; Under the prerequisite of not paying creative work property, can also obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 is the embodiment of the invention 1 Herba Verbenae tradition decoction pieces and compression prepared slices of Chinese crude drugs TLC collection of illustrative plates; S-ursolic acid wherein; C-Herba Verbenae control medicinal material; The b-Herba Verbenae compression prepared slices of Chinese crude drugs; A-Herba Verbenae tradition decoction pieces;
Fig. 2 is the stem epidermis cell microscope figure of the embodiment of the invention 1 Herba Verbenae tradition decoction pieces and the compression prepared slices of Chinese crude drugs; A-Herba Verbenae tradition decoction pieces wherein; The b-Herba Verbenae compression prepared slices of Chinese crude drugs;
Fig. 3 is the leaf lower epidermis microcytoscope figure of the embodiment of the invention 1 Herba Verbenae tradition decoction pieces and the compression prepared slices of Chinese crude drugs; A-Herba Verbenae tradition decoction pieces wherein; The b-Herba Verbenae compression prepared slices of Chinese crude drugs;
Fig. 4 is the unicellular microscope figure of handle of the embodiment of the invention 1 Herba Verbenae tradition decoction pieces and the compression prepared slices of Chinese crude drugs; A-Herba Verbenae tradition decoction pieces wherein; The b-Herba Verbenae compression prepared slices of Chinese crude drugs;
Fig. 5 is the unicellular microscope figure of nonglandular hair of the embodiment of the invention 1 Herba Verbenae tradition decoction pieces and the compression prepared slices of Chinese crude drugs; A-Herba Verbenae tradition decoction pieces wherein; The b-Herba Verbenae compression prepared slices of Chinese crude drugs;
Fig. 6 is the chromatogram of oleanolic acid, ursolic acid reference substance; G-oleanolic acid, f-ursolic acid;
Fig. 7 is a Herba Verbenae need testing solution chromatogram; G-oleanolic acid, f-ursolic acid;
Fig. 8 is the decocting liquid mirror image HPLC comparison diagram of the embodiment of the invention 1 Herba Verbenae tradition decoction pieces and the compression prepared slices of Chinese crude drugs; A-Herba Verbenae tradition decoction pieces wherein; The b-Herba Verbenae compression prepared slices of Chinese crude drugs;
Fig. 9 is the alcohol extract mirror image HPLC comparison diagram of the embodiment of the invention 1 Herba Verbenae tradition decoction pieces and the compression prepared slices of Chinese crude drugs; A-Herba Verbenae tradition decoction pieces wherein; The b-Herba Verbenae compression prepared slices of Chinese crude drugs;
Figure 10 is intelligent press perspective view;
Figure 11 is the perspective view at another visual angle of intelligent press;
Among the figure, the seat of honour 1, oil cylinder 1, piston rod one 11a, base 2, oil cylinder 2 21, piston rod two 21a, guide post 3, slide block 4, table top 5, horizontally push away cylinder 6, photoelectric sensor 7, feed opening 8, pack table top 9 automatically.
The specific embodiment
To combine the accompanying drawing in the embodiment of the invention below, the technical scheme in the embodiment of the invention is carried out clear, intactly description, obviously, described embodiment only is the present invention's part embodiment, rather than whole embodiment.Based on the embodiment among the present invention, those of ordinary skills are not making the every other embodiment that is obtained under the creative work prerequisite, all belong to the scope of the present invention's protection.
The compression decoction pieces of Herba Verbenae
Traditional decoction pieces is prepared into the compression decoction pieces, is convenient to store and the production of mechanical automation fractional pack.
Used instrument is: intelligent Chinese medicine press, and this equipment is in 201110443190.0 at application number, and is specific as follows:
Shown in Figure 10 and 11; The intelligence press comprises the seat of honour 1 and base 2 that connect through guide post 3, and described base 2 is provided with oil cylinder 2 21; The end of piston rod two 21a in this oil cylinder 2 21 is connected with the table top 5 on being arranged on base 2; Piston rod two 21a can eject table top 5 with the prepared slices of Chinese crude drugs that suppress, and are convenient to and blanking, avoid occurring easily in the press blanking process in the past omitting.1 is connected through bolt with base 2 two ends at the seat of honour; The seat of honour 1 is fixed with the oil cylinder 1 that has oil pump, through bolt be convenient to fixed oil cylinder 1 at the seat of honour 1 position, be provided with between them and can on guide post 3, slide up and down; And slide block 4 that can installation mold; Mould described here mainly is meant the general designation of upper die and lower die, and the patrix operated by rotary motion is in slide block 4 bottom surfaces, and the counterdie corresponding with it is arranged on the table top 5 of lower end; Described oil cylinder 1 is connected with slide block 4 through piston rod one 11a; Moving up and down just of piston rod one 11a can realize moving up and down of slide block 4, thereby realizes opening and closing of mould, can bring the potential safety hazard to operator in the process of holding and closing of mould simultaneously; In the present technique scheme, be provided with the horizontal cylinder 6 that pushes away through table top 5 one sides, this horizontal cylinder 6 that pushes away is provided with photoelectric sensor 7.Table top 5 opposite sides are provided with feed opening 8 in addition, and feed opening 8 other ends directly are connected with automatic packing table top 9.The prepared slices of Chinese crude drugs can directly get into automatic packing table top 9 in press, save the human resources.Crude drug: Herba Verbenae medical material.
1, cleans operation: the Herba Verbenae prepared slices of Chinese crude drugs or crude drug are cleaned, remove impurity.
2, quantitative: the Herba Verbenae prepared slices of Chinese crude drugs or the crude drug that clean that take by weighing predetermined weight (5-20g) are positioned in the compacting tool set.
3, suppression process:
With compacting tool set will be the Herba Verbenae decoction pieces or the raw medicinal herbs of weighing be placed in the intelligent Chinese medicine press, and intelligent Chinese medicine press compacting parameter is set to 30t-40t pressure, the press time is 7s-12s, the cylinder of compacting predetermined weight, and ejecting automatically.
Above-mentioned compacting parameter is adjusted according to the character of medicine, and adjustable pressure limit is 30t-200t, and time range is 2s-20s.The pressure of generally choosing medicine is 40t-160t; Better numerical value is: 50t-120t; Press time is at 3s-15.5s; Better numerical value is: 5s-12s.
4, according to the medical industry technology compression prepared slices of Chinese crude drugs are carried out dry sterilization;
5, packing:
The Herba Verbenae prepared slices of Chinese crude drugs or crude drug that compression is good are packed with selected packaging material, corresponding sign amount are arranged, date of manufacture, the sign of manufacturer and manufacturer on the packaging material.
Herba Verbenae compression prepared slice quality research on standard
(1) name of an article
Herba Verbenae compression decoction pieces
(2) source
These article are the dry aerial parts of Verenaceae plant Herba Verbenae Verbena officinalis L..Tapped when 6～August, the flowers are in blossom, remove impurity, dry.With Herba Verbenae tradition decoction pieces is raw material, does not add any binding agent, and the size of processing through modern pressing process is than homogeneous, quantitatively, the uniform novel decoction pieces of density.
(3) character
Herba Verbenae compression decoction pieces is more regular cylinder, and surperficial green and brown color is slightly coarse, or visible broken section shape stem, leaf.After scattering, stem is the section of flat, and there is longitudinal furrow on the surface, and the leaf flower is not seen fragmentation.Feeble QI, bitter in the mouth.
(4) specification
Single quality 15g～20g, diameter 44～46mm, thickness 12～17mm can cut.
(5) differentiate
1) the green and brown color of these article powder.The stem epidermis cell is long polygon or rectangle like, and how straight anticlinal wall is, the tool pore.The wavy bending of leaf lower epidermis cell anticlinal wall, pore infinitive or inequality, 3～5 of subsidiary cells.Glandular scale head 4 cells, diameter 23～58 μ m; Handle is unicellular.Nonglandular hair is unicellular.
2) get these article powder 2g, add 80% methanol 60mL, reflux 1 hour filters, the filtrating evaporate to dryness, and residue adds methanol 2mL makes dissolving, as need testing solution.Other gets Herba Verbenae control medicinal material 1g, shines medical material solution in pairs with legal system.Get the ursolic acid reference substance again, add methanol and process the solution that every 1mL contains 1mg, as reference substance solution.According to thin layer chromatography (" appendix VIB of Chinese pharmacopoeia version in 2010) test, draw each 1 μ L of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate; With cyclohexane extraction-chloroform-ethyl acetate-glacial acetic acid (20: 5: 8: 0.1) be developing solvent; Launch, take out, dry; Spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the speckle of same color.
(6) physico-chemical examination
Moisture: must not cross 10.0% (" appendix IXH first method of Chinese pharmacopoeia version in 2010).
Total ash: must not cross 12.0% (" appendix IXK of Chinese pharmacopoeia version in 2010).
Acid-insoluble ash: must not cross 4.0% (" appendix IXK of Chinese pharmacopoeia version in 2010)
(7) assay
Measure according to HPLC (" an appendix VI of Chinese pharmacopoeia version in 2010 D).
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filler; With methanol-0.2% acetum (82.5: 17.5) is mobile phase; Evaporative light scattering detector detects.Number of theoretical plate calculates by the ursolic acid peak should be not less than 5000.
The preparation of reference substance solution: even up pier fruit acid reference substance, the ursolic acid reference substance is an amount of, accurately claim surely, add methanol and process the mixed solution that every 1mL contains oleanolic acid 50 μ g, ursolic acid 0.1mg, promptly get.
The preparation of need testing solution: get the about 0.5g of these article powder (crossing sieve No. four), the accurate title, decide, and puts in the tool plug conical flask, the accurate dehydrated alcohol 25mL that adds; Claim decide weight, reflux 4 hours is put coldly, and weight decided in title again; Supply the weight that subtracts mistake with dehydrated alcohol, shake up, filter.Precision is measured subsequent filtrate 10mL, adds 1% ammonia spirit 3mL, and mixing extracts 3 times with petroleum ether (30～60 ℃) jolting, each 15mL; Discard petroleum ether liquid, get ethanol liquid evaporate to dryness, residue adds dissolve with methanol, is transferred in the 5ml measuring bottle, adds methanol to scale; Shake up, filter, get subsequent filtrate, promptly get.
Algoscopy: accurate respectively reference substance solution 10 μ L, the 20 μ L of drawing, need testing solution 20 μ L inject chromatograph of liquid, measure, and calculate with external standard two-point method logarithmic equation, promptly get.
These article are pressed dry product and are calculated, and contain oleanolic acid (C
30H
48O
3) and ursolic acid (C
30H
48O
3) total amount must not be less than 0.30%.
(8) the decoction made from powder time
These article of getting, single, put in 20 times of water gagings, leave standstill and soaked 30 minutes, be heated to boiling, recording liquid these article required time that all scatters that comes to life.Decoction pieces should all scatter in 2 minutes.
(9) storage
Airtight, put aeration-drying place
(10) quality standard is drafted explanation
[explanation of raw medicinal material source]
According to " Herba Verbenae medical material standard and different places of production Herba Verbenae chemical constitution study data that Chinese pharmacopoeia one one of version in 2010 is recorded in conjunction with the experimental result of Herba Verbenae Compression Study, are Zhejiang Province with the raw material of preparation Herba Verbenae compression decoction pieces is tentative.
Herba Verbenae is produced in Zhejiang, when 6～August, the flowers are in blossom, taps aerial parts, removes impurity, dries.
[method for preparing]
Adopt the prepared slices of Chinese crude drugs compressor of independent research, do not add any adjuvant and binding agent and be prepared into Herba Verbenae compression decoction pieces.
[character]
Herba Verbenae tradition decoction pieces is irregular section.The stem square column type, there is longitudinal furrow at the four sides, and surperficial green and brown color is coarse.Tangent plane has marrow or hollow.How broken leaf is, green and brown color, and complete person flattens rear blade 3 drastic cracks, and there is sawtooth at the edge.Spike has Xiao Hua most.Feeble QI, bitter in the mouth.
The Herba Verbenae compression decoction pieces of molding is more regular cylinder, and surperficial green and brown color is slightly coarse, or visible broken section shape stem, leaf.After scattering, stem is the section of flat, and there is longitudinal furrow on the surface, and the leaf flower is not seen fragmentation.Feeble QI, bitter in the mouth.
[thin layer discriminating]
According to " Chinese pharmacopoeia Herba Verbenae medical material of version in 2010 and decoction pieces item be regulation down, is that reference substance carries out thin layer and differentiates with the ursolic acid, require in the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, the speckle of apparent same color.The result shows that the chromatograph and the ursolic acid of Herba Verbenae tradition decoction pieces and compression decoction pieces show the same color speckle at same position.Both TLC differentiate no marked difference.As shown in Figure 1.
[microscopical identification]
Get Herba Verbenae tradition decoction pieces and cross sieve No. four with compression decoction pieces powder, a little puts picking on the clean microscope slide, drips the chloral hydrate test solution, on alcohol burner, adds heat penetrationization, and drips rare glycerol, covered.The powder film-making that makes is put microscopically and is observed, and the cell integrity of two kinds of decoction pieces relatively is like Fig. 2-shown in Figure 5.
[moisture, total ash, acid-insoluble ash]
Moisture: Herba Verbenae tradition decoction pieces and Herba Verbenae compression agreement that contracts a film or TV play to an actor or actress 3.0g, be tiled in the flat weighing bottle that is dried to constant weight, thickness is no more than 5mm, and loose test sample is no more than 10mm; Accurate claim surely, open bottle cap, bottle cap is built, in the dislocation exsiccator 100～105 ℃ of dryings 5 hours; Cooled off 30 minutes, and accurate claimed decide weight, again said temperature drying 1 hour; Cooling is weighed, and extremely double difference of weighing is no more than till the 5mg.According to the weight that subtracts mistake, calculate water content (%) in the test sample.The moisture that records both is respectively 9.40%, 9.37%." Chinese pharmacopoeia Herba Verbenae medical material of version in 2010 and decoction pieces item regulation moisture down must not be all up to specification above 10.0%, two kind of decoction pieces.
Herba Verbenae tradition decoction pieces and the moisture (n=3) of compressing decoction pieces
Total ash: Herba Verbenae tradition decoction pieces and each about 4g of Herba Verbenae compressed tablet, put in the crucible of ignition to constant weight, claim to decide weight (accurately to 0.01g); Slowly red-hot, note avoiding burning, during to carbonization fully; Elevated temperature to 500～600 ℃ gradually make complete ashing and to constant weight.According to residue weight, calculate the content (%) of total ash in the test sample.
Acid-insoluble ash: go up the ash of a gained, the careful about 10mL of dilute hydrochloric acid that adds covers crucible with surface plate in crucible; Put in the water-bath and heated 10 minutes; Surface plate is with hot water 5mL flushing, and washing liquid is incorporated in the crucible, filters with ashless filter paper; Residue in the crucible is with washing on filter paper, and wash do not show chloride and react to washing liquid till.Filtering residue is together with in the same crucible of filter paper dislocation, drying, ignition to constant weight.According to residue weight, calculate the content (%) of acid-insoluble ash in the test sample.
Herba Verbenae tradition decoction pieces and the total ash, the acid-insoluble ash content (n=3) that compress decoction pieces
" Chinese pharmacopoeia Herba Verbenae medical material of version in 2010 and decoction pieces item regulation total ash down must not surpass 12.0%; Acid-insoluble ash must not surpass 4.0%; The result shows that the total ash content of Herba Verbenae tradition decoction pieces and Herba Verbenae compacting decoction pieces is respectively 10.39%, 10.03%; Acid-insoluble ash is respectively 2.66%, 2.55%, and is all up to specification.
[assay]
" under Chinese pharmacopoeia Herba Verbenae medical material of version in 2010 and the decoction pieces item with the total amount of oleanolic acid and ursolic acid for containing the survey index, the regulation total amount must not be lower than 0.30%.Measure Herba Verbenae tradition decoction pieces and the total amount of compressing oleanolic acid, ursolic acid in the decoction pieces according to its following method.The result shows that the total amount meansigma methods of oleanolic acid, ursolic acid is 0.4423% in the Herba Verbenae compression decoction pieces, and the total amount average is 0.4365% in traditional decoction pieces, and both content value are approximate, and the compression decoction pieces is superior to traditional decoction pieces, all meets the pharmacopeia regulation.
[characteristic spectrum mensuration]
Herba Verbenae tradition decoction pieces and the HPLC relative analysis of compressing decoction pieces decocting liquid:
As shown in Figure 8, the HPLC collection of illustrative plates shows that chemical constituent does not have significant change in the decocting liquid of Herba Verbenae compacting decoction pieces and traditional decoction pieces.
The tradition decoction pieces is analyzed with the HPLC that compresses the decoction pieces alcohol extract, and is as shown in Figure 9;
The HPLC finger printing no significant difference of Herba Verbenae compacting decoction pieces and traditional decoction pieces, the peak area of each chemical constituent is close, and content does not have significant difference.
[decocting rate]
Get Herba Verbenae tradition decoction pieces and each 10g of Herba Verbenae compression decoction pieces, add 200mL water, soak 30min, decoct and also keep boiling 30min, filter, medicinal residues add entry 200mL once more, decoct also to keep boiling 30min, and filtration, merging filtrate is put coldly, measures its volume.
Precision pipettes each 50mL of decocting liquid respectively, puts in the evaporating dish that is dried to constant weight, and water bath method is put in 105 ℃ of baking ovens and is dried to constant weight, and accurate the title decides, and calculates the yield of solid content.Parallel 3 parts, average.The result is as shown in the table.
Herba Verbenae tradition decoction pieces compares with compression decoction pieces decocting rate
Can know that by the result decocting rate of Herba Verbenae compacting decoction pieces is higher than traditional decoction pieces.Stem, leaf, the more traditional decoction pieces of flower have further fragmentation in the compacting decoction pieces, are beneficial to the fried of composition.
5. Herba Verbenae compression decoction pieces and crude drug toxicity and analgesic activity comparative study
5.1 material and method
5.1.1 experiment medicine
It is some to take by weighing Herba Verbenae compression decoction pieces and traditional decoction pieces extract respectively, is solvent with water, processes maximum acceptable concentration, supplies toxicity test to use; It is some to take by weighing Herba Verbenae respectively, is solvent with water, processes the solution that contains medical material 1g/ml, supplies analgesic experiment to use.
5.1.2 laboratory animal
24 ICR mice ♂ ♀ half and half, 18-22g, the quality certification numbers 2008001615500 is available from Zhejiang University of Traditional Chinese Medicine animal experiment study center.The confession toxicity test uses.
24 ICR mice ♂ ♀ half and half, 18-22g, the quality certification numbers 2008001615500 is available from Zhejiang University of Traditional Chinese Medicine animal experiment study center.The confession analgesic experiment uses.
5.1.3 experimental technique
24 ICR mices are divided into 2 groups at random: Herba Verbenae compression decoction pieces group and Herba Verbenae crude drug group.Adopt Gastric lavage,, observe in the mice 24h and death condition and toxic reaction behind the 7d according to the Cmax and maximum administration volume (0.4ml/10g) administration of Herba Verbenae.The result sees table 1 after carrying out statistical procedures.
24 ICR mices; Be divided into 3 groups at random: normal saline group, Herba Verbenae compression decoction pieces group and Herba Verbenae crude drug group; After adopting gastric infusion 60min, each organizes equal i.p.0.1% acetum 0.1ml/10g, observes mouse writhing reaction times in the 15min; Try to achieve the writhing response suppression ratio, carry out statistical procedures after the result see table 2.Suppression ratio (%)=(1-administration group writhing response number of times/blank control group writhing response number of times) * 100%
5.2. experimental result
Table 1. Herba Verbenae toxicity test result
N＝12
Table 2. Herba Verbenae analgesic experiment result
N＝8，*P＜0.05
5.3 result
Owing to the decimal death condition in preliminary experiment, do not occur, therefore do not carry out the mensuration of LD50.According to maximum acceptable concentration 2.71g/ml (126 multiple doses are equivalent to be grown up) single administration; After the administration 7 days, the decimal mental status was good, hair color is smooth, diet, feces are normal, any toxic reaction and death do not occur; The 8th day sacrifice of animal observed each organ of internal organs and do not had obvious change.Herba Verbenae has remarkable inhibition acetic acid to cause the mouse writhing reaction, does not have significant difference between Herba Verbenae compression decoction pieces and the crude drug.
The following digital proof compression prepared slices of Chinese crude drugs and the traditional decoction pieces equity on chemical substance basis and drug effect:
The above is merely preferred embodiment of the present invention, and is in order to restriction the present invention, not all within spirit of the present invention and principle, any modification of being done, is equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. one kind is compressed the prepared slices of Chinese crude drugs; These compression prepared slices of Chinese crude drugs are raw material with the prepared slices of Chinese crude drugs or crude drug; The said compression prepared slices of Chinese crude drugs are the object of geometrical shape stability; The shape of the prepared slices of Chinese crude drugs or crude drug itself can be seen in the surface of the compression prepared slices of Chinese crude drugs, and the prepared slices of Chinese crude drugs in the compression prepared slices of Chinese crude drugs or the character of crude drug are constant.
2. a kind of compression prepared slices of Chinese crude drugs according to claim 1 is characterized in that the water content of the described compression prepared slices of Chinese crude drugs is lower than 15%.
3. a kind of compression prepared slices of Chinese crude drugs according to claim 2 is characterized in that the water content of the described compression prepared slices of Chinese crude drugs is lower than 5%.
4. a kind of compression prepared slices of Chinese crude drugs according to claim 1 and 2 is characterized in that, said geometry is cylindric, flat column, cuboid or sphere; The single weight of the said compression prepared slices of Chinese crude drugs is 1g-200g.
5. a kind of compression prepared slices of Chinese crude drugs according to claim 1 and 2 is characterized in that, the said compression prepared slices of Chinese crude drugs are cylindric or flat column, and diameter is 5mm-200mm, and thickness is 2mm-100mm.
6. a kind of compression prepared slices of Chinese crude drugs according to claim 5 is characterized in that the diameter of the said compression prepared slices of Chinese crude drugs is 10～180mm; Thickness is 5mm-90mm.
7. method for preparing of compressing the prepared slices of Chinese crude drugs comprises:
(1) gets the prepared slices of Chinese crude drugs or crude drug, clean, remove impurity;
(2) prepared slices of Chinese crude drugs or the crude drug with above-mentioned removal impurity gets into suppression process, promptly gets and compresses the prepared slices of Chinese crude drugs; Technological parameter does, pressure is 30t-200t, and the time is 2s-20s.
8. a kind of method for preparing of compressing the prepared slices of Chinese crude drugs according to claim 7 is characterized in that described pressure is 40t-160t, and the press time is 3s-15.5s.
9. a kind of method for preparing of compressing the prepared slices of Chinese crude drugs according to claim 7 is characterized in that described pressure is 50t-120t, and the press time is 5s-12s.
10. a kind of method for preparing of compressing the prepared slices of Chinese crude drugs according to claim 7 is characterized in that, the medical material or the decoction pieces of pressing for difficulty soften earlier, make its water content at 5%-15%, is getting into suppression process afterwards.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102836180A (en) * | 2012-09-28 | 2012-12-26 | 四川泰乐制药有限公司 | Technology for preparing traditional Chinese medicine decoction pieces through compression and sterilization |
| CN103349679A (en) * | 2013-06-08 | 2013-10-16 | 浙江中医药大学中药饮片有限公司 | Mulberry leaf fluid decoction tablets and preparation method thereof |
| CN103893014A (en) * | 2014-04-24 | 2014-07-02 | 李雪非 | Chinese herbal pieces with regular shape and preparation method thereof |
| CN104873454A (en) * | 2015-04-03 | 2015-09-02 | 邹宇聪 | TCM cakes containing single Chinese herbs and powders of TCM set prescription |
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| CN1193511A (en) * | 1997-03-19 | 1998-09-23 | 张敖何 | Manufacture of Chinese medicinal pills for prescriptions |
| CN1362059A (en) * | 2001-01-05 | 2002-08-07 | 唐山王清任制药有限公司 | Nano Chinese medicine piece and its prepn |
| CN201371588Y (en) * | 2008-12-19 | 2009-12-30 | 成都中医药大学附属医院 | Chinese herbal medicine and Chinese herbal piece pressing machine |
| CN101773524A (en) * | 2010-03-10 | 2010-07-14 | 江西中医学院 | Compressed traditional Chinese medicinal cake, preparation method and application thereof |
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2012
- 2012-05-02 CN CN2012101391427A patent/CN102670667A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1193511A (en) * | 1997-03-19 | 1998-09-23 | 张敖何 | Manufacture of Chinese medicinal pills for prescriptions |
| CN1362059A (en) * | 2001-01-05 | 2002-08-07 | 唐山王清任制药有限公司 | Nano Chinese medicine piece and its prepn |
| CN201371588Y (en) * | 2008-12-19 | 2009-12-30 | 成都中医药大学附属医院 | Chinese herbal medicine and Chinese herbal piece pressing machine |
| CN101773524A (en) * | 2010-03-10 | 2010-07-14 | 江西中医学院 | Compressed traditional Chinese medicinal cake, preparation method and application thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102836180A (en) * | 2012-09-28 | 2012-12-26 | 四川泰乐制药有限公司 | Technology for preparing traditional Chinese medicine decoction pieces through compression and sterilization |
| CN103349679A (en) * | 2013-06-08 | 2013-10-16 | 浙江中医药大学中药饮片有限公司 | Mulberry leaf fluid decoction tablets and preparation method thereof |
| CN103893014A (en) * | 2014-04-24 | 2014-07-02 | 李雪非 | Chinese herbal pieces with regular shape and preparation method thereof |
| CN103893014B (en) * | 2014-04-24 | 2016-09-21 | 李雪非 | Prepared slices of Chinese crude drugs with regular shape and preparation method thereof |
| CN104873454A (en) * | 2015-04-03 | 2015-09-02 | 邹宇聪 | TCM cakes containing single Chinese herbs and powders of TCM set prescription |
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Application publication date: 20120919 |