CN1616013A - Chinese medicine composition for treating dizziness and its preparing and quality control method - Google Patents
Chinese medicine composition for treating dizziness and its preparing and quality control method Download PDFInfo
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Abstract
The Chinese medicine composition is used in treating dizziness, nausea and vomiting, especially Meeniere's syndrome, and has the functions of eliminating phlegm, preventing dizziness, regulating the middle warmer and stopping vomiting. It is prepared with 12 kinds of Chinese medicinal materials, including gastrodia tuber, hooked uncaria, oriental water plantain, pinellia tuber, etc. and contains also beta-cyclodextrin as volatile oil including agent, beta-cyclodextrin as co-solvent for liposoluble component, aspartame as corrective and dextrin as excipient. The quality control method during the preparation process includes thin layer identification of hooked uncaria, white peony root, Chuanxiong rhizome and licorice, and measurement of gastrodin in gastrodia tuber as main material and paeoniflorin in white peony root.
Description
Technical field
The present invention relates to a kind of tool and eliminate the phlegm dizzyly surely, stomach function regulating preventing or arresting vomiting effect is treated dizzyly, feels sick, vomiting, is particularly useful for the medicine of Meniere's syndrome (now claiming Meniere) and preparation thereof, method of quality control, belongs to the field of Chinese medicines.
Background technology
Vertigo is the common disease of middle-aged and elderly people, is sudden more, occurs after wakeing up through being everlasting or after a side is rotated head and neck.Clinical cardinal symptom is a dizziness and tinnitus, and nausea and vomiting is looked thing rotation, perspires in the whole body, to high light noise allergy etc.Hypertensive arteriosclerosis be cause the dizzy commonly encountered diseases of old people because of, because of hypertension causes tiny arteriospasm, arterial lumen attenuates in addition, the vertebra basilar artery can cause blood supply insufficiency because for the treatment of arteriosclerosis hypertension, cause the vestibular system ischemia and bring out dizzy.
Step into the process of aged tendency of population along with Chinese society, the raising of life of elderly person quality will directly have influence on the progress and the development of society, simultaneously because the quickening of development of market economy and modern's rhythm of life, overtime work, the normal potluck that gets married of staying up late, dizzy sickness rate is in rising trend, the forfeiture behavioral competence that causes owing to vestibular dysfunction when especially falling ill has brought great loss and misery for patient's work, life and even family.But it is not a lot of specially to control dizzy medicine at present.Though the vertigo Western medicine is rapid-action, but toxicity, side effect is big, influence people's normal live and work, simultaneously to endocrine, heart, and the influence of liver, renal function easily cause his class disease, and Chinese medicine is characteristic with many active component, many target spots drug effect, curative effect is reliable when the treatment vertigo, really plays the effect of the dizzy outbreak of permanently effective control.Therefore develop the Chinese medicine traditional advantage, exploitation preparation stabilization, drug safety, dosage are accurate, quality controllable, taking convenience, Chinese medicine preparation rapid-action, that curative effect is reliable, bioavailability is high are significant.
Chinese medicine circle adopts XUANYUNNING soup treatment Meniere's syndrome to obtain than promising result more at present, and its preparation process falls behind, and is used as medicine with decoction, and the effective ingredient of Ramulus Uncariae Cum Uncis, Rhizoma Alismatis is a liposoluble constituent, and light water extracts not exclusively, influences drug effect.The present invention carries out the flavour of a drug increase and decrease on the basis of XUANYUNNING soup, adopt advanced technologies simultaneously, adopting cyclodextrin inclusion compound to make the suspension type granule simultaneously to volatile oil has successfully solved the volatile ingredient poor stability and has has easily scattered and disappeared, ferulic acid, ligustilide are unstable in aqueous solution easily to be decomposed, problems such as the easy precipitation of effective ingredient such as the Ramulus Uncariae cum Uncis alkali of poor solubility, isorhynchophylline, corynoxeine, 23-alisol acetyl B, table alisol, atractylone, atractylodes lactone, ligustrazine, ligustilide.
Summary of the invention
The present composition is the medicament of being made by the raw material of following weight portion:
Rhizoma Gastrodiae 120-150 part Ramulus Uncariae Cum Uncis 240-360 part Rhizoma Alismatis 480-720 part Rhizoma Pinelliae 240-360 part
Rhizoma Atractylodis Macrocephalae 300-420 part Poria 300-420 part Radix Paeoniae Alba 240-360 part Caulis Bambusae In Taenia 240-360 part
Rhizoma Chuanxiong 60-120 part Radix Glycyrrhizae 60-120 part Pericarpium Citri Reticulatae 120-240 part Rhizoma Zingiberis Recens 90-180 part
The present composition is the medicament of being made by the raw material of following weight parts:
300 parts of 600 parts of Rhizoma Pinelliaes of 300 portions of Rhizoma Alismatis of 150 parts of Ramulus Uncariae Cum Uncis of Rhizoma Gastrodiae
300 parts of 300 parts of Caulis Bambusae In Taenia of 360 portions of Radix Paeoniae Albas of 360 parts of Poria of the Rhizoma Atractylodis Macrocephalae
135 parts in 180 portions of Rhizoma Zingiberis Recenss of 90 parts of Pericarpium Citri Reticulataes of 90 portions of Radix Glycyrrhizaes of Rhizoma Chuanxiong
Above medicine is made clinically all acceptable forms such as granule, tablet, pill, capsule, injection or oral liquid, tincture, suppository, mixture, powder, lotion, membrane, drop pill through conventional method; Be preferably granule.
The purpose of this invention is to provide a kind of dizzy Chinese medicine composition for the treatment of, another object of the present invention provides a kind of advanced person's of granule of the present invention preparation technology, the present invention also adopts advanced technologies, make the suspension type granule, make the Ramulus Uncariae cum Uncis alkali of poor solubility, isorhynchophylline, corynoxeine, 23-alisol acetyl B, the table alisol, atractylone, atractylodes lactone, ligustrazine, effective ingredient such as ligustilide are hybrid state by hydrotropy or with adjuvant, kept effective ingredient to greatest extent, and the ferulic acid in the preparation, ligustilide is unstable in aqueous solution, by making particulate solid preparation, effective ingredient is significantly improved than former dosage form, improved our curative effect; Two of purpose of the present invention provides a kind of dosage form-granule easily of taking, transport, carry, store, and this dosage form also has taking convenience simultaneously, and the amount of getting is accurate, the characteristics that medicine stability is strong; Another object of the present invention provides the preparation and the method for quality control of this granule.
Granule of the present invention is that crude drug is made by 150 weight portion Rhizoma Gastrodiaes, 300 weight portion Ramulus Uncariae Cum Uncis, 600 weight portion Rhizoma Alismatis, the 300 weight portion Rhizoma Pinelliaes, the 360 weight portion Rhizoma Atractylodis Macrocephalaes, 360 weight portion Poria, the 300 weight portion Radix Paeoniae Albas, 300 weight portion Caulis Bambusae In Taenia, 90 weight portion Rhizoma Chuanxiongs, 90 weight portion Radix Glycyrrhizaes, 180 weight portion Pericarpium Citri Reticulataes, 135 weight portion Rhizoma Zingiberis Recenss, medicament also contains inclusion essential oil agent beta-schardinger dextrin-3.5-6.3 weight portion, the cosolvent beta-schardinger dextrin-45-60 weight portion of liposoluble constituent, contain correctives aspartame 6.4 weight portions, contain forming agent dextrin 480-520 weight portion.
The preparation method of granule of the present invention is as follows:
Take by weighing 150 weight portion Rhizoma Gastrodiaes, 300 weight portion Ramulus Uncariae Cum Uncis, 600 weight portion Rhizoma Alismatis, the 300 weight portion Rhizoma Pinelliaes, the 360 weight portion Rhizoma Atractylodis Macrocephalaes, 360 weight portion Poria, the 300 weight portion Radix Paeoniae Albas, 300 weight portion Caulis Bambusae In Taenia, 90 weight portion Rhizoma Chuanxiongs, 90 weight portion Radix Glycyrrhizaes, 180 weight portion Pericarpium Citri Reticulataes, 135 weight portion Rhizoma Zingiberis Recenss, standby;
More than 12 the flavor, Pericarpium Citri Reticulatae, Rhizoma Zingiberis Recens add the 1500-3000 weight parts water extract volatile oil, medicinal residues are standby; Volatile oil is used 4-7 weight portion beta-schardinger dextrin-inclusion in the time of 30-70 ℃, standby; Remaining medicinal liquid is concentrated into 50 ℃, and to measure relative densities be 1.18～1.20, adds ethanol and make that to contain the alcohol amount be 50%; The medicinal residues and the Radix Paeoniae Alba, Poria, Radix Glycyrrhizae, Caulis Bambusae In Taenia decocts with water secondary, for the first time add water 10000-15000 weight portion, decocted 1-3 hour, add water 8000-15000 weight portion for the second time, decocted 0.5-2 hour, collecting decoction filters concentrating under reduced pressure, pressure is-0.08Mpa, temperature is 50-80 ℃, is concentrated into 50 ℃ of clear paste of measuring relative density 1.18～1.20, puts cold, add ethanol and make that to contain the alcohol amount be 50%, leave standstill, filter filtrate and above-mentioned Pericarpium Citri Reticulatae, the pure liquid of Rhizoma Zingiberis Recens merges, decompression recycling ethanol, pressure is-0.08Mpa that temperature is 50-80 ℃, is concentrated into 50 ℃ and measures relative density 1.18～1.20; Rhizoma Gastrodiae is fried in shallow oil in addition, decoct with water secondary, add water 800-2000 weight portion for the first time, decocted 1-3 hour, add for the second time water 800-1500 weight portion, decocted 0.5-2 hour, collecting decoction filters, concentrating under reduced pressure, pressure is-0.08Mpa that temperature is 50-80 ℃, is concentrated into 50 ℃ of clear paste of measuring relative density 1.18～1.20, put cold, add ethanol and make that to contain the alcohol amount be 50%, leave standstill, filter, decompression filtrate recycling ethanol, pressure is-0.08Mpa that temperature is 50-80 ℃, is concentrated into 50 ℃ and measures relative density 1.18～1.20; The five tastes such as all the other Rhizoma Alismatis are according to the percolation (first appendix IO of version pharmacopeia in 2000) under fluid extract and the extractum item, with 50% alcohol dipping after 24 hours, percolation slowly, flow velocity is 3～5ml/min, percolation is closely colourless to the liquid of filtering, the liquid decompression recycling ethanol of filtering, pressure is-0.08Mpa that temperature is 50-80 ℃, adds beta-schardinger dextrin-45g, stir evenly, be concentrated into 50 ℃ and measure relative density 1.18～1.20.Above-mentioned three kinds of concentrated solutions are merged, stir evenly, mesh screen filters, and concentrates, and adds above-mentioned Pericarpium Citri Reticulatae, Rhizoma Zingiberis Recens volatile oil clathrate, dextrin and aspartame, and mixing is granulated, drying, and granulate, promptly.
Above-mentioned granulation comprises method of granulating such as dry granulation, wet granulation, spray granulation.
The discrimination method of granule of the present invention, concrete steps are:
(1) get this product powder 8g, add ethyl acetate 60ml, strong aqua ammonia 6ml, supersound extraction 30 minutes is got upper strata liquid, and evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution.Hook taking rattan control medicinal material powder 2g adds ethyl acetate 20ml in addition, strong aqua ammonia 2ml, and supersound extraction 30 minutes filters, and filtrate is put in the separatory funnel, gets upper strata liquid, and evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, makes control medicinal material solution.According to thin layer chromatography reference " 2000 editions appendix VIB tests of Chinese pharmacopoeia, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with ratio is that the subnatant of 20: 1: 1 methylene chloride-methanol-ammonia is developing solvent, launch, take out, dry, spray is inspected under the daylight lamp with the improvement bismuth potassium iodide test solution.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical orange red speckle.
(2) get this product powder 5g, add water 30ml supersound extraction 20 minutes, filter, filtrate is put in the separatory funnel, with ethyl acetate extraction 3 times, each 10ml discards the water saturated n-butanol extraction of reuse 3 times, each 10ml merges n-butyl alcohol liquid, and evaporate to dryness, residue add water 10ml makes dissolving, on the polyamide column handled well, the polyamide consumption is 15ml, the wet method upper prop, internal diameter 15-20mm washes with water to colourless, collects water lotion, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets the peoniflorin reference substance, adds methanol and makes every 1ml and contain 1mg solution, in contrast product solution.According to thin layer chromatography reference " 2000 editions appendix VIB tests of Chinese pharmacopoeia, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with ratio is 40: 5: 10: chloroform-ethyl acetate of 0.2-methanol-formic acid is 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 the corresponding position of reference substance chromatograph on, show identical aubergine speckle.
(3) get this product powder 5g, add 40ml ethyl acetate supersound extraction 20 minutes, filter, filtrate is put evaporate to dryness in the water-bath, and residue adds ethyl acetate 0.5ml makes dissolving, as need testing solution.Other gets Rhizoma Chuanxiong control medicinal material powder 0.05g, add 40ml ethyl acetate supersound extraction 20 minutes, filter, filtrate is put evaporate to dryness in the water-bath, residue adds ethyl acetate 0.5ml makes dissolving, make control medicinal material solution, according to thin layer chromatography reference " 2000 editions appendix VIB tests of Chinese pharmacopoeia, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be 10: 1 petroleum ether (60～90 ℃) with ratio: ethyl acetate is developing solvent, launch, take out, dry, put under the uviol lamp 365nm and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
(4) get this product powder 5g, add water saturated n-butyl alcohol 40ml, supersound extraction 30 minutes, filter, filtrate evaporate to dryness, residue add water 10ml makes dissolving, on the polyamide column handled well, the polyamide consumption is 15ml, the wet method upper prop, internal diameter 15-20mm washes with water earlier to colourless, continues with the 30ml70% ethanol elution, collect eluent, put evaporate to dryness in the water-bath, residue adds methanol 1ml makes dissolving, as need testing solution.Extracting liquorice control medicinal material powder 0.5g adds 30ml water-saturated n-butanol supersound extraction 20 minutes in addition, filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution.According to thin layer chromatography reference " 2000 editions appendix VIB tests of Chinese pharmacopoeia, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with ratio is that methylene chloride-methanol-water of 40: 10: 1 is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and putting 105 ℃, to be heated to the speckle colour developing clear.In the test sample chromatograph, respectively with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
The content assaying method of granule of the present invention, concrete steps are:
(1) the concrete parameter of measuring the gastrodin content in its monarch drug Rhizoma Gastrodiae is:
The preparation of reference substance solution: it is an amount of that precision takes by weighing the gastrodine reference substance, adds methanol and make the solution that contains 40 μ g among every 1ml, in contrast product solution;
The preparation of need testing solution: get powder 1.0g, accurate claim surely, put in the 25ml measuring bottle, add 50% methanol 20ml, supersound extraction 30min is put coldly, and standardize solution shakes up, and high speed centrifugation 10 minutes is got supernatant, promptly;
Chromatographic condition: with octadecylsilane chemically bonded silica is filler;
Volume ratio is that 12: 88 methanol-0.1% sour water is a mobile phase;
Detect wavelength 221nm;
Algoscopy: accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing, inject hplc determination.
(2) the concrete parameter of measuring the paeoniflorin content in its Radix Paeoniae Alba is:
The preparation of reference substance solution: it is an amount of that precision takes by weighing the peoniflorin reference substance, adds methanol and make the solution that contains 0.230mg among every 1ml, in contrast product solution.
The preparation of need testing solution: get powder 2.5g, accurate claim surely, put in the 25ml measuring bottle, add 80% methanol 20ml, supersound extraction 40min is put coldly, and standardize solution shakes up, and centrifugal 10 minutes of 10000rpm gets supernatant, promptly.
Chromatographic condition: with octadecylsilane chemically bonded silica is filler;
Volume ratio is that 30: 70 methanol-0.05% sour water is a mobile phase;
Detect wavelength 230nm; Its sour water is that the aqueous solution of organic acid or phosphoric acid is as acetic acid, trifluoroacetic acid, phosphoric acid etc.
The invention provides in the monarch drug Rhizoma Gastrodiae in the gastrodine and the Radix Paeoniae Alba content of paeoniflorin and measure, improved the quality control of medicine, guaranteed preparation homogeneity and effectiveness.
Granule of the present invention is used beta-schardinger dextrin-inclusion technology, with the volatile oil component inclusion, thereby reduce the loss of volatile oil, guaranteed the stable of its content, also adopt beta-schardinger dextrin-inclusion technology, hydrotropy technology simultaneously, inclusions such as water insoluble active ingredient such as Ramulus Uncariae cum Uncis alkali, isorhynchophylline, corynoxeine, 23-alisol acetyl B, table alisol, atractylone, atractylodes lactone, ligustilide were entered after original alcohol extraction was concentrated, reduce loss of active ingredients, improve curative effect of medication, and improved the preparation mouthfeel to a certain extent.
The specific embodiment
The preparation of embodiment one granule of the present invention
Weighting raw materials Rhizoma Gastrodiae 150g, Ramulus Uncariae Cum Uncis 300g, Rhizoma Alismatis 600g, Rhizoma Pinelliae 300g, Rhizoma Atractylodis Macrocephalae 360g, Poria 360g, Radix Paeoniae Alba 300g, Caulis Bambusae In Taenia 300g, Rhizoma Chuanxiong 90g, Radix Glycyrrhizae 90g, Pericarpium Citri Reticulatae 180g, Rhizoma Zingiberis Recens 135g
More than 12 the flavor, Pericarpium Citri Reticulatae, Rhizoma Zingiberis Recens add water 2835g extract volatile oil, medicinal residues are standby; Volatile oil is used 5g beta-schardinger dextrin-inclusion in the time of 50 ℃, standby; Remaining medicinal liquid is concentrated into relative density 1.18 (50 ℃), adds ethanol and makes that to contain the alcohol amount be 50%; The medicinal residues and the Radix Paeoniae Alba, Poria, Radix Glycyrrhizae, Caulis Bambusae In Taenia decoct with water secondary, add water 13650g for the first time, decoct 1.5 hours, for the second time add water 10920g, decocted collecting decoction 1 hour, filter, concentrating under reduced pressure (0.08Mpa, 60 ℃) is to the clear paste of relative density 1.18 (50 ℃), put coldly, add ethanol and make and contain the alcohol amount and reach 50%, leave standstill, filter, the pure liquid of filtrate and above-mentioned Pericarpium Citri Reticulatae, Rhizoma Zingiberis Recens merges decompression recycling ethanol (0.08Mpa, 60 ℃), be concentrated into relative density 1.18 (50 ℃); Rhizoma Gastrodiae is fried in shallow oil in addition, decocts with water secondary, adds water 1500g for the first time, decocted 1.5 hours, and added water 1200g for the second time, decocted 1 hour, collecting decoction filters concentrating under reduced pressure (0.08Mpa, 60 ℃) to the clear paste of relative density 1.18 (50 ℃), put coldly, add ethanol and make and contain the alcohol amount and reach 50%, leave standstill, filter, the pure liquid of filtrate and above-mentioned Pericarpium Citri Reticulatae, Rhizoma Zingiberis Recens merges, decompression recycling ethanol (0.08Mpa, 60 ℃) is concentrated into relative density 1.18 (50 ℃); The five tastes such as all the other Rhizoma Alismatis are according to the percolation (first appendix IO of version pharmacopeia in 2000) under fluid extract and the extractum item, with 50% alcohol dipping after 24 hours, percolation slowly, flow velocity is 5ml/min, percolation is closely colourless to the liquid of filtering, the liquid decompression recycling ethanol of filtering (0.08Mpa, 60 ℃), add beta-schardinger dextrin-45g, be concentrated into relative density 1.18 (50 ℃).
Above-mentioned three kinds of concentrated solutions are merged, stir evenly, mesh screen filters, and concentrates, and adds above-mentioned Pericarpium Citri Reticulatae, Rhizoma Zingiberis Recens volatile oil inclusion complex, dextrin 500g and aspartame 6.4g, and mixing is granulated, drying, and granulate, promptly.
The selection of embodiment two Pericarpium Citri Reticulataes, Rhizoma Zingiberis Recens volatile oil extraction conditions
For selecting Pericarpium Citri Reticulatae, Rhizoma Zingiberis Recens volatile oil optimum extraction process condition, get 600 gram Pericarpium Citri Reticulataes and 450 gram Rhizoma Zingiberis Recens medical materials, totally 9 parts, to the amount of water that extracts, extraction time and salt adding amount have carried out the orthogonal test examination, see Table 1.For investigating index, carried out 9 tests with volatile oil yield (v/w, v are the volatile oil volume, and w is a quality of medicinal material), each factor level sees Table 1.
Table 1 Pericarpium Citri Reticulatae, Rhizoma Zingiberis Recens volatile oil extract quadrature table as a result
R 0.66 0.15 0.06
Table 2 Pericarpium Citri Reticulatae, Rhizoma Zingiberis Recens volatile oil extract the orthogonal test analysis of variance table
The mean square F work of soruces of variation quadratic sum degree of freedom property
Amount of water 0.08 2 0.04 412.00 is remarkable
Extraction time 0.01 2 0.00 25.00 is remarkable
Salt adding amount 0.00 2 0.00 4.00 is not remarkable
Error 0.00 2 0.00
By the analysis of variance table of table 2 as can be seen: there are appreciable impact amount of water and extraction time to the volatile oil yield, and salt adding amount is not remarkable to the influence of volatile oil yield.Orthogonal experiments by table 3 shows, wherein K
2a＞K
3a＞K
1aSo factor A selects level 2, promptly selecting amount of water is 8 times of amounts; K wherein
2b=K
3b＞K
1b, for saving the energy, so factor B selects level 2, i.e. the selective extraction time is 12 hours; Not remarkable because of salt adding amount again to the influence of volatile oil yield, and K
2c=K
1c＞K
3cSo select not with salt.
Therefore, the optimum extraction process of Pericarpium Citri Reticulatae, Rhizoma Zingiberis Recens volatile oil is: medical material adds the water of 8 times of amounts, steam distillation 12 hours.
The selection of embodiment three volatile oil inclusion conditions
Because this medicine contains the volatile oil that extracts in Pericarpium Citri Reticulatae, the Rhizoma Zingiberis Recens, in order to reduce the loss of volatile oil as far as possible, so adopt beta-schardinger dextrin-inclusion technology to make its inclusion.In order to select the optimum condition of inclusion, designed orthogonal test.Select L9 (3 for use
4) orthogonal table, as investigating index, having carried out 9 tests with the inclusion rate of volatile oil, each factor level sees Table 3.
Table 3 volatile oil beta-cyclodextrin inclusion quadrature is table as a result
K3 193.60 165.50 194.10
R 14.10 59.00 8.90
Inclusion rate=[amount of volatile oil (g) in the inclusion complex/volatile oil addition (g)] * 100%
Table 4 volatile oil beta-cyclodextrin inclusion orthogonal test analysis of variance table
The mean square F work of soruces of variation quadratic sum degree of freedom property
β-CD: oil 39.50 2 19.75 7.77 is not remarkable
The inclusion temperature (℃) 610.07 2 305.03 120.04 remarkable
It is not remarkable to stir the Pan time 13.40 2 6.70 2.64
Error 5.08 2 2.54
By the analysis of variance table of table 4 as can be seen: by intuitive analysis as seen, the order that influences the volatile oil inclusion is: the proportioning＞mixing time of inclusion temperature＞β-CD and oil, and with inclusion temperature effect maximum.By the variance analysis of table 4 as can be seen, the inclusion temperature has the significance influence to the volatile oil inclusion, and β-CD does not have the significance influence with the proportioning and the inclusion time of oil to the volatile oil inclusion, and wherein β-CD is 5 with the proportioning of oil: 1-9: 1, the inclusion temperature is 40-50 ℃, and stirring the Pan time is 15-30min.Wherein best inclusion process conditions are: A
2B
2C
2The proportioning that is β-CD and oil is 7: 1, and the inclusion temperature is 50 ℃, and stirring the Pan time is 30min.
Embodiment four beta-schardinger dextrin-s disperse the selection of hydrotropy condition
Because contained active component water-soluble is relatively poor in the our alcohol extract, the preparation melting is bad, so adopt beta-schardinger dextrin-to make its better dispersion, increases the melting of granule.In order to select the dispersive optimum condition of beta-schardinger dextrin-, three comparative tests have been carried out.
Hook taking rattan 900g, Rhizoma Alismatis 1800g, Rhizoma Pinelliae 900g, Rhizoma Atractylodis Macrocephalae 1080g, Rhizoma Chuanxiong 270g, with five tastes medicinal material coarse powder with 50% alcohol dipping after 24 hours, percolation slowly, percolation is closely colourless to the liquid of filtering, ethanol is reclaimed in the liquid of filtering decompression (0.08Mpa,＜80 ℃), will reclaim three parts of liquid div in par aeq, add not commensurability beta-schardinger dextrin-respectively, test after stirring evenly.As investigating index, investigate its influence with 23-alisol acetyl B, the results are shown in Table 5 the retention rate of 23-alisol acetyl B.
Table 5 beta-schardinger dextrin-consumption is to the influence of 23-alisol acetyl B retention rate
The result shows, solubilization-aid effect was undesirable when the beta-schardinger dextrin-consumption was 15g, when increasing to 45g, the retention rate of index components 23-alisol acetyl B is higher, when increasing to 60g again as the beta-schardinger dextrin-consumption, the retention rate difference of index components is very little during with 45g, is 45-60g so select the consumption of beta-schardinger dextrin-, and the best is 45g.
Therefore, to disperse the consumption of hydrotropy be 45g to the concentrated medicament beta-schardinger dextrin-of five tastes medical material such as Rhizoma Alismatis.
Mainly contain effective component content in the embodiment five granule different process preparations of the present invention relatively
We have carried out the contrast experiment for the effect of investigating beta-cyclodextrin inclusion compound technology, under the constant situation of other condition with first group adopt common preparation method with five tastes medical material percolation such as Rhizoma Alismatis, concentrate, do not add beta-schardinger dextrin-and disperse hydrotropy, the second group two groups concentrated medicament beta-schardinger dextrin-s with five tastes medical materials such as Rhizoma Alismatis disperse hydrotropy, with the legal system granule, getting granule I and granule II respectively, is index with Ramulus Uncariae cum Uncis alkali and 23-alisol acetyl B, measure content in two groups of granules respectively, experimental result such as table 6.
The assay comparative test of table 6 granule
Project indicator composition
Ramulus Uncariae cum Uncis alkali 23-alisol acetyl B
Granule I 3.35 0.46
Granule II 10.27 1.36
Granule II is than the raising rate (%) 206.57 195.65 of granule I
Ramulus Uncariae cum Uncis alkali, 23-alisol acetyl B content of effective mensuration among the granule I of the present invention are shown, above-mentioned two kinds of content of effective are compared with granule I and are significantly improved among the granule II, granule II group has adopted the inclusion hydrotropy effect of beta-schardinger dextrin-to make particularly effective ingredient such as Ramulus Uncariae cum Uncis alkali, 23-alisol acetyl B reservation of effective ingredient in the former mixture, make the suspension type granule, the composition that extracts medicinal liquid is fully kept, and active constituent content obviously increases.And effective ingredient particularly Ramulus Uncariae cum Uncis alkali, 23-alisol acetyl B among the former side because of their poorly water-soluble is separated out, lose when medicinal liquid concentrates after-filtration, have influenced content of effective.
Embodiment five XUANYUNNING and granule vertigo of the present invention experimental study
In order to compare the power of XUANYUNNING and the particulate pharmacological action of the present invention, get and firmly to set up the mice that escapes the electric shock reflection and at first measure postrotational escape electric shock reflex latency (rotating speed 390r/min before the administration, each rotation 1min), measure altogether 3 times, before and after twice measurement 30min at interval, with administration 3 times the meansigma methods of measurement result as administration before the result.Use gastric infusion (ig) mode then, after the administration 45,75,105,150,195min measures the incubation period that the electric shock reflection is escaped in the rotation back respectively.The result is to represent incubation period.
Table 7 XUANYUNNING and vertigo experimental result of the present invention (X ± S)
Escape the electric shock reflex latency before and after the dosed administration
Group n
Blanking time (min) after (min) administration before the administration
(g/kg)
45 75 105 150 195
Physiology NS 14 90.5 ± 26.8 90.5 ± 26.8 102.6 ± 40.2 101.6 ± 34.8 103.8 ± 36.8 95.3 ± 33.2
The saline group
Hydrochloric acid ground fragrant 0.0065 14 98.1 ± 24.0 32.5 ± 13.7 34.4 ± 13.4 77.3 ± 38.0 99.7 ± 36.8 102.6 ± 23.7
Buddhist nun's multi-disc
XUANYUNNING 15.825 14 94.8 ± 18.6 70.5 ± 23.4
*80.0 ± 24.4
*85.9 ± 38.1 90.5 ± 32.4 102.5 ± 42.8
The present invention 15.825 14 98.3 ± 23.4 33.5 ± 14.1
*34.9 ± 12.6
*65.5 ± 37.6 95.9 ± 28.8 100.6 ± 25.8
Grain
P＜0.01, utmost point significant difference,
*P＜0.05, significant difference.
The result shows, compares with XUANYUNNING, and granule of the present invention can obviously shorten the incubation period that mice escapes the electric shock reflection, shows the vertigo effect that it is good.
The discriminating of Ramulus Uncariae Cum Uncis in embodiment six granules of the present invention
Get this product powder 8g, add ethyl acetate 60ml, strong aqua ammonia 6ml, supersound extraction 30 minutes filters, and filtrate is put in the separatory funnel, gets upper strata liquid, and evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution.Hook taking rattan control medicinal material powder 2g adds ethyl acetate 20ml in addition, and strong aqua ammonia 2ml shines medical material solution in pairs with legal system.According to thin layer chromatography (" 2000 editions appendix VIB of Chinese pharmacopoeia) test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, subnatant with methylene chloride-methanol-water (20: 1: 1) is developing solvent, launch, take out, dry, spray is inspected under the daylight lamp with the improvement bismuth potassium iodide test solution.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical orange red speckle.
The discriminating of the Radix Paeoniae Alba in embodiment seven granules of the present invention
Get this product powder 5g, add water 30ml supersound extraction 20 minutes, filter, filtrate is put in the separatory funnel, with ethyl acetate extraction 3 times, each 10ml discards the water saturated n-butanol extraction of reuse 3 times, each 10ml merges n-butyl alcohol liquid, evaporate to dryness, residue adds water 10ml makes dissolving, on the polyamide column handled well (the polyamide consumption is 15ml, the wet method upper prop, internal diameter 15-20mm), washes with water, collect water lotion to colourless, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.It is an amount of that other gets the peoniflorin reference substance, adds methanol and make the reference substance solution that every 1ml contains 1mg.According to thin layer chromatography (" 2000 editions appendix VIB of Chinese pharmacopoeia) test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-methanol-formic acid (40: 5: 10: 0.2) 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 the corresponding position of reference substance chromatograph on, show identical aubergine speckle.
The discriminating of Rhizoma Chuanxiong in embodiment eight granules of the present invention
Get this product powder 5g, add ethyl acetate 40ml supersound extraction 20 minutes, filter, filtrate is put evaporate to dryness in the water-bath, and residue adds ethyl acetate 0.5ml makes dissolving, as need testing solution.Other gets Rhizoma Chuanxiong control medicinal material powder 0.05g, shine medical material solution in pairs with legal system, according to thin layer chromatography (" 2000 editions appendix VIB of Chinese pharmacopoeia) test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (60～90 ℃): ethyl acetate (10: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, respectively with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
The discriminating of Radix Glycyrrhizae in embodiment nine granules of the present invention
Get this product powder 5g, add water-saturated n-butanol 40ml, supersound extraction 30 minutes, filter, filtrate evaporate to dryness, residue add water 10ml dissolving, on the polyamide column (the polyamide consumption is 15ml, wet method upper prop, internal diameter 15-20mm) handled well, wash with water earlier to colourless, continue with the 30ml70% ethanol elution, collect eluent, put evaporate to dryness in the water-bath, residue adds methanol 1ml makes dissolving, as need testing solution.Extracting liquorice control medicinal material powder 0.5g adds 30ml water-saturated n-butanol supersound extraction 20 minutes in addition, filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, as Radix Glycyrrhizae control medicinal material solution.According to thin layer chromatography (" 2000 editions appendix VIB of Chinese pharmacopoeia) test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with methylene chloride-methanol-water (40: 10: 1) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and putting 105 ℃, to be heated to the speckle colour developing clear.In the test sample chromatograph, respectively with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Gastrodin content is measured in embodiment ten granules of the present invention
Measure according to high performance liquid chromatography (" 2000 editions appendix VID of Chinese pharmacopoeia).
Chromatographic condition and system suitability test:
Agilent 1100 high performance liquid chromatographs, QuatPump pump, VWD ultraviolet-visible detector, the full-automatic injector of Agilent, Agilent chromatographic work station.
With octadecylsilane chemically bonded silica is filler, and methanol-0.1% sour water was a mobile phase in 12: 88; Detect wavelength 221nm, flow velocity 1.0ml/min, 30 ℃ of column temperatures, number of theoretical plate calculate by gastrodine should be not less than 3000.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the gastrodine reference substance, adds methanol and make the solution that contains 40 μ g among every 1ml, in contrast product solution.
The preparation of need testing solution: get content under this product content uniformity item, porphyrize is got powder 1.0g, and accurate the title decides, and puts in the 25ml measuring bottle, add 50% methanol 20ml, supersound extraction 30min, put cold, standardize solution, shake up, high speed centrifugation (10000rpm) 10 minutes is got supernatant, promptly.
Algoscopy: accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing, inject hplc determination, calculate, promptly.
This product contains the gastrodine meter for every bag, must not be less than 3.5mg.
Paeoniflorin content is measured in embodiment 11 granules of the present invention
Measure according to high performance liquid chromatography (" 2000 editions one appendix VI D of Chinese pharmacopoeia).
Chromatographic condition and system suitability test:
Agilent 1100 high performance liquid chromatographs, QuatPump pump, VWD ultraviolet-visible detector, the full-automatic injector of Agilent, Agilent chromatographic work station.
With octadecylsilane chemically bonded silica is filler, and methanol-0.05% sour water was a mobile phase in 30: 70; Detect wavelength 230nm, flow velocity 1.0ml/min, 30 ℃ of column temperatures, number of theoretical plate calculate by peoniflorin should be not less than 3000.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the peoniflorin reference substance, adds methanol and make the solution that contains 0.230mg among every 1ml, in contrast product solution.
The preparation of need testing solution: get content under this product content uniformity item, porphyrize is got powder 2.5g, and accurate the title decides, and puts in the 25ml measuring bottle, add 80% methanol 20ml, supersound extraction 40min, put cold, standardize solution, shake up, high speed centrifugation (10000rpm) 10 minutes is got supernatant, promptly.
Algoscopy: accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing, inject hplc determination, calculate, promptly.
This product contains the peoniflorin meter for every bag, must not be less than 7.5mg.
Embodiment 12
Rhizoma Gastrodiae 120g Ramulus Uncariae Cum Uncis 360g Rhizoma Alismatis 720g Rhizoma Pinelliae 360g
Rhizoma Atractylodis Macrocephalae 420g Poria 420g Radix Paeoniae Alba 360g Caulis Bambusae In Taenia 360g
Rhizoma Chuanxiong 120g Radix Glycyrrhizae 120g Pericarpium Citri Reticulatae 240g Rhizoma Zingiberis Recens 180g
More than 12 the flavor, Pericarpium Citri Reticulatae, Rhizoma Zingiberis Recens add water 1500g extract volatile oil, medicinal residues are standby; Volatile oil is used 7g beta-schardinger dextrin-inclusion in the time of 30 ℃, standby; Remaining medicinal liquid is concentrated into relative density 1.18 (50 ℃), adds ethanol and makes that to contain the alcohol amount be 50%; The medicinal residues and the Radix Paeoniae Alba, Poria, Radix Glycyrrhizae, Caulis Bambusae In Taenia decoct with water secondary, add water 10000g for the first time, decoct 3 hours, for the second time add water 15000g, decocted collecting decoction 0.5 hour, filter, concentrating under reduced pressure (0.08Mpa, 60 ℃) is to the clear paste of relative density 1.18 (50 ℃), put coldly, add ethanol and make and contain the alcohol amount and reach 50%, leave standstill, filter, the pure liquid of filtrate and above-mentioned Pericarpium Citri Reticulatae, Rhizoma Zingiberis Recens merges decompression recycling ethanol (0.08Mpa, 60 ℃), be concentrated into relative density 1.18 (50 ℃); Rhizoma Gastrodiae is fried in shallow oil in addition, decocts with water secondary, adds water 1500g for the first time, decocted 1.5 hours, and added water 1200g for the second time, decocted 1 hour, collecting decoction filters concentrating under reduced pressure (0.08Mpa, 60 ℃) to the clear paste of relative density 1.18 (50 ℃), put coldly, add ethanol and make and contain the alcohol amount and reach 50%, leave standstill, filter, the pure liquid of filtrate and above-mentioned Pericarpium Citri Reticulatae, Rhizoma Zingiberis Recens merges, decompression recycling ethanol (0.08Mpa, 60 ℃) is concentrated into relative density 1.18 (50 ℃); The five tastes such as all the other Rhizoma Alismatis are according to the percolation (first appendix IO of version pharmacopeia in 2000) under fluid extract and the extractum item, with 50% alcohol dipping after 24 hours, percolation slowly, flow velocity is 5ml/min, percolation is closely colourless to the liquid of filtering, the liquid decompression recycling ethanol of filtering (0.08Mpa, 60 ℃), add beta-schardinger dextrin-45g, be concentrated into relative density 1.18 (50 ℃).
Above-mentioned three kinds of concentrated solutions are merged, concentrate, drying adds above-mentioned Pericarpium Citri Reticulatae, Rhizoma Zingiberis Recens volatile oil inclusion complex, dextrin 300g and aspartame 4.6g, and mixing is granulated, drying, and granulate, promptly.
Embodiment 13
Rhizoma Gastrodiae 150g Ramulus Uncariae Cum Uncis 240g Rhizoma Alismatis 720g Rhizoma Pinelliae 360g
Rhizoma Atractylodis Macrocephalae 420g Poria 420g Radix Paeoniae Alba 360g Caulis Bambusae In Taenia 360g
Rhizoma Chuanxiong 120g Radix Glycyrrhizae 120g Pericarpium Citri Reticulatae 240g Rhizoma Zingiberis Recens 180g
More than 12 the flavor, Pericarpium Citri Reticulatae, Rhizoma Zingiberis Recens add 3000 weight parts waters extract volatile oil, medicinal residues are standby; Volatile oil in the time of 70 ℃ with 4 weight portion beta-schardinger dextrin-inclusions, standby; Remaining medicinal liquid is concentrated into 50 ℃, and to measure relative densities be 1.18～1.20, adds ethanol and make that to contain the alcohol amount be 50%; The medicinal residues and the Radix Paeoniae Alba, Poria, Radix Glycyrrhizae, Caulis Bambusae In Taenia decoct with water secondary, for the first time add water 15000 weight portions, decocted 1 hour, add water 8000 weight portions for the second time, decocted 2 hours, collecting decoction filters concentrating under reduced pressure, pressure is-0.08Mpa, temperature is 50-80 ℃, is concentrated into 50 ℃ of clear paste of measuring relative density 1.18～1.20, puts cold, add ethanol and make that to contain the alcohol amount be 50%, leave standstill, filter, the pure liquid of filtrate and above-mentioned Pericarpium Citri Reticulatae, Rhizoma Zingiberis Recens merges, decompression recycling ethanol, pressure is-0.08Mpa that temperature is 50-80 ℃, is concentrated into 50 ℃ and measures relative density 1.18～1.20; Rhizoma Gastrodiae is fried in shallow oil in addition, decocts with water secondary, adds water 800 weight portions for the first time, decocts 3 hours, for the second time add water 800 weight portions, decocted 2 hours, collecting decoction filters, concentrating under reduced pressure, pressure are-0.08Mpa that temperature is 50-80 ℃, be concentrated into 50 ℃ of clear paste of measuring relative densities 1.18～1.20, put coldly, add ethanol and make that to contain the alcohol amount be 50%, leave standstill, filter decompression filtrate recycling ethanol, pressure is-0.08Mpa that temperature is 50-80 ℃, is concentrated into 50 ℃ and measures relative density 1.18～1.20; The five tastes such as all the other Rhizoma Alismatis are according to the percolation (first appendix IO of version pharmacopeia in 2000) under fluid extract and the extractum item, with 50% alcohol dipping after 24 hours, percolation slowly, flow velocity is 3～5ml/min, percolation is closely colourless to the liquid of filtering, the liquid decompression recycling ethanol of filtering, pressure is-0.08Mpa that temperature is 50-80 ℃, adds beta-schardinger dextrin-45g, stir evenly, be concentrated into 50 ℃ and measure relative density 1.18～1.20.Above-mentioned three kinds of concentrated solutions are merged, stir evenly, drying adds above-mentioned Pericarpium Citri Reticulatae, Rhizoma Zingiberis Recens volatile oil clathrate, dextrin and aspartame, mixing, and dry granulation is granulated, granulate, promptly.
Claims (10)
1, a kind ofly treat dizzy Chinese medicine preparation, it is characterized in that it is to be made by the raw material of following weight portion:
Rhizoma Gastrodiae 120-150 part Ramulus Uncariae Cum Uncis 240-360 part Rhizoma Alismatis 480-720 part Rhizoma Pinelliae 240-360 part
Rhizoma Atractylodis Macrocephalae 300-420 part Poria 300-420 part Radix Paeoniae Alba 240-360 part Caulis Bambusae In Taenia 240-360 part
Rhizoma Chuanxiong 60-120 part Radix Glycyrrhizae 60-120 part Pericarpium Citri Reticulatae 120-240 part Rhizoma Zingiberis Recens 90-180 part
2, preparation as claimed in claim 1 is characterized in that it is to be made by the raw material of following weight parts:
300 parts of 600 parts of Rhizoma Pinelliaes of 300 portions of Rhizoma Alismatis of 150 parts of Ramulus Uncariae Cum Uncis of Rhizoma Gastrodiae
300 parts of 300 parts of Caulis Bambusae In Taenia of 360 portions of Radix Paeoniae Albas of 360 parts of Poria of the Rhizoma Atractylodis Macrocephalae
135 parts in 180 portions of Rhizoma Zingiberis Recenss of 90 parts of Pericarpium Citri Reticulataes of 90 portions of Radix Glycyrrhizaes of Rhizoma Chuanxiong
3, Chinese medicine preparation as claimed in claim 1 or 2 is characterized in that said medicament is acceptable clinically all dosage forms.
4, Chinese medicine preparation according to claim 3 is characterized in that said medicament is a granule.
5, the preparation method of Chinese medicine preparation according to claim 4 is characterized in that it is to be prepared from by following concrete steps:
A. it is standby to take by weighing 150 parts in Rhizoma Gastrodiae, 300 parts of Ramulus Uncariae Cum Uncis, 600 parts of Rhizoma Alismatis, 300 parts of the Rhizoma Pinelliaes, 360 parts of the Rhizoma Atractylodis Macrocephalaes, 360 parts in Poria, 300 parts of the Radix Paeoniae Albas, 300 parts of Caulis Bambusae In Taenia, 90 parts of Rhizoma Chuanxiongs, 90 parts in Radix Glycyrrhizae, 180 parts of Pericarpium Citri Reticulataes, 135 parts in Rhizoma Zingiberis Recens;
B. above 12 flavors, Pericarpium Citri Reticulatae, Rhizoma Zingiberis Recens add 1,500 3000 weight parts waters extract volatile oil, medicinal residues are standby; Volatile oil is used 4-7 weight portion beta-schardinger dextrin-inclusion in the time of 30 70 ℃, standby; Remaining medicinal liquid is concentrated into 50 ℃, and to measure relative densities be 1.18～1.20, adds ethanol and make that to contain the alcohol amount be 50%; The medicinal residues and the Radix Paeoniae Alba, Poria, Radix Glycyrrhizae, Caulis Bambusae In Taenia decocts with water secondary, for the first time add water 10000-15000 weight portion, decocted 13 hours, add water 8,000 15000 weight portions for the second time, decocted 0.5 2 hours, collecting decoction filters concentrating under reduced pressure, pressure is-0.08Mpa, temperature is 50-80 ℃, is concentrated into 50 ℃ of clear paste of measuring relative density 1.18～1.20, puts cold, add ethanol and make that to contain the alcohol amount be 50%, leave standstill, filter filtrate and above-mentioned Pericarpium Citri Reticulatae, the pure liquid of Rhizoma Zingiberis Recens merges, decompression recycling ethanol, pressure is-0.08Mpa that temperature is 50-80 ℃, is concentrated into 50 ℃ and measures relative density 1.18～1.20; Rhizoma Gastrodiae is fried in shallow oil in addition, decoct with water secondary, add water 800 2000 weight portions for the first time, decocted 13 hours, add for the second time water 800-1500 weight portion, decocted 0.5 2 hours, collecting decoction filters, concentrating under reduced pressure, pressure is-0.08Mpa that temperature is 50-80 ℃, is concentrated into 50 ℃ of clear paste of measuring relative density 1.18～1.20, put cold, add ethanol and make that to contain the alcohol amount be 50%, leave standstill, filter, decompression filtrate recycling ethanol, pressure is-0.08Mpa that temperature is 50-80 ℃, is concentrated into 50 ℃ and measures relative density 1.18～1.20; The five tastes such as all the other Rhizoma Alismatis are according to the percolation (first appendix IO of version pharmacopeia in 2000) under fluid extract and the extractum item, with 50% alcohol dipping after 24 hours, percolation slowly, flow velocity is 3～5ml/min, percolation is closely colourless to the liquid of filtering, the liquid decompression recycling ethanol of filtering, pressure is-0.08Mpa that temperature is 50-80 ℃, adds beta-schardinger dextrin-45g, stir evenly, be concentrated into 50 ℃ and measure relative density 1.18～1.20.Above-mentioned three kinds of concentrated solutions are merged, stir evenly, mesh screen filters, and concentrates, and adds above-mentioned Pericarpium Citri Reticulatae, Rhizoma Zingiberis Recens volatile oil clathrate, dextrin and aspartame, and mixing is granulated, drying, and granulate, promptly.
6,, it is characterized in that its authentication method is according to the described Chinese medicine preparation of claim 4:
A. the discriminating of Ramulus Uncariae Cum Uncis
Get this product powder 8g, add ethyl acetate 60ml, strong aqua ammonia 6ml, supersound extraction 30 minutes is got upper strata liquid, and evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution.Hook taking rattan control medicinal material powder 2g adds ethyl acetate 20ml in addition, strong aqua ammonia 2ml, and supersound extraction 30 minutes filters, and filtrate is put in the separatory funnel, gets upper strata liquid, and evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, makes control medicinal material solution.According to thin layer chromatography reference " 2000 editions appendix VIB tests of Chinese pharmacopoeia, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with ratio is that the subnatant of 20: 1: 1 methylene chloride-methanol-ammonia is developing solvent, launch, take out, dry, spray is inspected under the daylight lamp with the improvement bismuth potassium iodide test solution.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical orange red speckle.
B. the discriminating of the Radix Paeoniae Alba
Get this product powder 5g, add water 30ml supersound extraction 20 minutes, filter, filtrate is put in the separatory funnel, with ethyl acetate extraction 3 times, each 10ml discards the water saturated n-butanol extraction of reuse 3 times, each 10ml merges n-butyl alcohol liquid, and evaporate to dryness, residue add water 10ml makes dissolving, on the polyamide column handled well, the polyamide consumption is 15ml, the wet method upper prop, internal diameter 15-20mm washes with water to colourless, collects water lotion, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets the peoniflorin reference substance, adds methanol and makes every 1ml and contain 1mg solution, in contrast product solution.According to thin layer chromatography reference " 2000 editions one appendix VI B test of Chinese pharmacopoeia, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with ratio is 40: 5: 10: chloroform-ethyl acetate of 0.2-methanol-formic acid is 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 the corresponding position of reference substance chromatograph on, show identical aubergine speckle.
C. the discriminating of Rhizoma Chuanxiong
Get this product powder 5g, add 40ml ethyl acetate supersound extraction 20 minutes, filter, filtrate is put evaporate to dryness in the water-bath, and residue adds ethyl acetate 0.5ml makes dissolving, as need testing solution.Other gets Rhizoma Chuanxiong control medicinal material powder 0.05g, add 40ml ethyl acetate supersound extraction 20 minutes, filter, filtrate is put evaporate to dryness in the water-bath, residue adds ethyl acetate 0.5ml makes dissolving, make control medicinal material solution, according to thin layer chromatography reference " 2000 editions one appendix VI B test of Chinese pharmacopoeia, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be 10: 1 petroleum ether (60～90 ℃) with ratio: ethyl acetate is developing solvent, launch, take out, dry, put under the uviol lamp 365nm and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
D. the discriminating of Radix Glycyrrhizae
Get this product powder 5g, add water saturated n-butyl alcohol 40ml, supersound extraction 30 minutes, filter, filtrate evaporate to dryness, residue add water 10ml makes dissolving, on the polyamide column handled well, the polyamide consumption is 15ml, the wet method upper prop, internal diameter 15-20mm washes with water earlier to colourless, continues with the 30ml70% ethanol elution, collect eluent, put evaporate to dryness in the water-bath, residue adds methanol 1ml makes dissolving, as need testing solution.Extracting liquorice control medicinal material powder 0.5g adds 30ml water-saturated n-butanol supersound extraction 20 minutes in addition, filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution.According to thin layer chromatography reference " 2000 editions one appendix VI B test of Chinese pharmacopoeia, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with ratio is that methylene chloride-methanol-water of 40: 10: 1 is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and putting 105 ℃, to be heated to the speckle colour developing clear.In the test sample chromatograph, respectively with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
7, according to the described Chinese medicine preparation of claim 4, it is characterized in that: contain gastrodine 1.5mg-6mg in every gram granule, contain peoniflorin 1-10mg in every gram granule.
8,, it is characterized in that the content assaying method of gastrodine is according to the described effective ingredient of claim 7:
The preparation of reference substance solution: it is an amount of that precision takes by weighing the gastrodine reference substance, adds methanol and make the solution that contains 40 μ g among every 1ml, in contrast product solution;
The preparation of need testing solution: get powder 1.0g, accurate claim surely, put in the 25ml measuring bottle, add 50% methanol 20ml, supersound extraction 30min is put coldly, and standardize solution shakes up, and high speed centrifugation 10 minutes is got supernatant, promptly;
Chromatographic condition: with octadecylsilane chemically bonded silica is filler;
Volume ratio is that 12: 88 methanol-0.1% sour water is a mobile phase;
Detect wavelength 221nm;
Algoscopy: accurate respectively reference substance solution and each 5 μ l of need testing solution of drawing, inject hplc determination.
9. according to the described effective ingredient of claim 7, it is characterized in that the paeoniflorin content assay method is:
The preparation of reference substance solution: it is an amount of that precision takes by weighing the peoniflorin reference substance, adds methanol and make the solution that contains 0.230mg among every 1ml, in contrast product solution.
The preparation of need testing solution: get powder 2.5g, accurate claim surely, put in the 25ml measuring bottle, add 80% methanol 20ml, supersound extraction 40min is put coldly, and standardize solution shakes up, and centrifugal 10 minutes of 10000rpm gets supernatant, promptly.
Chromatographic condition: with octadecylsilane chemically bonded silica is filler;
Volume ratio is that 30: 70 methanol-0.05% sour water is a mobile phase;
Detect wavelength 230nm;
10, according to Claim 8,9 described content assaying methods, it is characterized in that: its sour water is the aqueous solution of organic acid or phosphoric acid.
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